where P is absolute pressure (kilopascal or    test. In addition, the system displays the
lbf·in.–2 absolute); Pgage is gage pressure    ambient pressure and temperature
(kilopascal or lbf·in.–2); Pbarometer is       conditions. Flow measurements, vital to
barometric pressure (kilopascal or lbf·in.–2)  leakage verification tests, are also integral
obtained in uncorrected form from local        functions. This system accommodates the
weather bureau or read from a precision        superimposed leak tests technique or the
barometer and converted to pressure            pumpback technique (the mass change
units. Where pressures are measured in         verification leak test). The leakage test
other units such as torr, inch of mercury      data are represented by a visual display, a
or foot of water, the pressures must be        printed record of the raw test data and a
converted consistently either to English       concurrent minicomputer calculation of
units or preferably to SI units. After         the leakage rates, in several forms.
conversions have been made, the rate of
absolute pressure change can again be          Components of Integrated
calculated by use of Eqs. 10 or 11.            Leakage Rate Measurement
                                               System
Data Acquisition, Analysis
and Recording Systems for                      Figure 21 shows a schematic diagram of
Leakage Rate Testing                           the components and system used in an
                                               integrated leak testing system. Typical
Data recording for large scale pressure        leakage rate computations are based on
change leakage tests is made simpler by        measurements of the changes in the
sophisticated numerical data acquisition       absolute pressure, water vapor pressure
systems. There systems automatically           and the dry bulb temperature. The
multiplex the conditioned signals from         absolute pressure is measured with a fused
the pressure, temperature, dewpoint and        quartz Bourdon tube. The low internal
flow measuring sensors (during the             viscosity of fused quartz makes it the most
verification phase of leak testing) at preset  perfectly elastic material available. This
automatically timed intervals. Data are        type of pressure sensor has no measurable
transmitted through an interface for           hysteresis. It also has fast response, high
numerical analysis by computer, recorded       resolution and high accuracy. The water
on magnetic tape or disk systems,              vapor pressure is measured by use of
displayed by printout or graphical             chilled mirror dewpoint sensors and is
recordings and evaluated by error analysis     presented to the minicomputer as a
and statistical techniques.                    dewpoint temperature in degrees celsius
                                               or fahrenheit.
    In many cases, this numerical test data
analysis system can analyze the data by            The dry bulb temperature is measured
progressive analysis (with least mean          by resistance temperature detectors and is
squares fit to straight line approximations    also presented to the minicomputer as
of leakage as a function of testing time).     digital data. Because the changes in the
Computers provide the fastest and most         test parameters are small in magnitude, all
accurate technique for analysis of the         input sensors must be capable of high
pressure change leak test data. The data       sensitivity, accuracy, repeatability and
can be fed into the computer directly          resolution. Similar high accuracy, high
from the acquisition system interface,         resolution and reliability are required of
from tape or manually from printer or          the electronic networks and digital
recorder readouts. This absolute technique     computer analyses.
analysis of leakage rate may be performed
by mass point or leakage rate point-to-        Microprocessor Data Acquisition
point, point-to-point cumulative and total     and Analyses with Leakage Rate
time statistical analysis techniques.          Measurement System
Minicomputer Integrated                            A microprocessor (minicomputer)
Leakage Rate                                   controls the minicomputer data
Measurement System                             acquisition and raw data recording
                                               system. The microprocessor system
Integrated leakage rate measurement            includes both read-only memory (ROM)
systems are available that include all         and random access memory (RAM), a
components from input sensors to               scanner system and various interfaces
minicomputer analyses of test data. This       with sensor and output system
system will measure and record the             components. Digital data for pressure, dry
absolute pressure, the dewpoint                bulb temperature and dewpoint
temperature and the dry bulb temperature       temperature are presented in ASCII
of the air within the system under leakage     (American Standard Code for Information
                                               Interchange) to the computer which then
                                               operates on these raw test data and
                                               calculates the leakage rate (see discussion
                                               below).
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Example of Analysis of                                        [∆ P    =    (42.0 + 14.7)
Data from Pressure Hold
Test of Small Volume Test                                     ∆T
Object
                                                                      ( )−       +        89.5  +  460    ⋅     h –1
Table 6 shows leak test data analysis for                                  42.0     14.7  95.8  +  460       2
pressure hold tests of a small volume test                                                              
object with an allowable temperature
corrected pressure loss of 0.5 lbf·in.–2 in                           = 56.7 − 56.7 549.5 loss in 2 h
2 h. In these tests, corrections for                                                        555.8
variations in barometric pressure were not
required.                                                             = 0.6 lbf ⋅ in.–2 loss in 2 h
    Analysis of data for the first pressure                           = 0.3 lbf ⋅ in.–2 ⋅ h–1
hold test on day one by means of Eq. 8
shows that the test object has failed the                         This leakage rate exceeds the maximum
requirements of the pressure hold test:                       acceptable temperature corrected pressure
                                                              loss of 0.5 lbf·in.–2 in 2 h, so the test
                                                              results are not satisfactory. A leak was
                                                              located in the pressure zone and the welds
                                                              repaired. The pressure hold test was then
                                                              repeated four days later with the results
                                                              shown in the last two columns of the
                                                              table in the left hand column. In this
                                                              case, analysis of the pressure hold test
                                                              data showed:
FIGURE 21. Information flow diagram for minicomputer controlled integrated leakage rate measurement system using a
microcomputer, dual disk memory and instrument display console.
Containment                     Console                                          Digital
                        Quartz manometers
 Containment                                          Preset up/down
    pressure                                               counter
                                              Analog                       Digital
 Verification air flow  Turbine flow meters           Microprocessor data
                                                            conversion
       Resistance
      temperature                                                                                       RS-232-C
        detectors                                                                                                      Input/output
                                                                                                                       port
       Dew point
     hygrometers            Resistance                Analog               Digital              Analog
                          temperature
    Linear variable     detectors (signal
differential and other   conditioning)
      transducers                                                                   Scanner
                             Hygrometer               Analog
                        control conditioning
                                                                                                              Digital data encoder
                                circuitry
                                                                                                        Digital
                                                                                    Manual
                                                                                    scanner
                                                      Analog                                                     Panel meter
                          Structural                                                               Analog
                        integrity test
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 189
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∆P  =  56.7 − 56.7 550.0     +  56.7 − 56.6    rates of leakage, the compressor must
                      550.7                    operate for a large proportion of the test
                                               time. With low leakage rates, the same
∆T 2 h                            2h           compressor need operate only
                                               occasionally for relatively short time
    = 0.1 lbf ⋅in.–2 loss in 2 h               periods. If it is desired to measure the
                                               absolute value of leakage by this
    = 0.05 lbf ⋅in.–2 ⋅h–1                     technique, the capacity of the compressor
                                               at the test operation pressure should be
This leakage rate is well below the            known or be determined in a separate
                                               compressor calibration test.
maximum allowable temperature
corrected pressure loss rate of 0.5 lbf·in.–2      When leak testing by the cyclic
in 2 h, so the test object is now              pressurization technique, operators need
                                               two stopwatches and a rapid response
acceptable.                                    pressure gage with a clear scale. Prior to
                                               the first measurements, the compressor is
    The calculations in SI would reflect the   allowed to charge the system under test to
fact that 1 lbf·in.–2 ≅ 6.9 kPa.               its normal operating (or delivery)
                                               pressure. The compressor control valve is
Determining If Pressure                        then shut off to isolate the test vessel. The
Hold Test is Completed or                      compressor is allowed to operate under no
Should Be Extended                             load conditions while the pressure in the
                                               test vessel falls off to a suitable lower
A pressure hold leakage rate test may be       pressure limit value, well below the initial
concluded at the end of the required test      compressor delivery pressure. When this
period if the magnitude of the pressure        pressure limit is reached, one stopwatch is
loss is within (lower than) the specified      started and the compressor is put under
allowable rate of pressure loss. If the test   load by manual opening of the isolation
results are subject to question, the test can  control valve. During this operation step,
be continued over a longer time period to      the compressor pumps air or gas into the
increase the reliability of the test data. If  test vessel to raise its internal pressure.
the extended test confirms that the actual     This first stopwatch is stopped when the
pressure loss rate is in excess of the         test pressure has risen to a predetermined
specified allowable limits, the system         upper pressure limit.
should be reinspected to detect the
locations of the excess leakage. The               When this upper limit is reached, the
system leaks should then be repaired and       compressor is cut off by closing the
the system retested to the same                isolation valve of the test vessel and the
specifications and procedures.                 second stopwatch is started. When the
                                               internal pressure of the test vessel or
Leak Testing Techniques                        system again falls to the original lower
Using Cyclic                                   pressure limit, the second stopwatch is
Repressurization with                          stopped and reset. Then the first watch is
Compressor                                     started as the compressor is again put
                                               under load to repressurize the test system.
Intermittent operation of a compressor         A new cycle of pressurization is initiated
can be used for leakage measurements by        and the alternating stopwatch readings for
evaluating the load cycle (duty cycle)         pressurization time and leakage time are
when a compressor of known capacity            taken. Four or five cycles of
maintains a specified pressure in the          repressurization and pressure decay are
system under test. (The duty cycle is the      carried out in succession to ensure that
ratio of the time the pump operates, on        the compressor is running under constant
time, to the total time testing — on time      and reproducible conditions, as required
plus off time for the pump.) With large        to obtain accuracy in the leak test
                                               measurements.
TABLE 6. Pressure hold test data.             _________D__a_y_O__n_e_________  _________D_a_y__F_o_u_r________
 Date:                                         09:50        11:50              15:30  17:30
 Time:                                         31.9 (89.5)   35.4 (95.8)        32.2 (90.0) 32.6 (90.7)
                                              290 (42.0)    290 (42.0)         290 (42.0) 290 (42.0)
  Average surface temperature, °C (°F)                      285 (41.4)
  Actual test pressure, kPa (lbf·in.–2 gage)                                                       289 (41.9)
  Final temperature corrected
                                                            4.1 (0.6)                 0.7 (0.1)
    test pressure, kPa (lbf·in.–2 gage)
  Loss in test pressure, kPa (lbf·in.–2)
190 Leak Testing
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The cyclic repressurization leak test      2. A rubber dual tubing (two separate
technique is based on the assumption that          tubular passages) of length sufficient
no gas is supplied to the system under test        to reach from the rubber bags to a leak
during the no load period. With a                  test control panel. One of the tubular
reciprocating pump compressor unit,                passageways connects to the rubber
when the load is removed it is not                 bags and is used for their
uncommon for the compressor to                     pressurization. The second tubular
continue to deliver some gas during the            passageway extends through the
no load period. This can be avoided by             adjacent rubber bag and opens into
ensuring that the compressor is provided           the pipeline interior space between the
with a delivery system that enables all gas        two rubber bag seals. This tube
in the intercooler to be discharged into           transmits the contained natural gas
the atmosphere during the no load                  pressure to the control panel, where
period.                                            any loss of pressure due to leakage of
                                                   gas from the test volume can be
Advantages and Limitations of                      monitored.
Cyclic Repressurization Leak
Testing                                        3. A control panel with an inclined water
                                                   gage connected to the test volume by
The cyclic repressurization leak testing           the rubber tube. This gage is used to
technique has the advantage of requiring           measure any variation in gas pressure
only very simple equipment. Its accuracy           in the gas line section between the
in leakage measurements is less than the           rubber bag seals. A spring gage is used
accuracy of more direct leak testing               to indicate the air pressure within the
techniques. It is subject to random errors         sealing bags.
caused, for instance, by malfunctioning
compressor valves. Therefore, these valves     4. Connections are provided to a
should be checked for satisfactory                 pressure pump used to inflate the
operation before starting each cyclic              rubber sealing bags and to a suction
pressurization leak test. The cyclic               pump that deflates the bags.
pressurization test does not indicate the
volume of the system under test, nor does      5. A steel rod is used to propel the bag
it provide means for leak location.                frame and tubing along the inside of
                                                   the gas main. The rod and bag frame
    When several compressors are                   have sufficient flexibility to be passed
available, the compressor selected for the         through a tape on the gas line and yet
leak tests should be one which if possible         have stiffness sufficient to avoid
gives charging times at least as long as the       buckling when the apparatus is
leakage times. It is not advisable to              pushed along inside the gas main.
operate the compressor under part load
conditions, because its delivery capacity is  Procedure for Leak Testing of
rarely determined with the same accuracy      Natural Gas Mains with Rubber
for lower loads as for full load.             Sealing Bags
Compressors with dead space regulation
have a part load capacity that may differ     When testing for leakage in natural gas
between (1) a compressor calibration test     mains, the sealing bags described
and (2) a system leakage test, if the         previously are inserted into a main
quantity and temperature of the               pipeline containing gas under moderate
compressor cooling water are different in     distribution pressure. The rubber sealing
these two cases.                              bags are spaced a set distance apart on the
                                              frame. These bags seal off a portion of the
Localizing Leaks in Low                       main line when they are inflated with a
Pressure Gas Mains                            pressure tire pump to 20 to 40 kPa (3 to
                                              6 lbf·in.–2). The gas pressure in the test
Gas utilities use a modification of the       volume between the two sealing bags is
pressurizing mode of leakage                  indicated on the inclined water gage on
measurement to localize leaks in gas          the test control panel as soon as the bags
mains. The main is tested, section by         are inflated to form pressure seals. When
section, with the leak locator inside the     the main gas distribution line is sealed off
pipe. The leak locator consists of the        completely by both bags, the pressure in
following parts:                              the test volume between the bags will
                                              remain constant, as in a pressure hold
 1. A flexible frame on which are spaced      leak test. Loss of pressure would indicate
     two rubber gas bags jointed by a         gas leakage through the wall of the
     rubber tube. These bags are pressurized  distribution pipeline, in the length
     to seal off a short section of gas       between the two sealing bags.
     pipeline for the leakage test.
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 191
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PART 3. Pressure Change Tests for Measuring
Leakage in Evacuated Systems
Introduction to Pressure                     International System of
Measurements in                              Units (SI Units) for
Evacuated Systems                            Vacuum Pressures
By popular usage, atmospheric pressure is    The SI unit for pressure is the pascal (Pa)
taken as the upper limit of vacuum. Any      and is introduced here as the unit of
pressure less than standard atmospheric      pressure in vacuums. Many processes
pressure (101 kPa) is some form of           require medium levels of vacuum of the
vacuum. On Earth, vacuum pressure can        order of 0.1 to 1 Pa. However, for many
be anything between absolute zero            applications such as high altitude
pressure and the barometer reading at the    simulation chambers, pressures much
particular location and time. Earlier, the   lower than 0.1 Pa are required. Units of
vacuum pressure was measured in inch of      millipascal (mPa) or micropascal (µPa) are
mercy (in. Hg) or millimeter of mercury      used to describe pressures in this range of
(mm Hg) below atmospheric pressure. A        hard vacuum, to avoid negative
vacuum of 28 or 29 in. Hg was considered     exponents or powers of ten. The
to be a fairly good vacuum. Now, using SI    previously used unit of torr (1 torr =
units, this same vacuum level would be       1 mm Hg) must be multiplied by 133 to
expressed as an absolute pressure of 3 to    equal the pressure in pascal. The millitorr
6 kPa, which is 3 to 6 percent of normal     is equal to pressure of 133 mPa. Because
sea level atmospheric pressure, 101 kPa      the pressure of the standard atmosphere
(1 atm).                                     at sea level is 1.01 × 105 Pa or 101 kPa, it
                                             follows that perfect vacuum would have a
Meaning of Absolute                          (negative) gage pressure of (–) 101 kPa
Pressure and Gage                            because the gage pressure in vacuum is
Pressure in Vacuum                           referred to the standard atmospheric
Systems                                      pressure at sea level.
As suggested earlier, the concept of a       Conversions of Vacuum Pressures
vacuum is related to the pressure exerted
by the earth’s atmosphere. Atmospheric       from Prior Units to Pascal
pressure indicates the weight of a column
of atmospheric air of unit cross sectional   The twentieth century has seen many
area measured at a particular altitude       change in the units used to describe
above sea level. With increasing altitude,   pressure levels in vacuums. Early
the pressure decreases until, at some        investigators described their vacuum
indefinitely great height above the earth’s  pressure in terms of millimeter of
surface (where only empty space exists),     mercury, or torr, where the atmospheric
the pressure approaches absolute zero. An    pressure at standard conditions was taken
enclosure is said to be under vacuum if its  as 760 torr. Hard vacuum pressures were
internal pressure is less than that of the   later described in terms of micrometer of
surrounding atmosphere. Because of           mercury (1 µm is one millionth of a meter
atmospheric pressure changes due to          of mercury). Vacuum pressures are
meteorological factors and altitude, the     variously expressed in pound per square
numerical value assigned to gage pressure    inch absolute pressure (lbf·in.–2 absolute),
in vacuum is referred to atmospheric         inch of mercury, torr and the SI unit
pressure under standard conditions at sea    pascal. For example, 1 µm Hg = 0.001 torr
level (an absolute pressure of 101 kPa). As  = 10–6 m Hg = 133 mPa = 0.133 Pa. The
vacuums were improved, it became             pressure of the standard atmosphere is
necessary to provide a scale of absolute     then equal to 760 torr. The (negative)
pressures (somewhat analogous to the         gage pressure for a perfect vacuum would
scale of absolute temperatures). The         then be –760 torr in this system of units.
concept of a perfect vacuum corresponds      (An absolute pressure of 1 torr is equal to
to the hypothetical state of zero absolute   133 Pa.) The preferred unit is pascal.
pressure.
                                                 Conversion factors relate the various
                                             units used to describe pressures in
                                             evacuated systems, including the pascal,
                                             atmosphere (atm or torr and the
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micrometer of mercury). Figure 22 shows                     might seem that eventually a pressure of
a scale useful for approximate conversions                  absolute zero would be obtained. This
of vacuum pressures between SI units of                     would be true if the only molecules to be
pascal and earlier units of millimeter of                   removed were those in the gas space.
mercury (equal to torr) for several typical                 However, other gas sources do exist and
ranges of vacuum pressure. These                            must be considered. The predominant gas
comparisons may also help personnel to                      sources are leakage and outgassing.
convert their data into SI units.                           Leakage is the direct transmission of gas
                                                            molecules, driven by the higher external
Limitations on Ultimate                                     pressure, through holes or porosities in
Vacuum Pressure Caused                                      the vacuum chamber wall, in welds or in
by Leakage and                                              the various seals used in the system.
Outgassing                                                  Outgassing refers to all forms of gas
                                                            coming from the materials in the vacuum
During evacuation of a container,                           system. It includes gases that are adsorbed
molecules are constantly being removed                      on the surface, dissolved in the material
by the pumping process. Therefore, it                       and occluded in gas pockets, as well as
                                                            those due to evaporation or
FIGURE 22. Histogram for conversion of vacuum absolute      decomposition.
pressures between prior unit of torr and SI unit of pascal
(1 std atm = 100 kPa = 760 torr).                               The continual addition of gas from
                                                            these sources represents the major
1000                                   133 kPa              limitation on the ultimate pressure that
         800                           100 kPa = 1 atm      can be obtained in evacuated systems.
                                   80                       Mathematically, the ultimate pressure Pu is
 760                               60                       given by the influx of gas Q divided by
         600                                                the pumping speed S, so that Pu = Q /S.
                                   40                       Because the vacuum pump is itself a
         400                                                source of outgassing, it can contribute a
                                                            limiting component Pp to the ultimate
200                                                         vacuum pressure. Its effect is frequently
                        20                                  included in the prior equation for
                                                            ultimate pressure. In this case, Pu = Q /S +
                              100torr                       Pp, where the term Q now refers to the
                               80                      kPa  influx of gases from all sources except the
                               60                           vacuum pump.
                                   10 kPa
                               40   8                           Even though the pump may be
                                    6                       operating at a particular limit pressure for
25.4 torr = 1 in. Hg                4                       one type of gas, because of a leak or
                               20                           outgassing, it can still pump other gases
                                    2                       to extremely low partial pressure. This is
                                                            true because, in molecular flow, all types
10                                                          of gases flow independently of each other.
 8                                                          Typically, a gas analysis of an ultrahigh
                               1                            vacuum system operating at a total
                                                            pressure of 10 nPa (~1 × 10–10 torr) will
                                                            show hydrogen and carbon monoxide as
                                                            the residual gases still coming from the
                                                            walls of the vacuum system in this
                                                            ultrahigh vacuum range. This occurs even
                                                            when the partial pressure of the original
                                                            nitrogen and oxygen are too low to be
                                                            measured.
                                                            Pumping Requirements for
                                                            High Vacuum Systems
                                                            The ideal gas laws apply to ideal gases
                                                            even at very low vacuum pressures. They
                                                            do not apply, however, to condensable
                                                            vapors such as water vapor or refrigerant
                                                            gases. The implications of the ideal gas
                                                            laws become evident when considering
                                                            the effect of reduced pressure on the
                                                            volume of a fixed quantity of ideal gas
                                                            held at constant temperature. A liter of
                                                            gas at standard atmospheric pressure
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 193
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would increase in volume as pressures are         total amount of moisture is very small
                          lowered in the vacuum region (Table 7).           (such as water adsorbed over a small
                                                                            surface area).
                              Tremendous multiplying factors come
                          into existence as the pressure drops in an        Ensuring Cleanliness of
                          evacuated system. The pumping speed in            Welded Vessels to Be
                          cubic meters per second does not increase         Evacuated for Leak Testing
                          as pressure is lowered, so much smaller
                          masses of gas (fewer gas molecules) are           In preparation for leak testing by pressure
                          removed per unit of time, as system               change or helium tests with a tracer probe
                          pressure drops.                                   or hood, the interior of the system under
                                                                            test is evacuated. A sensitive vacuum
                          Residual Gas Molecule                             pressure gage is then used to measure
                          Densities in High Vacuum                          pressure change or a helium mass
                          Systems                                           spectrometer is used to detect helium
                                                                            tracer gas that reaches the vacuum pump
                          Because the mass reduction factor is so           input. Joints for high vacuum vessels are
                          great when evacuating a test system, it           far more critical than joints in pressure
                          might be assumed that after pumping to            vessels that also operate under 100 kPa
                          reach low pressure, there is really nothing       (1 atm) of differential pressure.
                          in the container to affect any work that
                          may be inserted within it. However, one               Microporosity in the weld, entrapped
                          must consider the number of molecules             gases or solids and surface layers that
                          that remain at various pressures. It may be       outgas become major problems with high
                          recalled that there is a physical                 vacuum equipment or equipment that
                          relationship stating that 22.4 L (0.89 ft3)       will be evacuated for leak testing.
                          of any gas will contain 6.023 × 1023              Extremely small defects or inclusions in
                          molecules at 0 °C (32 °F) and 101.325 kPa.        welded joints may not be detectable with
                          The natural constant, 6.023 × 1023, is            the usual nondestructive testing
                          known as Avogadro’s number. If the gas            techniques. The leak testing of the
                          pressure is now reduced to 0.1 Pa or one          evacuated system may be compromised
                          millionth of its previous value, the 22.4 L       because of such small leak and gas
                          (0.89 ft3) volume of gas still within the         sources.
                          container contains 6 × 1017 molecules.
                          Even at 1 µPa, some 6 × 1012 molecules                For valid leak detection and location by
                          will still remain in the 22.4 L (0.89 ft3)        the tracer probe technique or leakage
                          volume. This provides a residue of                measurement by the hood technique,
                          3 × 1011 molecules or almost one trillion         cleanliness of the test object surfaces and
                          molecules per liter of volume (one billion        the leak testing system is essential. Tracer
                          per cubic centimeter). To obtain low              gas can accumulate in surface dust and oil
                          ultimate vacuum pressures, one must               or grease, including that within leak
                          reduce the various sources of gas within          passageways, possibly causing small leaks
                          the system being pumped down. Leakage             to remain undetected when they are
                          can be eliminated only by first locating          exposed to the tracer probe gas only
                          each leak and then properly repairing it or       briefly. Alternatively, evaporation of
                          by placing an adequate temporary seal             condensed vapors and gases from such
                          over it. Maintaining cleanliness and              contamination layers may cause a
                          avoiding introduction of moisture into            sensitive leak detector system to indicate
                          the test system before the vacuum                 leakage when the system is actually
                          pumpdown are vital. However, where                leaktight. The larger the system under
                          moisture has contaminated the interior            test, the more important it is to ensure
                          volume of a test system, vacuum pumping           cleanliness (including weld crevices and
                          can help to remove the moisture, if the           surface discontinuities). The inert gas
                                                                            tungsten arc welding (GTAW) process
TABLE 7. Gas volume variation with pressure.                                produces clean welded joints with
                                                                            minimum permeability to atmospheric or
_G__a_s_P_r_e_s_s_u_r_e_  ___V_o_l_u_m__e_o__f _G_a__s__                    tracer gases. The absence of welding flux
                                                                            minimizes post weld cleaning operations
                          m3 (ft3)                                          and problems of outgassing from slag
                                                                            inclusions.
Pa (atm)                                                  Description
105   (100)               10 –3  (3.5 × 10–2)             atmosphere
103   (10–2)              10 –1  (3.5 × 100)
100   (10–5)              10 2   (3.5 × 103)              high vacuum
10–3  (10–8)              10 5   (3.5 × 106)              very high vacuum
10–6  (10–11)             10 8   (3.5 × 109)
10–9  (10–14)             10 11  (3.5 × 1012)
194 Leak Testing
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Effects of Weld Joint                                    volumes (at the roots of butt welds made
Design on Leak Testing of                                from two sides of the plate, or fillet welds
Evacuated Vessels                                        with unwelded areas between abutting
                                                         plates).
For pressure vessels to be evacuated
during leak testing (and vessels designed                Factors Influencing Speed
for vacuum operation), the weld joint                    of Vacuum Pumping of
design and preparation should avoid                      Large Volume Systems
trapped volumes or unwelded faying
surface areas that will be exposed to the                The pumpdown time or time required for
vacuum side of the joint. Both form                      evacuation of large vessels and systems
crevices that may hold foreign matter that               from atmospheric pressure is highly
can outgas during evacuation or may                      dependent on the condition of the
provide traps for tracer gases. Because                  vacuum system, the volume to be
cleaning of such crevices is often                       evacuated and the pumping speed. Any
impossible, joint design and welding                     significant amount of water contained in
procedures must eliminate such traps.                    the system will have a powerful effect on
Welding should be performed from the                     the time required for pumpdown because
side of the joint that will be evacuated                 water has a vapor pressure of 2.26 kPa
whenever practical. The under bead often                 (17 torr) at 20 °C (68 °F). When water is
contains unavoidable microporosity too                   present within the system to be
small to affect most strength and                        evacuated, the pressure will not drop
toughness properties of the welded                       below this value until the bulk of the
structure. However, if exposed to the                    water has been pumped out. (Drying by
vacuum, these voids could act as trapped                 evacuation is often a useful way to
volumes. Leakage from this source can be                 remove water trapped or condensed
avoided by welding the cover (or seal)                   within pressure vessels, piping and
pass from the side of the pressure                       components.) Consequently, water or
boundary that will be evacuated.                         other vaporizing liquids should not be
Figure 23a shows examples of preferred                   introduced into test systems before leak
joint designs for systems that will be                   tests that require evacuation, if it can
exposed to high vacuum. Figure 23b                       possibly be avoided. Evacuation rates
shows undesirable joint designs which                    attained by mechanical pumps drop
provide dirt traps and create trapped                    rapidly as the pressure is reduced by
FIGURE 23. Weld joint designs for welded vessels: (a) preferred designs have no crevices or volume traps open to evacuated
side of pressure boundary; (b) undesirable joints trap contamination and tracer gases, which may outgass during evacuation or
leak testing with sensitive mass spectrometer or other vacuum leak detectors.
(a)
(b)                                      T               T
                                                      T               T
       T
Legend
         = Vacuum side
         = Continuous weld
    T = Locations of probable gas traps
         = Intermittent weld
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 195
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pumping. Gas evolution by evaporation                 factor of 5, so that the pumpdown time is
of liquids at very low pressures increases            estimated as:
rapidly and prolongs the pumping period
required to attain desired vacuums.                           T = 2.3 × 5 V = 11.5 V
                                                                                          SS
Techniques for Estimating
Time Required for                                     Alternative Technique for
Pumpdown to 10 kPa                                    Estimating Pumpdown
(75 torr)                                             Time to 10 kPa (75 torr)
A technique for approximating the                     An alternative approximation technique
mechanical pumpdown time for very                     for estimating pumpdown time of
large systems as given by Guthrie in                  practical industrial systems with prior
Vacuum Technology7 uses the relation:                 contamination is also presented by
                                                      Guthrie.7 This technique applies for many
(64) T = 2.3 V                                        average industrial systems that may have
                           S                          various sources of gas, vapor and leaks
                                                      that will require larger pump sizes for any
where T is approximate pumpdown time                  given pumpdown time. For example, gas
(2.3 time constants) to ten percent of                may be trapped on interior surfaces by
initial atmospheric pressure (to about                mechanisms such as absorption (which
10 kPa or 75 torr); V is volume of test               refers to binding of gas in the interior of
system to be evacuated from atmospheric               solid or liquid materials) or adsorption
pressure (100 kPa or 750 torr); S is                  (which refers to condensation of gas or
pumping speed of evacuation pumps,                    vapor on the surface of a solid). Despite
volume unit per unit of time.                         efforts to maintain or restore cleanliness
                                                      to the system, there will be variations
    Consistent units must be used for each            from system to system in the rates of
term in the above equation, such as those             outgassing of these trapped gases and
in Table 8.                                           vapors, which will change the required
                                                      pumpdown time to achieve specific
    Equation 64 indicates the pumpdown                vacuum pressures.
time required to reduce pressure to one
tenth of an atmosphere or about 10 kPa.                   This approximation technique makes
To attain lower vacuum system pressures,              use of pumping down curves such as
much more pumping time is required.                   would apply typically to clean systems of
The term on the right side of Eq. 64 must             known interior volume. For typical
be multiplied by the factors in Table 9, for          industrial systems with contamination,
various indicated final pressures within              leaks or outgassing conditions, the time
the system being pumped down.                         indicated on the pumpdown curve for
                                                      clean systems would be multiplied by a
    For example, to evacuate the system to            service factor that accounts for the effects
a pressure of only 1 Pa (7.5 mtorr), the              of nonideal systems. The service factors to
right side of Eq. 64 is multiplied by a               be used for average industrial systems are
                                                      listed in Table 10, in terms of the pressure
TABLE 8. Consistent units for pumpdown                region to which the system will be
calculation.                                          pumped down.
Time    Volume  Pumping Speed                             For example, suppose that a specific
                                                      system pumpdown curve shows a
Second  Cubic meter Cubic meter/second                pumpdown time of 200 min to pump
Second  Liter Liter/second                            from 100 Pa (750 mtorr) to a final
Minute  Cubic foot Cubic foot/minute                  pressure of 10 Pa (75 mtorr). The service
                                                      TABLE 10. Service factors for pressure
                                                      regions in pumpdown calculations.
TABLE 9. Calculation of approximate                   _________P_r_e_s_s_u_r_e__R_e_g_i_o_n__________ Service
pumpdown time.
__F_i_n_a_l_P_r_e_s_s_u_r_e__ Multiplying Factor for  Pa          (torr)                Factor
Pa (millitorr)  Equation 64                           105 to 104  (760 to 100)          1.0
                                                      104 to 103  (100 to 10)           1.25
10      100     4                                     103 to 102                        1.5
 1       10     5                                     102 to 101   (10 to 0.5)          2.0
 0.1       1    6                                     101 to 100     (0.5 to 0.05)      3.0
                                                      100 to 0       (0.05 to 0.005)    4.0
                                                                     (0.005 to 0.0002)
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factor corresponding to this final pressure                             absorption of water vapor or other
range is 2.0. The estimated pumpdown                                    condensable vapors within the interior of
time for this pressure range is then                                    the test volume. The entire interior
obtained by multiplying this pumpdown                                   surfaces were then cleaned with a broom
time of 200 min for an ideal system by a                                to remove loose dust and dirt to eliminate
factor of 2.0, to obtain an estimated                                   these particles as surfaces on which vapors
pumpdown time of 400 min in this                                        might condense and later outgas.
pressure range for the average industrial
system with contamination or leaks.                                         The technique for calculating
                                                                        pumpdown time for very large systems is
Comparison of Theoretical                                               used to predict the pumpdown time
and Actual Pumpdown                                                     periods ∆t between the initial pressure P1
Curves for Welded Steel                                                 and the final pressure P2 in accordance
Tank                                                                    with the approximation Eq. 65 and 66:8
The following is an example of a                                        (65) ∆t = K V                                ln P1
theoretical and an actual pumpdown                                                                S                      P2
curve for the annular space of a double
wall vacuum insulated liquified natural                                 (66) ∆t  =      2.3 K V                      log10   P1
gas tank. Figure 24 shows typical pump                                                            S                          P2
curves relating pumping speed to pressure
for a combination of mechanical pumps                                            = K′ V
with booster pumps. For the test to be                                                      S
reported here, the pump unit’s
performance curve is typical of several                                     In Eq. 66, K’ = 2.3 K[log10 (P1/P2)]; ∆t is
shown in Fig. 24. Before the pumpdown                                   the pumpdown time between the initial
tests, the annular space welds were
deslagged. The metal surfaces were                                      pressure P1 and the final pressure P2.
examined with a near ultraviolet light                                  Reasonable values for the K and for the K’
(used for fluorescent tracer inspection) to
detect any deposits of hydrocarbons                                     factors are given in Table 11.
(which also fluoresce under ultraviolet
radiation). All deposits detected were then                                 K values cannot be added. However, for
removed with solvent cleaner to reduce                                  calculating the pumpdown time ∆t for a
                                                                        pressure range that spans two or more of
                                                                        the pressure ranges listed above, the K’
                                                                        value to be used is equal to the sum of the
                                                                        K’ values given for the two or more ranges
                                                                        covering the pressure difference for which
                                                                        ∆t is to be calculated. For example, if the
FIGURE 24. Curves relating pumping speed to pressure in vacuum chamber for various mechanical pumps with booster pump
units.
600
                                                                                                                             1 200
                                                                                                       Instrument 1
500
                                                                                        Instrument 2                         1 000
400
                                                          Instrument 3
Speed (L·s –1)                                                                                                                      800
                                                                                                                                                               Speed (ft3·min–1)
300                                              Instrument 4                           Booster cut                                 600
                                                                                        in pressure
                                             Booster cut in pressure                    2.6 kPa (20 torr)
                                                        2 kPa (15 torr)
200 400
100 200
0                                                                                                                                   0
     10–2  10–1  100                           101                       102     103                 104                      105
                                             (0.075)                    (0.75)   (7.5)               (75)                    (750)
     (7.5 × 10–5) (7.5 × 10–4) (7.5 × 10–3)
                                             Pressure, Pa (torr)
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 197
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pump speed is fairly constant from                          Equations Used in Analysis of
atmospheric pressure (101 kPa) to a                         Vacuum Pumpdown Leak Tests
pressure of 100 Pa (1 torr), an estimated ∆t
for the pressure range could be                             The fundamental response curve for a
determined in one calculation using a K’                    vacuum system during pumpdown is
value of 7.3 or (4.0 + 3.3).                                described by Eq. 67:
    The values of K and K’ for computing                    (67) d P = Q − S P
pumpdown times as listed above apply                        dt V                        V
only for the case of clean mild steel tanks.
At pressures below 0.1 Pa (0.001 torr), the                 where P is pressure in system being
pumpdown times are primarily                                evacuated; t is time elapsed from start of
determined by outgassing conditions and                     pumping; S is effective pumping speed of
the relationships of Eqs. 65 and 66 are no                  vacuum pump; V is volume of system
longer valid.                                               being evacuated; Q is total in-leakage rate
                                                            plus outgassing load of test system; dP/dt
Vacuum Pumpdown                                             is time rate of change of pressure. The gas
Technique for Leakage                                       load may be due to leakage, evolution of
Measurements                                                gas from the walls of the evacuated
                                                            system or both.
The evacuation pumpdown technique of
leak testing involves the determination                         In the lower vacuum pressure range
and evaluation of a pressure time response                  where outgassing has significant effect,
curve for a vacuum test chamber within                      integration of Eq. 67 leads to the
which the test object is placed for testing.                pumpdown response characteristic of
Leakage measurement can be performed                        Eq. 68:
in either of two ways.
                                                                              −V     1  −  P2  S
 1. Determining leakage rate at                                                   ln           Q
     equilibrium pressure attained during                   (68) t 2 − t1  =
     pumpdown. The vacuum test chamber                                        S                S
     is pumped down to equilibrium                                                1     −  P1  Q
     pressure. Test object leakage and
     outgassing from the test chamber are                   Equation 68 describes an exponential
     measured and then subtracted from                      decay curve with a time constant equal to
     the value of outgassing measured in a                  S/V, which becomes asymptotic to an
     leakfree system.                                       equilibrium pressure defined by Eq. 69:
 2. Deriving an allowable pressure time                     (69) P = Q
     curve for the pumpdown of a system                                          S
     under test. Systems deviating from this
     relationship are considered to be                      This ultimate pressure is approached in
     leakers.                                               approximately five time constants, when
                                                            t2 – t1 = 5(S/V).
With either type of test system, it is
possible to set up an automated leak test                   Procedure for Pressure Rise
station involving a carousel system. The                    (Vacuum Retention) Test for
carousel moves the test samples into                        Leakage Rate
position, pumps them down and
measures the resultant pressures. The                       The pressure rise test (also called a
biggest difficulty with this type of leak                   vacuum retention test) is a pressure
test is the false reading produced by                       change leakage measurement technique
outgassing of dirty samples.                                performed on a system evacuated below
                                                            atmospheric pressure. It can be performed
TABLE 11. Values of pumpdown time estimation factors K      on systems at any vacuum level but is
and K’.                                                     most effective on systems evacuated to an
                                                            absolute pressure (vacuum) in the range
___________P_r_e_s_s_u_r_e_R__a_n_g_e___________  K K’      from 10 to 0.001 Pa (100 to 0.01 mtorr).
            Pa (torr)                                       This leakage rate test is performed by
                                                            isolating the system under test after it has
101 000 to 2600       (760 to 20)                 1.1 4.0   been evacuated to the required (or
   2600 to 133         (20 to 1.0)                1.1 3.3   specified) absolute pressure (vacuum).
     133 to 13.3         (1 to 0.1)               1.5 3.45  Then the pressure and, when exposed to
       13.3 to 6.6       (0.1 to 0.05)            4.0 2.77  ambient weather conditions, the surface
         6.6 to 1.3      (0.05 to 0.01)           4.0 6.44  temperature of the system are observed
         1.3 to 0.13     (0.01 to 0.001)          4.0 9.21  for a specific time to determine the rate of
                                                            pressure rise per unit of time for the
                                                            system. Figure 25 shows schematically the
                                                            test arrangement and the connections
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FIGURE 25. Arrangement of equipment for pressure rise leakage rate testing of an evacuated
system. Also known as a vacuum retention test, this test measures overall leakage rates and
requires use of a vacuum pumping system and a vacuum gage. For systems exposed to
ambient weather conditions, surface temperature detectors are used to approximate internal
air temperatures in the system. Ambient temperature must be measured in shade, not in
direct sunlight.
                                                                            Surface thermometer
                                                                                                          Boundary of test system
       Surface    Evacuated
thermometer         system
                                                              Surface thermometer
Open during test                              Closed          Vacuum pump
Vacuum gage                                   during test          system
                  Gage tube
                                              Optional valve
between the test volume, the vacuum           included in the effects described by the
pump system and the instrumentation.          General ideal gas law of Eq. 70. For this
                                              reason, in an evacuated system, it is not
Effects of Condensable                        mathematically realistic to make accurate
Vapors on Vacuum                              temperature corrections to the final
Retention Leakage Test                        pressure for pressure data taken at
                                              different temperatures.
As noted earlier in this chapter, the
behavior of vapors in an evacuated system         Therefore, to establish a fairly accurate
deviates significantly from the General       leakage rate by this pressure change
ideal gas law:                                technique for an evacuated system
                                              exposed to ambient weather conditions, it
(70) PV = n RT                                is necessary to compare pressure data at
                                              periods when the temperature is the same
A vapor is the gaseous form of any            or nearly the same and the temperature
substance that usually exists in the form     trends are in the same direction. For a
of a liquid or solid, such as water vapor. A  system enclosed in a temperature
pure liquid in equilibrium with its own       controlled building, such as a vacuum
vapor will have two phases (liquid and        chamber evacuated to lower absolute
vapor) that coexist at a specific partial     pressure ranges, temperature
pressure known as the vapor pressure.         measurements are usually not necessary. A
                                              pressure rise test of such an enclosed
    Because condensation or evaporation       system can be used to determine both the
occurs with changes in temperature, vapor     leakage rate and the outgassing rate for
molecules enter or leave the gaseous          that system.
phase with any change in temperature.
This changes the number of molecules of       Advantages of Pressure
a particular vapor and the partial pressure   Rise (Vacuum Retention)
which that vapor exerts in a particular gas   Leakage Test Technique
volume. These vapor effects, called
outgassing in a vacuum system, are not        The pressure rise leakage rate test is
                                              relatively simple in principle and fairly
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 199
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easy to perform on smaller test systems.        Factors Affecting Leakage
The test is capable of attaining increased      Sensitivity of Pressure Rise
leakage sensitivity as the system size or       Test Technique
volume decreases. That is, the total
leakage rate that can be measured as a          The leakage rate sensitivity of the pressure
pressure rise per unit time becomes             rise (or vacuum retention) leakage rate
smaller as the system under test gets           test is influenced by five major factors:
smaller in volume. This test technique can
serve as a final test or as a preliminary test   1. absolute pressure attained in the
preceding other leak test techniques,                evacuated system, when the test is
depending on the size and configuration              performed (this, in turn, affects the
of the system to be leak tested. This                resolution of the smallest measurable
quantitative leakage rate test can be used           pressure change);
to determine the total leakage rate (in the
form of a pressure rise per unit of time)        2. internal volume of the system to be
through the test boundary of any system              tested;
capable of being evacuated.
                                                 3. time duration of the leakage rate test;
Limitations of Pressure                          4. ambient temperature and weather
Rise (Vacuum Retention)
Leakage Test Technique                               conditions; and
                                                 5. internal surface areas and cleanliness
The sensitivity of the pressure rise leakage
rate test diminishes as the size or volume           of the test system.
of the system to be tested increases. Larger
rates of leakage must exist if they are to      Each of these factors is discussed next, in
be detected in large volume systems by          greater detail.
this test technique. In addition, the
location of unacceptable leakage cannot         Effect of Absolute Pressure in
be determined by this test alone. If the        Evacuated System Being Tested
actual total leakage rate exceeds the
allowable value, another leak test              When vacuum retention leakage rate tests
technique must be used to locate any            are performed within the absolute
unacceptable leaks or the numerous small        pressure range of 10 to 0.001 Pa (100 to
leaks that might contribute to an               0.01 mtorr) on large systems, the lower
unacceptable high overall rate of leakage.      the pressure, the greater the test
Thus, performance of a pressure rise test       sensitivity becomes. The limitation on the
on the evacuated annular space of a             high pressure end of this range results
double wall vessel, with a resultant total      from inability to measure very small
leakage rate indication in excess of that       pressure changes resulting from leakage
allowable, will not reveal whether the          from large volumes.
unacceptable leakage is in the inner
vessel, in the outer vessel or in a                 For example, it might be necessary to
combination of both.                            detect changes of a fraction of a pascal at
                                                2.5 kPa (a few micrometers at 20 torr).
    Because of the effect of vapors that do     The limitation on the low pressure side is
not obey the general gas laws for ideal         the increase in the portion of the pressure
gases, it becomes difficult to determine an     change attributable to outgassing. At these
accurate true gas pressure rise per unit of     very low absolute pressures, the pressure
time for very large volume systems              rise due to actual leakage is small in
exposed to wide temperature variations          relation to the pressure rise due to
during the leakage test period. Lowering        outgassing. This makes it difficult to
the absolute pressure within the                determine the true rate of pressure rise
evacuated vessel in an effort to increase       caused by real leakage.
the leakage rate test sensitivity may be
unfeasible because of the vacuum                Effect of Volume of Tested System
pumping system limitations. Alternatively,
the rate at which gas can be pumped out         The test sensitivity and, in turn, the rate
may be limited by the size of the hole          of pressure rise both vary inversely with
(penetration) through which it must be          the size or volume of the evacuated system
removed. Trying to increase the test            being tested. For example, a leakage rate of
sensitivity by increasing the duration of       5 × 10–3 Pa·m3·s–1 (5 × 10–2 std cm3·s–1) in
the test, in an effort to achieve the ability   a 570 m3 (2 × 105 ft3) system would cause
to read a smaller pressure rise per unit        a rate of pressure rise of only 0.8 Pa
time more reliably, may prove unrealistic       (5.8 mtorr) per day. This same rate of
as costs increase and schedule completion       leakage in a 0.3 m3 (10 ft3) system would
is made more difficult.                         cause a rate of pressure rise of 1.5 kPa
                                                (11.6 torr) per day.
                                                Effect of Duration of Leakage Test
                                                The sensitivity of the leakage rate test
                                                increases directly with the elapsed time
                                                during the test. As the time duration of
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the test increases, the test sensitivity       detectable total leakage rate can be
increases. The three factors of absolute       computed by Eq. 71. If instead the test
pressure P, system volume V and time           sensitivity or total leakage rate Q is
duration t of the pressure rise test are       specified or known because of system
related by Eq. 71 and 72:                      performance requirements, the allowable
                                               pressure rise per unit of time for that total
( )(71) Q = P2 − P1  V                         leakage rate can be determined by using
                     t                         the transposed form of Eq. 71 shown
                                               below as Eq. 73:
where Q is leakage rate (Pa·m3·s–1); P1 is
initial absolute pressure (torr); P2 is final  (73) P2 − P1 = Q
pressure (pascal); V is volume of                             tV
evacuated system under test (cubic meter);     or in torr·h–1:
t is time duration of test (second).
( )(72) Q = P2 − P1    V                       (74)  P2 − P1       = 96.6 Q
                     96.6 t                               t                     V
where Q is total leakage rate (std cm3·s–1);   Units for variables in Eqs. 73 and 74 are
P1 is initial absolute pressure (torr); P2 is  given below Eqs. 71 and 72, respectively.
final absolute pressure (torr); V is volume
of evacuated system (cubic foot); t is time        If the rate of pressure rise computed by
duration of test (hour). For other systems     Eqs. 73 and 74 is measurable with
of units, the conversion factor of 96.6 will   available test equipment at the specified
change.                                        test pressure, the required or specified
                                               leakage rate test sensitivity can be
Effects of Weather and Ambient                 achieved. If it is not measurable, then an
                                               attainable test sensitivity must be
Temperature Conditions                         established by Eqs. 71 and 72.
In pressure rise (vacuum retention) tests      Example Computation to
of evacuated systems, the greater the          Determine Pressure Rise Test
exposure of the system to direct sunlight      Feasibility
and the greater the variations in ambient
temperature, the more difficult it becomes     As an example of the application of
to determine an accurate pressure rise.        Eq. 74, suppose that the performance
Temperature variations lead to                 specification for a system requires that the
uncontrollable effects on the rate of          completed system contain no leakage in
outgassing or condensation of vapors           excess of 2 × 10–3 Pa·m3·s–1 (2 × 10–2 std
within the system, which also influence        cm3·s–1). This 300 m3 (105 ft3) system can
the pressure variations in the system.         be evacuated to an absolute pressure of
                                               1 Pa (or about 10 mtorr) with the
Effects of Internal Surface Area and           permanent vacuum pump system. Would
                                               a pressure rise test be a realistic test
Cleanliness of Test System                     technique for quantitatively verifying that
                                               this system meets the specification
With evacuated systems under pressure          requirements? Because Q and V are
rise leak testing conditions, the smaller      known, Eq. 73 can be solved as follows in
the internal surface area and the cleaner      SI units: (P2 – P1)/t = Q/V =
that surface is, the less the outgassing in    (2 × 10–3)/300 = 7 × 10–6 Pa·s–1 or 0.6 Pa
the systems. This reduces the effect on        per day. For mixed units, Eq. 74 indicates
pressure change from outgassing due to         that:
temperature variations.
Estimating Leakage Test                        P2 − P1          = 96.6 Q
Sensitivity Attainable in                          t                       V
Pressure Rise Tests
                                                                =         2 × 10−2
To determine the leakage rate sensitivity                          96.6
attainable with a pressure rise (vacuum                                       104
retention) test, it is necessary to know in
advance the volume (estimated or                                = 1.93 × 10−2 torr ⋅ h−1
calculated) of the system and the absolute
pressure at which the test must be             These requirements can be met by the
performed. If the allowable pressure rise      pressure rise (vacuum retention) leakage
per unit of time is known or specified and     rate test technique. The time required for
it is realistic for the absolute pressure      the test depends on the surrounding
(vacuum) level at which the test is to be      temperature conditions. If the system is in
performed, the test sensitivity or             a building in a controlled temperature
                                               environment, a test duration of only a
                                               few hours should be adequate. If the
                                               system is exposed to the weather, then a
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 201
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comparable temperature cycle must be          The specification for the pressure rise
                                  experienced. If the weather is cloudy and     (vacuum retention) leakage rate test
                                  the temperature is stable, a few hours may    required that the test be conducted over a
                                  be adequate. Normally, for an exposed         period of 72 h. The allowable pressure rise
                                  system, a temperature cycle of 12, 24 or      was 3.3 Pa (25 mtorr) in 72 h. For this
                                  36 h is necessary to achieve the necessary    time span, this was a reasonable leakage
                                  reliable comparison data.                     allowance. For the 650 m3 (2.3 × 104 ft3)
                                                                                annulus volume and allowable pressure
                                  Example of Pressure Rise Leakage              rise rate of 3.3 Pa (25 mtorr), the total
                                  Rate Test of Liquid Hydrogen                  leakage rate allowable was computed in SI
                                  Vessel                                        units as:
                                  The following example illustrates test                Q = 3.3 × 650
                                  conditions and test results for the leakage                       72 × 3600
                                  rate of the annular inner space between
                                  concentric inner and outer spheres of a                     = 8.3 × 10−3 Pa ⋅ m3 ⋅ s−1
                                  double wall vacuum insulated liquid
                                  hydrogen vessel. The outer sphere has a                     = 8.3 × 10−2 std cm3 ⋅ s−1
                                  15.81 m (51 ft, 10.5 in.) inside diameter
                                  and the inner sphere has an inside            The results of the pressure rise test
                                  diameter of 13.9 m (45 ft, 7 in.) and a       performed on the annular space of this
                                  wall thickness of about 19 mm (0.75 in.).     double wall liquid hydrogen sphere are
                                  The volume of this annular space was          shown in the pressure rise test data of
                                  calculated to be about 650 m3                 Table 12 and are plotted in the graphs of
                                  (2.3 × 104 ft3). Critical areas of the inner  pressure and temperature as a function of
                                  sphere were tested by the more sensitive      time during testing in Fig. 26. Pressure
                                  helium tracer probe or hood leak testing      levels may be compared at any of the
                                  techniques.                                   nearly equivalent temperature points
                                                                                during the night time periods marked
FIGURE 26. Graphs showing variations in temperature and absolute pressure of liquid hydrogen sphere annular space during
72 h pressure rise leakage rate test. Arrows with asterisks indicate time periods when temperatures and trends in change of
temperature were comparable. Pressure rise test liquid hydrogen sphere with 13.9 m (45 ft, 7 in.) inside diameter inner tank
and 15.8 m (51 ft, 10.5 in.) inside diameter outer tank.
                   43 (110)
Temperature, °C (°F)           38 (100)                   Average shell
                               32 (90)                    temperature
                               27 (80)
                               21 (70)       Ambient
                               16 (60)       temperature
Absolute pressure, Pa (mtorr)  6.7 (50)                   Absolute
                               5.3 (40)                   Pressure
                               4.0 (30)
                               2.7 (20)
                               1.3 (10)
                               0
                                         600 1000 1400 1800 2200 200 600 1000 1400 1800 2200 200 600 1000 1400 1800 2200 200 600
                                                                                                        Real time (h)
                                         04  8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72
                                                                                Elapsed time (h)
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with brackets and footnotes on the            Example of Pressure Rise Leakage
elapsed time column of Table 12. These        Rate Test of Laboratory Vacuum
time points are also marked by arrows and     Chamber
asterisks on the graphs of Fig. 26. The
results for this 52 h time span indicate      The following example illustrates test
that the pressure rise on this system could   conditions and test results for a pressure
have been a maximum of 250 to 400 mPa         rise test of a stainless steel solvent cleaned
(2 to 3 mtorr) in 72 h. This was an           vacuum chamber. The purpose of the test
acceptable leakage test rate because it was   was to determine the leakage rate and the
much less than the allowable rate of 3 kPa    outgassing rate of the chamber. The
(25 torr) in 72 h. The total leakage rate is  chamber had an inside diameter of
equivalent to 6.6 × 10–4 to 9.9 × 10–4        590 mm (23.25 in.) and a length of 1.6 m
Pa·m3·s–1 (6.6 × 10–3 to 9.9 × 10–3 std       (63 in.). Its volume was calculated to be
cm3·s–1). Because this loss of 250 to         about 0.487 m3 or 487 L (17.2 ft3). Its
400 mPa (2 to 3 mtorr) is less than the       inside surface area was calculated to be
error in reading of the Pirani or             about 4.63 m2 (49.8 ft2). The results of the
thermocouple vacuum pressure gage used        pressure rise test with the chamber
for the test, the pressure rise was probably  vacuum conditioned for approximately
much less. A longer test period could have    189 h are given in Table 13 and shown
proved this but would have served no          graphically in Fig. 27. Figure 27b is an
useful purpose.                               enlargement of the upper linear portion
                                              of the graph of Fig. 27a, from whose slope
                                              the final leakage rate was determined.
TABLE 12. Test data for pressure rise test of liquid hydrogen sphere.
 Real Elapsed  ______S_h_e_l_l_T_e_m__p_e_r_a_t_u_r_e_,_°_F_a______     Ambient   A_n__n_u_l_u_s_P_r_e_s_s  Information and
Time Time (h)                                                        Temperature                               Comments
               No. 1 No. 2 No. 3 Average                             °F           Pa (millitorr)
0600   0       59 56 57 57.3                                         60           2.0 (15)                  Begin hold test
0800   2
1000   4       65 77 62 68.0                                         66 2.7 (20)
1200   6
1400   8       72 100       69 80.3                                  72           3.9 (29)                  Windy, clear and sunny
1600  10
1800  12       78 112       81 90.3                                  77 5.1 (38)
2000  14
2200  16b      81 100 100                     93.7                   80 6.6 (49)
2400  18b
0200  20b      83 97 97 93.0                                         80 6.9 (52)
0400  22
0600  24       79 87 82 82.7                                         78 6.3 (47)
0800  26
1000  28       70 69 69 69.3                                         69 3.7 (28)
1200  30
1400  32       65 65 63 64.3                                         65 2.7 (20)
1600  34
1800  36       63 62 61 62.0                                         63 2.4 (18)
2000  38
2200  40b      61 59 59 59.7                                         61           2.1 (16)                  Clear and calm
2400  42b
0200  44b      58 57 56 57.0                                         59 1.9 (14)
0400  46
0600  48       56 53 54 54.3                                         57 1.5 (11)
0800  50
1000  52       63 81 57 67.0                                         65           2.4 (18)                  Clear, calm and sunny
1200  54
1400  56       76 108       69 84.3                                  77 3.5 (26)
1600  58
1800  60       80 120       85 95.0                                  79 4.5 (34)
2000  62
2200  64       82 113       96 97.0                                  80 5.7 (43)
2400  66
0200  68b      84 106       98 96.0                                  80 6.0 (45)
0400  70b
0600  72b      78 86 80 81.3                                         78 5.3 (40)
               67 70 68 68.3                                         68 3.5 (26)
               63 65 63 63.7                                         64 2.5 (19)
               61 62 61 61.3                                         62 2.3 (17)
               59 60 58 59.0                                         60           2.1 (16)                  Clear and calm
               57 58 56 57.0                                         58 1.7 (13)
               56 55 54 55.0                                         57 1.3 (10)
               65 87 70 74.0                                         71           4.0 (30)                  Clear, calm and sunny
               82 120 100 100.7                                      80 8.0 (60)
               85 129 103 105.7                                      85 10.1 (76)
               90 124 106 106.7                                      87 10.7 (80)
               93 120 104 105.7                                      88 10.7 (80)
               87 110       97 98.0                                  85 10.0 (75)
               80 93 86 86.3                                         80 8.1 (61)
               73 78 75 75.3                                         73 6.0 (45)
               70 72 66 69.3                                         68 3.9 (29)
               65 68 62 65.0                                         65 2.9 (22)
               62 63 61 62.0                                         63 2.5 (19)
               59 59 59 59.0                                         60           2.3 (17)                  End of 72 h hold test
a. (°F – 32)/1.8 = °C.
b. Data comparison points.
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 203
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The total rate of pressure rise due to      TABLE 13. Pressure rise leakage rate test of type 487 L
                                        both outgassing and leakage during the          stainless steel vacuum chamber. See Fig. 27.
                                        entire 41 h, 44 min (≅ 2500 min =
                                        150 000 s) test period was computed as:         Real Time   Elapsed  _____C_h__a_m_b__e_r_P_r_e_s_s_u_r_e_____
                                                                                        (h : min)  Time (h)        Pa (torr)
                                                  ( ) ( )1.64 × 10−2 1.72 × 101
                                                                                        16:36       0        2.9 × 10–4              (2.2 × 10–6)
                                        Total Q =                                       16:38       0.033    7.2 × 10–4              (5.4 × 10–6)
                                                                     96.6 × 41.73       16:39       0.05     9.5 × 10–4              (7.1 × 10–6)
                                                                                        16:40       0.067    1.2 × 10–3              (8.7 × 10–6)
                                                      = 7.0 × 10−6 Pa ⋅ m3 ⋅ s −1       16:41       0.083    1.3 × 10–3              (1.0 × 10–5)
                                                                                        16:44       0.133    1.9 × 10–3              (1.4 × 10–5)
                                                      = 7.0 × 10−5 std cm3 ⋅ s −1       16:47       0.183    2.7 × 10–3              (2.0 × 10–5)
                                                                                        16:53       0.283    4.1 × 10–3              (3.1 × 10–5)
                                            Based on the straight line portion of       16:57       0.35     4.9 × 10–3              (3.7 × 10–5)
                                        the last 23.5 h of the test as shown in the     08:50      16.23                             (7.2 × 10–3)
                                        graph of Fig. 27b, the leakage rate Q for       10:50      18.23     1.0                     (8.0 × 10–3)
                                        the chamber was computed as:                    14:00      21.40                             (8.7 × 10–3)
                                                                                        16:50      24.23     1.1                     (9.7 × 10–3)
FIGURE 27. Pressure rise leakage rate test of a type 487-L                              08:30      39.90                             (1.58 × 10–2)
stainless steel vacuum chamber: (a) pressure rise as a                                  10:20      41.73     1.2                     (1.64 × 10–2)
function of time; (b) enlargement of upper portion of curve,
showing rate of pressure rise due to leakage, following                                                      1.3
outgassing of steel vacuum chamber. See Table 13.
                                                                                                             2.1
                                                                                                             2.2
(a)                                     (10–2)                                                 ( ) ( )8.4 × 10−3 1.72 × 101
       1.3 × 100                                                                         Q=
                                                                                                                96.6 × 23.5
Pressure, Pa (torr)           1.3 × 10–1 (10–3)
                                                                                               = 6.4 × 10−6 Pa ⋅ m3 ⋅ s−1
                                                                                               = 6.4 × 10−5 std cm3 ⋅ s−1
                                                                                        Subtracting the leakage rate from the total
                                                                                        rate results in the outgassing rate
                                                                                        computed as:
                              1.3 × 10–2 (10–4)
                              1.3 × 10–3 (10–5)                                                Q = 6.0 × 10−7 Pa ⋅ m3 ⋅ s−1
                                                                                                     = 6.0 × 10−6 std cm3 ⋅ s−1
       1.3 × 10–4 (10–6)                         10 20 30 40                     50                  = 4.6 × 10−6 torr - L ⋅ s−1
                                    0                   Elapsed time (h)
                                                                                        This results in outgassing computed in
(b)                                                                                     torr-L·s–1·cm–3 as:
        1.5 × 10–2 (2)                                                                         Outgassing = 4.6 × 10−6
Absolute pressure, Pa (torr)                                                                                            4.63 × 104
                                                                                                                  = 1.0 × 10−10
                                                                                        per square meter of surface area. This
                                                                                        agrees very closely with published
                                                                                        outgassing data for degreased stainless
                                                                                        steel with 200 h vacuum conditioning.
                                                 Leakage rate
                              1 × 10–2 (1.3)
                              5 × 10–3  (0.7)    After 10:50
                                              0
                                                      4 8 12 16                  20 24
                                                               Elapsed time (h)
204 Leak Testing
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PART 4. Flow Rate Tests for Measuring Leakage
Rates in Systems near Atmospheric Pressure
Principles of Leakage                         decrease during pumpdown of a leaktight
Testing by Measurement                        system.
of Flow Rates
                                                  In an alternative leak testing
The flow measurement procedure for            procedure, the sealed enclosure can be
leakage testing consists of determining the   evacuated and allowed to reach pressure
extent of leakage by measuring the rate of    equilibrium with its vacuum pumps. The
flow of gas moving into or out of the         rate at which gas is being pumped to
system or component under test. Flow          maintain this equilibrium is then
rates can be measured with a flow meter       measured to determine the rate of leakage
or by means of pumping at known               from the test volume into the enclosure.
volumetric pumping rates to maintain a
fixed system pressure or to compare rates     Pumping Technique for
of change of pressure. The flow               Measuring Leakage Rate
measurement leakage test procedure can        from Pressurized Systems
be roughly separated into two broad
classes of technique: (1) observation and     In an alternative pumping technique for
measurement of gas flow rates or volume       measuring leakage rates, the test volume
of gas displaced and (2) analysis of effects  can be pressurized and the compressor is
of pumping gas during pressurization or       then operated only sufficiently to keep
evacuation of systems, on pressure or rates   the test system pressure constant. The
of change of pressure. When leak testing      leakage rate can then be calculated from
by the flow observation technique, the        the volumetric pumping speed (m3·s–1)
amount of leakage is measured. The            and the length of time the compressor
system under test is pressurized or           must operate to regain a predetermined
evacuated and placed within a sealed          system pressure.
enclosure. The enclosure volume is
connected through a flow meter to a           Sensitivity of Flow
regulated pressure source. The gas transfer   Measurement Leak Testing
by leakage between the system under test      Techniques
and its enclosure causes a pressure
difference between the enclosure volume       The sensitivity of leakage rate testing by
and the regulated pressure source. The gas    flow measurements is relatively low,
transfer between the sealed enclosure and     compared to the sensitivity of many other
the reference pressure source is measured     leak testing techniques described in this
by flow meters, by movement of a liquid       volume. In most cases, the leakage
(slug) indicator in a capillary tube in       sensitivity depends on that of the
which the leaking gas is accumulated or
by other techniques. In some cases, the       FIGURE 28. Arrangement for leakage rate testing of system
reference pressure may be atmospheric         enclosed in a sealed test enclosure connected to a capillary
pressure. Figure 28 shows a leakage testing   tube flow meter with an opaque visible liquid indicator slug.
system using a fluid slug indicator of the    Leakage from pressurized system into enclosure would cause
amount of gas leakage.                        indicator slug to move to the right by a displacement
                                              proportional to the volume of gas leakage.
Pumping Technique for
Measuring Leakage Rate                         System                     Liquid            Connection to
from Evacuated Test                             under                    indicator        reference volume
Systems                                                                                   or pressure source
                                                  test                      slug           (or atmosphere)
In the pumping technique of leakage
testing of evacuated systems, the system      Enclosure
under test is evacuated by a vacuum
pump. The rate of system pressure                        Capillary tube
decrease during pumpdown is then
compared with the rate of pressure
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 205
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instrument used to measure the flow rate     different techniques are used to solve
and is relatively independent of the test    individual leak testing problems.
system volume. In a flow observation
technique, leakage rates between 10–3 and    Sealed Volume Technique
10–5 Pa·m3·s–1 (10–2 and 10–4 std cm3·s–1)   of Leak Testing by Flow
can be detected, depending on the flow       Measurements
instrument used. If a sealed system is
being evacuated, flow rates of the order of  Figure 28 shows the arrangement of leak
0.1 Pa·m3·s–1 (1 std cm3·s–1) may be         testing equipment using the most
observed. (Note that 1 Pa·m3·s–1 is          common technique of flow measurement
equivalent to 10 std cm3·s–1.)               by observation of the movement of fluid
                                             in a glass capillary tube. The system under
    The leakage sensitivity attainable with  test is enclosed and sealed within the test
the pumping pressure analysis technique      enclosure. The system being tested can be
depends on the size (pumping speed ) of      either evacuated or pressurized. It can
the pumps. With evacuated test objects or    either be sealed or connected to a source
test systems, leakage sensitivity depends    of pressure or of vacuum.
critically on the outgassing within the
system being measured.                           Care must be taken to ensure that the
                                             leakage being measured is not occurring
Advantages and                               in the connection to the source of
Limitations of Leak Testing                  pressure or vacuum. The capillary
by Flow Measurements                         containing the indicating fluid is attached
                                             to the test enclosure. This type of testing
Flow measurement leak testing procedures     can be performed with the capillary fluid
are applicable to a large variety of test    indicator connected between the test
systems. The procedures are useful only      enclosure and a standard testing volume
for measurement of leakage. They are not     on the other end of the capillary. In this
appropriate for locating leaks. They are     way, the leak test can be compensated for
used to measure total leakage rates in       temperature variations, if both test
small sealed parts. They can be used to      enclosure and the comparison volume are
measure total leakage rates in large sealed  subject to the same temperature
systems and in systems that can be           conditions. Alternatively, the capillary can
pressurized or evacuated. The major          be connected between the test enclosure
advantages of leak testing by means of       and the atmosphere. For accurate leakage
flow measurements are as follows.            measurements and rapid response, the
                                             enclosure containing the system under
 1. No special tracer gas is necessary. the  test should have a net volume as small as
     flow measurement leak testing           practical.
     procedure is applicable to whatever
     fluid is present within the system to       One advantage in the construction of
     be tested. The test system need not be  the sealed volume type of leak testing
     placed in any special environment for   equipment shown in Fig. 28 is that there
     leak testing. Instead, systems may be   are no critical, leaktight connections
     tested in their normal operating        within the enclosure. This is because the
     modes.                                  system is operating at atmospheric
                                             pressure. Therefore, although it is possible
 2. The cost of the equipment for flow       that a leak could exist between the
     measurement leak testing is low.        enclosure and the atmosphere, leakage
                                             does not occur through this leak because
 3. The sensitivity of overall leakage       no pressure differential is applied across it.
     measurement is independent of           Any differences in pressure are
     system volume.                          compensated for by the pressure
                                             transmission through the liquid slug
 4. The leakage rate can be measured         within the interconnecting capillary tube.
     without extensive calibration.
     However, the accuracy of leakage        Measuring Leakage Rates with Glass
     measurement is not very high, as        Capillary (Pipette) Tubes
     compared with that for many other
     techniques.                             Glass capillary tubes containing a slug of
                                             indicating fluid provide a means for direct
 5. When calibration is required, it can be  quantitative measurement of leakage rates
     readily attained with standard flow or  if a record is made of the time required
     volume measurement equipment.           for the small liquid plug to move a given
                                             distance. Because the cross sectional area
    There are two major disadvantages of     of the capillary bore is known, the
flow measurement leak testing.               volume swept out by the liquid plug
                                             during the measured time interval can be
 1. The test sensitivity is low.
 2. Flow measurement procedures have
     not gained wide recognition.
Flow measurement uses various types of
equipment with little similarity and
206 Leak Testing
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computed. A 1.5 mm (0.06 in.) diameter         4. The fluid should have a low surface
glass capillary tube is used to measure            tension so that it can be placed easily
leakage rates in the range from 10–3 to            within the bore of the capillary tube.
10–1 Pa·m3·s–1 (10–2 to 100 std cm3·s–1). A
0.5 mm (0.02 in.) glass capillary tube can    Alternative Flow
be used to measure smaller leakage rates      Measurement Instruments
from 10–5 to 10–3 Pa·m3·s–1 (10–4 to          Used in Sealed Volume
10–2 std cm3·s–1). These capillary tubes are  Leakage Tests
marked with scales given in convenient
units for computing leakage rates. A          The basic principles of sealed volume leak
stopwatch is commonly used for timing         testing can be used in numerous ways. For
the movements of the liquid plug within       large leaks, flow measuring devices such
the capillary tube. Pipettes used for liquid  as a wet type gas meter or a rotameter
measurements provide convenient               may be used. These instruments produce
calibrated capillary tubes.                   accurate leakage rate measurements but
                                              are useful only on very large leaks. For
    The upper limit on leakage rates          measurements over a wide range of
measurable with capillary tubes is reached    leakage rates, the instrument shown in
when the liquid plug moves so fast that       Fig. 29 can form a U-tube capable of
timing is difficult. The lower limit on       withstanding extremely high pressures.
leakage rate measurement is determined        Tubes B and C have different diameters so
by the accuracy desired and is influenced     that the proper tube can be selected for
by errors introduced by the resistive and     measuring various leakage rates.
inertial forces affecting the movement of
the liquid plug within the capillary tube.        When all the valves in Fig. 29 are open
Changes in atmospheric pressure               and the test components are pressurized,
(barometric readings) may move the            the liquid columns all reach the same
liquid slug in capillary systems with one     height. By closing the shutoff valve in the
end open to the earth’s atmosphere. As        main line between columns A and B,
the speed of movement of the liquid plug      leakage is indicated by upward movement
decreases, these errors are increased. This   of fluid in columns B or C. The meter in
causes the leakage measurements to            Fig. 29 was designed primarily for
become more inaccurate with slow              determining leakage rates in hydraulic
movements of the liquid plug.                 power systems. The principle of
                                              operations is to displace the leaking fluid
    Errors due to starting inertia are        with the indicating fluid. This can be
decreased with liquids of lower density.      done because there is a pressure loss in
Errors can be reduced, for example, by        the leaking component. When the meter
using a water plug about 1 mm (0.04 in.)      of Fig. 29 is installed in the hydraulic
long and timing the movement of the           power line to the component being
water plug only after it reaches a constant   tested, leakage can be measured by the
velocity. If a water plug is used, the error  displacement of the separation level
due to the resistive forces of surface        between the two different liquids in
tension can be minimized by coating the       column A as compared with column B
inside (bore) surface of the clean capillary  or C.
tubing with an organosilicon compound.
This coating acts to prevent the water            In another type of flow meter, leakage
from wetting the glass.                       flow in the line between meter and
                                              component under test is measured by the
    Mercury is almost impossible to use for
the liquid slug in a glass capillary.         FIGURE 29. Connection of delta-vee U-tube manometer for
Mercury has a very high surface tension       leakage measurements, with tubes (A,B,C) of different
and it is almost impossible to force it into  diameters.
a very small diameter capillary tube bore.
However, there should be negligible gas                           Shutoff valves
transfer through a mercury plug.
                                              Regulated pressure
    An ideal fluid for use as the indicator           source
plug in a glass capillary should have the
following characteristics.                                                                  Test system
 1. It should be a fluid in which the         A BC
     leaking gas is not soluble, so that no
     gas transfer by diffusion can occur
     through it,.
 2. The fluid should not wet the walls of
     the tube, so that the surface tension
     forces on either end of the plug are
     balanced.
 3. The fluid should be opaque for easy
     visibility and measurement of its
     position.
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 207
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displacement of a bellows. The deflection     FIGURE 30. Mass flow meter with thermal sensor that
of the pressure difference sensing bellows    measures flow through capillary tube: (a) photograph;
system varies the setting of a                (b) schematic of components of thermal mass flow
potentiometer. An output electrical signal    transducer; (c) temperature distribution under static (no-flow)
from the potentiometer indicates leakage      and flowing conditions in flow meter transducer system.
directly in volume units. This bellows
system replaces the observation of            (a)
movements of a liquid slug in a capillary
tube. Each of the preceding types of flow
meter will work with liquids as well as
with gases, provided that the indicating
liquid slug is immiscible in the fluid
whose leakage is being measured. This
versatility makes the sealed volume leak
testing techniques extremely useful for
leak testing under operational conditions.
Fast Response Thermopile                      (b) Direct current voltage source
Mass Flow Meter
                                                                                                 Heater
The flow meter (Fig. 30a) comprising a
sensor, electronic circuitry and a shunt                                         Thermocouple 1              Thermocouple 2
measures gas flow rate from 0 to
60 Pa·m3·s–1 (0 to 600 std cm3·s–1). The                                                         Meter
shunt causes the flow to divide such that
the flow through the sensor is a precise                            Heat sink                                Heat sink
percentage of the flow through the shunt.
The circuit board amplifies the sensor        (c)
output linearly to a 0 to 5 V direct current
signal proportional to the flow rate.         Tube temperature (relative units)  Zero flow
    A thermal sensor measures flow                                                               Small flow  TC-2
through a capillary tube. This flow is a                                                    TC-1
fixed percentage of the total flow through
the instrument. This sensor develops an                                          L/2 0                                       L/2
essentially linear output signal
proportional to flow, which is about                                                        Length of tube (relative units)
0.8 mV full scale magnitude (Fig. 30b).
This signal is amplified by the meter
circuitry so that the full scale output is
5.00 V direct current. The output is routed
to interface terminals and to decoding
circuitry in the display.
    Measurement of flow rates higher than
60 Pa·m3·s–1 (600 std cm3·s–1) full scale is
achieved by dividing the flow with a fixed
ratio shunting arrangement. The
measuring capillary tube is placed parallel
with one or more dimensionally similar
channels, call laminar flow elements. The
sensor only needs to heat the gas passing
through the capillary tube while retaining
all the mass measuring characteristics.
    The fast response of this instrument at
very low rates of air flow permits fast,
accurate leak testing by manual or
automatic means. Table 14 lists
multiplication factors for the air scale
meter indications when this flow meter is
used for gases other than air.
    The metal capillary tube of Fig. 30b is
heated uniformly by current from the
transformer. The temperature distribution
is symmetrical about the tube midpoint
with zero flow (Fig. 30b). The external
thermocouples TC1 and TC2 develop equal
but opposing electromotive force outputs
with a symmetrical temperature
208 Leak Testing
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distribution. When air or gas flows                                    gas composition requires only a simple
                  through the tubing, heat is transferred to                             multiplier of the air calibration to account
                  the gas and back again, creating an                                    for the differences in heat capacity. The
                  asymmetrical temperature distribution                                  flow meter can be used for a wide variety
                  (Fig. 30c). For constant power input to the                            of gases during leakage rate testing. The
                  tube, the differential thermocouple output                             full scale flow through the flow meter is
                  voltage is a function of the mass flow rate                            about 1 Pa·m3·s–1 (10 std cm3·s–1).
                  and heat capacity of the gas. Changes in
                                                                                             Figure 31 shows typical arrangements
TABLE 14. Multiplication factors for different gases of                                  for leak testing of small items. Figure 31a
mass flow meter air scale.a                                                              shows a pneumatic bridge arrangement.
                                                                                         The object to be tested and an identical,
                                                                               Relative  leaktight part used as a reference volume
                                             Conversion Densityc Specific                are charged with air at pressures up to
     Gas Symbol Factorb (g·L–1) Gravityd                                                 135 kPa (20 lbf·in.–2) gage. The effects of
                                                                                         adiabatic heating or cooling of the air
Acetylene             C2H2    0.67    1.09   0.90                                        during the pressurizing cycle should be
Air                           1.00e   1.20   1.00                                        avoided. The flow meter is then
                              0.77    0.71   0.59                                        connected between the unknown and
Ammonia               NH3     1.43e   1.66   1.38                                        reference parts to detect any evidence of
Argon                 A       0.76    3.25   2.70                                        leakage (which would allow the pressure
                              0.88    5.98   4.96                                        to decrease in the part under test).
Arsine                AsH3    0.30    2.51   2.08                                        Because the adiabatic effects are nearly
Bromine               Br2     0.34    2.40   1.99                                        identical in the reference and the test
Butane                C4H10   0.73e   1.84   1.53                                        parts, the thermopile flow meter quickly
Butene 1              C4H8    1.00e   1.17   0.97                                        detects the leakage rate without requiring
Carbon dioxide        CO2     0.85    2.98   2.47                                        a waiting period for attainment of full
Carbon monoxide       CO      0.45    3.78   3.14                                        equilibrium in temperatures and
                              0.52    1.75   1.45                                        pressures. Leakage testing may also be
Chlorine              Cl2     0.50    1.15   0.95                                        done by a direct inline leak testing
Chlorine trifluoride  ClF3    0.56    1.26   1.05                                        procedure, as sketched in Fig. 31b, but
Cyclopropane          C3H6    0.69    1.17   0.97                                        this test procedure requires a longer time
Diborane              B2H6    0.60    1.79   1.49                                        cycle than the differential flow
Ethane                C2H6    0.93    1.58   1.31                                        measurement technique.
Ethene (ethylene)     C2H4    1.43e   0.17   0.14
Ethylene oxide        C2H4O   1.03e   0.08   0.07                                        Orifice Flow Detector with
Fluorine              F2      1.01    1.48   1.23                                        Differential Pressure
Helium                He      1.00    1.53   1.27                                        Transducer
                              0.85    1.43   1.19
Hydrogen              H2      0.31    2.48   2.06                                        Figure 32a shows a leakage test
Hydrogen chloride     HCl     1.39    3.49   2.90                                        instrument system that uses an orifice to
                              0.69e   0.68   0.56                                        convert flow across the orifice element
Hydrogen fluoride HF          1.38    0.84   0.70                                        into a pressure differential sensed by the
                              1.00    1.24   1.03                                        differential capacitance sensor (see also
Hydrogen sulfide      H2S     1.02e   1.17   0.97                                        Fig. 14a). The orifice (which produces a
Isobutane             C4H10   0.75    1.85   1.54                                        pressure loss when air flows through it) is
Krypton               Kr      0.97e   1.33   1.10                                        connected in series with the air supply
                              0.15    2.83   2.35                                        line to the item under test, as shown in
Methane               CH4     0.22    3.18   2.64                                        Fig. 32). This system is used with
Neon                  Ne      0.79    1.53   1.27                                        automatic flow and leakage testers
                              0.32e   1.89   1.57                                        providing fully automatic cycling and
Nitric oxide          NO      0.36    5.93   4.92                                        accept/reject test indicators and output
                              0.36e   5.13   4.26                                        signals. Leakage sensitivity and
Nitrogen              N2      0.42    4.59   3.81                                        stabilization time are both programmable.
                              0.48    3.65   3.04
Nitrous oxide         N2O     0.43e   3.65   3.03                                            A compensation network provides a
                              0.22e   6.99   5.80                                        programmed electronic time base signal to
Oxygen                O2      0.68    1.33   1.10                                        match the dynamic characteristics of
                              0.70    2.72   2.26                                        short time cycle flow measurements.
Pentaborane           B5H9    0.28    6.43   5.34                                        Figure 32a is a photograph showing
                              0.23    8.22   6.82                                        instrument connections to the differential
n-Pentane             C5H12   0.23   14.65  12.16                                        pressure transducer (capacitance gage) and
                              0.80    0.76   0.63                                        the orifice or flow restriction element (in
Phosphine             PH3     1.37    5.54   4.60                                        this example, a short length of tubing).
                                                                                         Typical ranges vary from 0.05 to 250 L·s–1
Propane               C3H8                                                               (0.002 to 9.0 ft3·min–1). The dynamic
                                                                                         range is indicated to be 50:1 for operation
Refrigerant-11        CCl3F                                                              with laminar flow pressure loss elements.
Refrigerant-12        CCl2F
Refrigerant-13        CClF3
Refrigerant-14        CF4
Refrigerant-22        CHCIF2
Refrigerant-114       CClF2
Silane                SiH4
Sulfur dioxide        SO2
Sulfur hexafluoride SF6
Tungsten hexafluoride WF6
Uranium hexafluoride UF6
Water vapor           H2O
Xenon                 Xe
a. No corrections or compensations for temperature or pressure of gas
    required.
b. Multiply air scale by these conversion factors.
c. Density in grams per liter at 20 °C (70 °F) and 100 kPa (1 atm).
d. Specific gravity (air = 1.00).
e. Empirical data; other data is theoretical. Example: Flow meter NALL-1K,
    0–1000 std cm3·s–1 in air would be 1000 × 1.43 = 1430 std cm3·s–1 at
    full scale in helium.
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 209
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Total leakage test cycle times from 0.5 to   instantaneously in standard engineering
2 s are obtainable. The flow compensation    units and in the range selected. A self
network allows dynamic air flow              check mode provides means for verifying
measurements without requiring a             the integrity of the flow monitor both
stabilization period.                        electrically and pneumatically.
Digital Electronic Flow                      Vacuum Pumping
Meter for Monitoring                         Technique of Leak Testing
Leakage Rate Tests                           with Flow Measurements
Figure 33 shows a portable, digital          If the test system can be safely evacuated,
electronic flow meter designed for fast,     leakage can be measured directly by
accurate indication of leakage rates of      means of flow meter with vacuum
pressurized components such as valves,       pumping arrangement sketched in Fig. 34.
O-ring seals, pressure vessels, holding      The system under test is evacuated
tanks, tank cars and processing vessels. It  through an opened isolation valve
provides a broad range of flow rate          connected to the vacuum pump inlet. The
measurements up to 2 × 102 Pa·m3·s–1         exhaust gases from the vacuum pump go
(2 × 103 std cm3·s–1) with a resolution of   through a surge tank to the flow meter. A
one part in 2000. Repeatability is           bypassing valve around the pump
indicated as ±0.2 percent of full scale and  provides an alternative path between the
accuracy is ±1.0 percent of full scale       isolation valve and the surge tank. Before
values. The instrument includes a broad      performing the leak test, the vacuum
range, high accuracy solid state digital     pumping system leak tightness is first
flow indicator, combined with an integral    determined by closing the isolation valve
flow regulator and a digital pressure        and measuring the rate of gas flow
indicator. The only additional equipment     through the flow meter. If this flow is
required is a pressure source such as        negligible, the isolation valve is then
instrument air or nitrogen for tests as      opened and the flow meter readings are
pressures up to 400 kPa gage (0 to           taken only after an equilibrium (constant
60 lbf·in.–2 gage) or 700 kPa gate (0 to     flow rate) condition has been achieved.
100 lbf·in.–2 gage) and means for making
connections to the test unit. Once the           The vacuum pressure in the system
system and object under test have been       under test is adjusted by means of the
pressurized, operation is changed from       bypass valve, which controls the backflow
the charge mode to the leakage test mode.    of gas from, the exhaust port of the
The leakage rate indication is displayed     vacuum pump to its inlet port. The lower
                                             limit of vacuum pressure for which the
FIGURE 31. Arrangements for leak testing with thermopile air flow meter: (a) pneumatic bridge leakage testing arrangement
with thermopile flow meter arranged to measure difference in pressure between test object and an identical leaktight object
(reference volume); (b) inline leakage testing arrangement in which test part is pressurized, line valve is closed and leakage is
indicated by pressure drop in flow meter sensing element.
(a) Bridge arrangement
            Regulator  Valve                                      Test part
                                                                Reference part
                                             Valve  Transducer
                                             Valve
Air source
                       Flow indicator and alarm
(b) Inline arrangement
            Regulator  Valve                        Transducer
                                                                Test part
Air source
                       Flow indicator and alarm
210 Leak Testing
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vacuum pumping leak analysis technique         verify the accuracy of the leakage test
                      is useful is in the range of 3 kPa (25 torr).  results and instrumentation used in that
                      The lower limit of leak testing sensitivity    test. It also verifies the validity of the
                      is about 0.1 Pa·m3·s–1 (1 std cm3·s–1) and is  dewpoint and temperature sensor
                      mainly dependent on the availability of        locations within the containment
                      suitable flow meters for the vacuum            structure. Flow meters used in these large
                      pressure range used during the leak test.      scale leakage rate tests include thermal
                                                                     mass flow sensors, rotameters and
              Sealed Volume Flow Meter                               integrating gas flow meters usually with
              Leak Testing of Nuclear                                ranges of 25 to 700 Pa·m3·s–1 (0.5 to
              Containment Systems                                    15 std ft3·min–1). These flow meters are
                                                                     usually designed for the planned leak
                      Sealed volume leak testing techniques are      testing conditions and they produce
                      also used on large volume systems such as      readouts compensated to standard
                      nuclear containment systems. For this          pressure and temperature conditions. The
                      application, this procedure is commonly        accuracy of the flow meter must be
                      called a verification test. Its purpose is to
                                                                     FIGURE 33. Portable digital electronic flow meter for
FIGURE 32. Air flow meter with orifice and differential              monitoring leakage rates in pressurized systems.
pressure transducer: (a) photograph; (b) pneumatic circuit.
(a)
                                                                     FIGURE 34. Arrangement for vacuum pumping technique of
                                                                     leakage measurement with flow meter.
(b)        Dial         Quick
          gage       disconnect
     Air
supply                                      Pressure                         Isolation Bypass
                                           transducer
                                                                     System  valve  valve
                                                                     under
                                                                       test
                                 Out In                Test
                                                       item
          Pressure                                                                             Surge
          regulator                                                                            tank
                                 Solenoid                                    Pump                     Flow meter
                                  valves
                                              Quick
                                           disconnect
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 211
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commensurate with the accuracy of the         section of its length. Sensor coils are
leakage rate test instrumentation and also    wound around the flow tube on either
with the accuracy required in the             side of the heater coil and are connected
containment leakage rate test results.        in a bridge circuit. The zero flow, the
                                              bridge circuit is balanced and the output
Procedures for Flow Meter                     signal is zero. With flow the sensor coils
Verification Test of Nuclear                  detect the resulting temperature
Containment Systems                           difference, which is proportional to mass
                                              flow. The output electrical signal varies
The verification test is normally             linearly with the gas flow rate. Signals can
performed as the last phase of a              be used for measuring, recording or
containment test. It follows the test for     controlling gas flow rates with valves and
the system measured leakage rate Qam          an automatic controller. Sensors for
(usually given as a percentage of air mass    specific gases such as air, nitrogen,
lost in 24 h). The flow meter is installed    hydrogen, oxygen and helium are
in the system with a valve to isolate it
from the system under test. The               FIGURE 35. Thermal mass flowmeter uses a true mass flow
verification test may be performed by         sensor for measuring gas flow rates accurately: (a) sensor;
measuring either the out-leakage or the       (b) principle of operation.
in-leakage that passes through the flow
meter. For either technique, a meter valve     (a)
is placed downstream from the direction
of leakage flow through the flow meter, to    (b) To power
minimize the pressure loss across the flow
meter. After opening the isolation valve                                                    supply
between the test system and the flow
meter, this metering valve is adjusted to        Upstream                                           Downstream   Bypass sensor
produce a leakage flow through the flow       temperature                                           temperature  tube
meter from (or into) the test system that                                                           sensor
is some required percentage (usually 75 to            sensor
125 percent) of the allowable leakage rate
Qa for the system under test.                 Flow                 Bridge                           Amplifier
                                                                    for ∆T
    The leakage rate test of the                      15 to 28 V  detection                                     0 to 5 V direct
containment is then continued. After a            direct current                                                current and
period of 4 to 6 h with a minimum of ten                                                                        4 to 20 mA
sets of data, the combined leakage rate Qc
of the containment system and flow
meter and the leakage rate Q0 of the flow
meter are determined using the flow
meter readings. The difference between
these two leakage rates is Qc – Q0 = Q´am.
This difference Q´am in reading is then
compared to the leakage rate Qam
measured previously on the containment
test system alone, before the inflow or
outflow of air from the containment
through the flow meter. The two values
must agree with 25 percent of the
measured containment leakage rate Qam.
This is to say that Qam – Qam must be
equal to or smaller than 0.25 Qam.
True Thermal Mass Flow
Meters for Accurate Flow
Rate Measurements
The containment verification test just
described requires a true mass flow meter
that measures the mass of gas that passes
through it. Figure 35 shows a true mass
flow sensor element which does not
require temperature or pressure
compensation and provides ±1 percent of
full scale accuracy and linearity. The
sensor unit has a stainless steel flow tube.
A heater coil is wound around the center
212 Leak Testing
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available with ranges from 0 to 0.015 up
                       to 0 to 10 Pa·m3·s–1 (0 to 10 up to 0 to
                       5 × 103 std cm3·min–1). Repeatability of
                       indications is claimed as ±0.2 percent of
                       full scale. Output signals from the thermal
                       mass flow sensors of Fig. 35 can actuate
                       indicating meters or provide 0 to 5 V
                       direct current signals that can be
                       transmitted up to 300 m (1000 ft) to
                       recording instruments, digital indicators
                       or controllers. The electrical output signal
                       is linearly proportional to the mass flow
                       rate through the sensor.
               Flow Meter Tests to Locate
               Leaks in Gas Filled Electric
               Power Cables
                       Electric utility companies have made use
                       of a U-tube manometer equipped with
                       appropriate valving to use as a flow meter
                       for locating gas leaks in gas pressurized
                       electric power cable sheaths. When the
                       manometer is installed in a segment of
                       the pressurized gas filled cable sheathing,
                       oil will rise in the glass tube of the
                       manometer, on the side closer to the leak.
                       In this test, the manometer measures the
                       pressure loss in the segment of cable
                       across which it is connected, when gas
                       flows toward the leak.
                                                             Pressure Change and Flow Rate Techniques for Determining Leakage Rates 213
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References
                       1. CRC Handbook of Chemistry and
                           Physics. Cleveland, OH: Chemical
                           Rubber Company (1964).
                       2. Fleshood, D.L. “Containment Leak
                           Rate Testing: Why the Mass-Plot
                           Analysis Method Is Preferred.” Power
                           Engineering. Barrington, IL: Technical
                           Publishing Company (February 1976):
                           p 56-59.
                       3. Lau, L.W. “Data Analysis during
                           Containment Leak Rate Test.” Power
                           Engineering. Barrington, IL: Technical
                           Publishing Company (February 1978):
                           p 46-49.
                       4. Kendall, M.G. and A. Stuart. The
                           Advanced Theory of Statistics, third
                           edition. Vol. 2. New York, NY: Hafner
                           Publishing Company: p 130-132.
                       5. Tietjen, G.L., R.H. Moore and R.J.
                           Beckman. “Testing for a Single Outlier
                           in Simple Linear Regression.”
                           Technometrics. Vol. 15, No. 4.
                           Alexandria, VA: American Statistical
                           Association (November 1973):
                           p 717-721.
                       6. ANSI/ANS-56.8-1981, Containment
                           System Leakage Testing Requirements,
                           Appendix C. La Grange Park, IL:
                           American Nuclear Society (1981).
                       7. Guthrie, A. Vacuum Technology. New
                           York, NY: John Wiley and Sons (1963).
                           Reprint, Malabar, FL: Krieger
                           Publishing (1990).
                       8. Steinherz, H.A. Handbook of High
                           Vacuum Engineering. New York, NY:
                           Reinhold Publishing Corporation
                           (1963).
 214 Leak Testing
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6
                                                                   CHAPTER
                    Leak Testing of Vacuum
                                             Systems
                                                             Charles N. Sherlock, Willis, Texas
                                                             Carl A. Waterstrat, Varian Vacuum, Lexington, Massachusetts
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PART 1. The Nature of Vacuum
Definition of a Vacuum                         and computer chip manufacturing,
                                               vacuum is used in magnetrons, cathode
The word vacuum is derived from the            ray tubes, television picture tubes,
Greek word meaning empty. In practice,         semiconductor devices, solar cells, plating
use is made of some type of vessel             metals and plastics, thin film deposition,
(vacuum enclosure, chamber or container)       lifting objects, plasma physics, cryogenics,
to contain a vacuum. When the enclosure        metallurgical processing, electron beam
is closed to the surrounding atmosphere        welding, brazing, distillation organic
and air or gas is removed by some              chemistry, packaging, mass spectrometry,
pumping means, a vacuum is obtained.           space simulation and leak detection.
Various degrees of vacuum can be               Many other areas find application for
obtained, depending on how much air is         vacuum equipment.
removed from the enclosure. Common
terms such as partial vacuum, rough            Changes in Pressure Units
vacuum, high vacuum and ultrahigh              Used for Vacuum
vacuum are used to describe degrees of         Measurements
vacuum. A vacuum is any pressure below
the prevailing atmospheric pressure.           The presently preferred SI unit for
Practically speaking, a vacuum such that       pressure is the pascal (Pa). The standard
the containing vessel is empty, i.e., free of  atmospheric pressure at sea level and 0 °C
all matter (molecules), is never obtained.     (32 °F) is equal to 101.325 kPa. Earlier
If this were possible, the vacuum would        units used for pressure in vacuum relate
be called a perfect or absolute vacuum.        to atmospheric pressure indicated by the
                                               height (nearly 760 mm) of the mercury
Applications of Vacuum                         barometer column at sea level and 0 °C
Environments                                   (32 °F). The unit known as the torr was
                                               defined as 1/760th of the pressure of the
Vacuum is used to reduce the interaction       mercury column. The torr was named in
of gases or air with solids and to provide     honor of an Italian physicist, Evangelista
control over electrons and ions by             Torricelli (1608-1647), inventor of the
reducing the probability of collision with     mercury barometer. The torr is almost
molecules of air. Vacuum pumps are used        identical to the millimeter of mercury
by industry and laboratories to create a       (mm Hg), because there are 759.96 torr in
vacuum environment for these                   a standard atmosphere. The difference
operations. Most gases react with solids to    between the two units amounts to so little
cause effects such as oxidation, which it      that torr and mm Hg have been used
may be necessary to avoid. In a vacuum         interchangeably.
environment, the necessary operation
may be performed so that undesirable           Variation of Atmospheric
effects are reduced or eliminated. For         Pressure with Altitude
example, unless most of the air is
removed from an incandescent light bulb,       The mercury barometer is a device for
oxygen in its atmosphere will react with       measuring atmospheric pressure. As the
the hot tungsten filament, causing it to       altitude increases, the pressure decreases
burn out prematurely. An electron tube         because fewer gas molecules press on any
could not operate at atmospheric pressure.     surface. A knowledge of how the pressure
Electron flow would be impeded by              changes with altitude is very important in
collision with air molecules due to the        connection with various space studies.
extremely small mean free path. In             Table 1 shows the relationship between
addition, elements within the tube may         pressure and altitude in the earth’s
react with the air. Other examples can be      atmosphere.
cited where vacuum is necessary to
produce desired results that could be              At an altitude of 50 km (27 mi) the
unattainable in any other way.                 pressure is about 0.1 percent of standard
                                               atmospheric pressure or 100 Pa
    Vacuum is required in many industries      (0.015 lbf·in.–2). Air at this altitude
and products. In addition to light bulbs
216 Leak Testing
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contains one thousandth of the number                   ability of a gas to diffuse increases when
                  of molecules per unit volume in air at sea              its pressure is reduced. Consider the
                  level. At 400 km (250 mi) altitude, the                 example of ammonia vapor being released
                  pressure is in the range of 1 µPa or 10–11              in a room. The reason that it is not
                  parts of sea level pressure. Table 2 gives a            detected immediately at the other end of
                  relative measure of gas characteristics at sea          the room is that the path each ammonia
                  level and at 1 nPa (10 ptorr). Compared                 molecule takes is restricted by the air
                  with the number of molecules in a cubic                 molecules with which it collides. It is only
                  centimeter at atmospheric pressure, it is               after many billions of collisions with air
                  seen that there are one hundred                         molecules that the ammonia molecules
                  thousandth of one millionth as many                     finally make their way across the room. If
                  molecules at 10–6 Pa (1.5 × 10–10 lbf·in.–2).           the room were pumped down a high
                  However, a tremendous number of                         vacuum, there would be many fewer air
                  molecules (3 × 108) still remain in a cubic             molecules and far fewer collisions to
                  centimeter at a pressure of 1 µPa (10 ntorr).           impede the path of the ammonia
                  Pressures around 1 µPa (10 ntorr) are not               molecules. Thus, an ammonia molecule in
                  uncommon in good vacuum systems.                        a high vacuum takes less time to complete
                                                                          its trip across a given distance than in
                  Diffusion and Adsorption                                gases at higher pressures.
                  of Gases in Vacuum
                  Systems                                                     Only those molecules that are in
                                                                          motion within a vacuum chamber create a
                  The kinetic molecular theory of gases and               pressure through collisions with its walls.
                  the ideal gas laws (Boyle’s, Charles’,                  A molecule that is adsorbed to the wall
                  Dalton’s and the general gas law), are                  surface is stationary and does not produce
                  applicable to vacuums. In vacuum, fewer                 collisions. Therefore, adsorbed gas
                  molecules are dealt with, but their basic               molecules do not contribute to the total
                  behavior is predictable by the molecular                pressure. However, molecules adsorbed on
                  theory of gases and does not change. The                surfaces can be returned to the gas phase
                                                                          by thermal agitation produced by the
TABLE 1. Change in atmospheric pressure with altitude.                    application of heat. Thus, outgassing
                                                                          effects can contribute to pressure in an
____A__lt_it_u_d__e____ _________P_r_e_s_s_u_r_e_________                 evacuated system, because a molecule can
                                                                          undergo repeated collisions and exert
km (mi)           kPa             (atm)                    Remarks        pressure only when it is in the gaseous
                                                                          state.
     0     (0.6)  101.325              (1.00)              international
           (1.2)                                            standard      Mean Free Path of Gases
     1     (3.1)   89.90              (0.887)                             in Vacuum Systems
     2     (6.2)   79.50              (0.785)              jetliner
     5             54.00              (0.533)               altitude      At normal atmospheric pressure, gas
   10    (12.4)    26.50              (0.262)                             molecules make many collisions with
         (31.1)                                            low orbit      each other. The average distance that a
   20    (62)        5.53             (0.055)                             molecule travels before colliding with
   50   (124)        7.98 × 10–2   (7.9 × 10–4)                           another molecule is known as the mean
 100    (311)        3.2 × 10–5    (3.2 × 10–7)                           free path. The mean free path of two
 200    (621)        8.5 × 10–8   (8.39 × 10–10)                          different gases at the same pressure will
 500                 3.0 × 10–10    (3 × 10–12)                           not be the same; this is because the mean
1000                 7.5 × 10–12  (7.4 × 10–14)                           free path depends on the molecular size,
                                                                          which varies from one gas to another. In
                                                                          spite of this fact, it is still possible to give
                                                                          a useful relationship between mean free
                                                                          path and pressure. The approximate
                                                                          values of mean free paths for air and
TABLE 2. Comparison of atmospheric properties at sea level and at high altitude.
                  Condition                                               At Sea Level               At 400 km (250 mi) Altitude
Pressure                                                                    101.325 kPa (760 torr)            1 µPa (10 ntorr)
Number of molecules in 1 cm3 (0.06 in.3)                                            2.7 × 1019                      3 × 108
Mean free path
Time to form a monolayer of adsorbed gas on a clean surface                  93 nm (3.7 × 10–6 in.)            9.3 km (5.8 mi)
Average speed of nitrogen molecule at room temperature 20 °C (68 °F)                   >10 ns                        120 s
                                                                          1600 km·h–1 (1000 mi·h–1)    1600 km·h–1 (1000 mi·h–1)
                                                                                                                      Leak Testing of Vacuum Systems 217
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other gases are given as a function of gas    flow. The motion of a particular molecule
pressure in Eq. 1:                            is entirely random and unpredictable; it is
                                              as likely to move in one direction as in
                    0.0095                    any other direction. To a molecule, tube
(1) λ =                                       wall appear very rough and irregular. The
                                              direction of molecule rebound after
                        P                     impact with the tube wall thus tends to
                                              be independent of the direction of
where λ is mean free path (meter) and P is    incidence. (This is an over simplified
gas absolute pressure (pascal).               description.) Figure 1 is a sketch of
                                              particle motions during molecular flow of
Effects of Molecular Friction and             gases through a tube. Note that not all of
Gas Viscosity in Viscous Flow                 the molecules entering at the left exit at
                                              the right. The gas flow will continue as a
As shown by Eq. 1, the mean free path         net movement to the right only as long as
length varies inversely with absolute         there is some driving force causing
gaseous pressure. The concept of mean         movement from left to right. As gas
free path is useful in describing vacuum      concentration gradient is such a force. A
ranges. The mean free path at                 pressure differential is another force that
atmospheric pressure is very short (see       can control the direction of net flow of a
Table 2), due to the large molecular          gas. Both can contribute to flow of a
density. Therefore, collisions occur much     tracer gas through a leak.
more frequently between gas molecules
than between molecules and the walls of       Specifying Gas Flow Rates
the container. Thus, the gas acts much
like a fluid. Under a pressure differential   The flow rate of liquids is expressed
this gaseous fluid moves as a unit and is     simply as so many volume units per unit
considered to flow. The molecules, while      time, such as liters per second. When,
drifting slowly in the direction of flow,     however, the flow rate of gases is
move rapidly along random paths. Any          considered, it is necessary to know not
resistance to this flow is due to the         only the volume of a gas but its pressure
viscous properties of the gas. The term       and temperature as well. A cubic meter
viscous refers to molecular friction and is   volume of gas at 100 kPa (15 lbf·in.–2)
used to describe the flow characteristics of  pressure and a temperature of 20 °C
a fluid. Water, for example, is less viscous  (68 °F) will contain ten times as many
than syrup because it flows or pours more     molecules as a cubic meter volume of gas
easily. The cross sectional dimension of      at 10 kPa (1.5 lbf·in.–2) and 20 °C (68 °F).
the container or tube through which the       Only a complete statement of volume,
gas flows is important because it             displacement rate, gas pressure and
determines the velocity of the molecules      temperature can accurately describe the
within the flowing gas. The viscous           total quantity of gas that flows per unit of
properties of the gas are functions of the    time. In both liquids and gases, it is mass
gas viscosity and the gas velocity. When      flow that is of interest. For liquids of
viscous properties control gas flow rates,    constant density, the mass rate of flow is
the situation is termed viscous flow.         directly proportional to volume flow rate.
                                              With gases, density varies both with
Effects of Mean Free Path and                 temperature and with pressure. Thus, for a
Flow Cross Section on Molecular               given gas, volume displacement rate,
Flow of Gas                                   pressure and temperature must be known
                                              to define the mass flow rate.
As the pressure of the gas within a system
is reduced, the mean free path of the         FIGURE 1. Molecular motion along a tube, with particle mean
molecules increases and the flow              free path far larger than tube diameter.
characteristics change gradually. As the
mean free path becomes comparable to             3                                          1
the cross sectional dimensions of the                                                           5
tube, collisions occur less frequently          2
between molecules and the apparent              4                                            3
viscosity of the gas decreases. Under these
conditions, the event that is most likely       2
to affect the direction of the molecules;     5
travel is a molecular collision with the      41
tube wall. As the pressure is further
reduced, the mean free path becomes
greater than the tube’s cross sectional
dimensions. The diameter of the tube
alone then determines the resistance to
flow; this situation is called molecular
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The Concepts of Gas                           By combining Eqs. 2 and 3, the product of
Quantity and Pumping                          pumping speed S and gas pressure P can
Speed                                         be equated to throughput by Eq. 4:
From the gas laws, it is known that the       (4) Q = S × P
product PV of pressure P and volume V is
proportional to the number of molecules       Equation 4 is the universal relationship
in a sample of gas. In static systems, the    on which vacuum pumping throughput
PV product is constant at a given             calculations are based. As an example of
temperature. This product PV is known as      its use, suppose the gas in the pipe
the quantity of gas. Common units of gas      between Sections 1 and 2 of Fig. 2 passes
quantity include torr liter (torr-L); the     Section 1 in 1 s and this volume V is
atmospheric cubic centimeter (cm3 of          100 L (0.1 m3) and pressure P at Section 1
volume at standard sea level atmospheric      is 10–4 Pa and displaced volume V =
pressure or std cm3); and the bar liter       0.1 m3, divided by the time t = 1 s:
(bar-L). The preferred SI unit of gas
quantity is the pascal cubic meter (Pa·m3).           Q = S × P = PV
                                                                                       t
    In steady flow, the same quantity of
gas (number of molecules) that enters one                   = 10−4 × 0.1 = 10−5
end of a tube must leave at the other end,
even though there may be different            Comparison of Gas Flow with
volumes of gas entering and leaving per       Liquid Flow
unit time. If the PV product is used as a
measure of the amount of gas flowing          Before attempting a more thorough
through a tube, computation may be            discussion of gas flow, it may be helpful
done with a minimum of complication.          to compare gas flow with water flow. To
                                              get any fluid to flow within a pipe, a
    The volumetric pumping speed S is the     pressure differential must be established
time rate of volume displacement, as          between the two sections across which
given by Eq. 2:                               the fluid is to flow. (Gravitational effects
                                              are neglected in this introductory
(2) S = V                                     discussion.) The fluid would then flow
                     t                        from the high pressure region P1 to the
                                              low pressure region P2. Consider a closed
    Typical units of pumping speed S          system of pipes through which water is
would be cubic meter per minute               circulated as in an automobile. The water
(m3·min–1), cubic meter per second            pump creates the pressure differential
(m3·s–1), liter per second (L·s–1) and cubic  necessary for water to flow. Across each
foot per second (ft3·s–1).                    component (radiator, engine block,
                                              thermostat, different sizes of piping) in
Concepts of Throughput                        the system, the pressure drops. The sum
and Leakage Rate                              of all these pressure drops equals the
                                              pressure differential across the water
In vacuum practice, the preferred             pump. The magnitude of the pressure
description of the rate of flow of gas is     drop across each component of the
commonly called throughput.                   system depends on its physical geometry.
Throughput is the quantity of gas or a        Clearly, a smaller diameter pipe will result
measure of the total number of molecules      in decreased flow for the same size pump.
at a specified temperature, passing an        similarly, increasing the length of the pipe
open section of the vacuum system per         will reduce the flow, whereas decreasing
unit time. Leakage rate is a similar          the length of the pipe will increase the
measure of the total number of molecules      flow. Shorter lengths and larger diameters
at a specified temperature passing through    reduce the resistance to flow through the
a leak per unit time. Q is the symbol         pipe.
commonly used for gas throughput per
unit time, in pascal cubic centimeter per     Analogy of Gas Flow to Electric
second:                                       Current through Resistance
(3) Q = PV                                    The analogy may be carried further by
                      t                       comparing the gas flow system to an
                                              electrical circuit. Given an electrical
                                              circuit with a battery and a resistor in
                                              series with it, the battery may be
                                              considered to be the pump and the
                                              resistor the pipe. Increasing or decreasing
                                              the resistance decreases or increases the
                                              current flow (analogous to gas flow),
                                                                                                                      Leak Testing of Vacuum Systems 219
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respectively. If the circuit consists of a             In an electrical circuit, the voltage drop
           series of resistors and a battery, the sum of          across a resistor is the product of the
           the voltage drops across each of the                   current and resistance. In a vacuum
           resistors (pressure drops) is equal to the             circuit, the pressure differential across a
           total voltage generated by the battery                 pipe is the product of throughput (gas
           (pressure differential created by the                  flow) Q and resistance R. Equation 5 states
           pump). The voltage drop across each                    this relation mathematically for the
           resistor will depend on the magnitude of               pressure differential ∆P:
           resistance of that component. The larger
           the resistance, the larger the voltage drop            (5) ∆ P     =  P1 – P2  = Q×R      =  Q
           (see Fig. 3).                                                                                C
           Gas Conductance and Its Electrical                     Because R is equal to 1/C, Eq. 5 may be
           Analogy                                                written in the form of Eq. 6 for gas
                                                                  conductance C:
           In vacuum, one speaks not of the
           resistance a tube or component offers to               (6) C = Q
           gas flow, but instead uses the reciprocal                                   ∆P
           term conductance. Conductance is a
           measure of the ability of a vacuum                     Equation 6 is the defining equation for
           component to permit gas flow or not to                 gas conductance: the ratio of throughput
           impede it. Consequently, the greater the               Q to pressure differential ∆P across the
           resistance, the smaller the conductance                conductance.
           and vice versa. Figure 3 shows the
           electrical analogy of a tube in a vacuum               Gas Conductance with
           system. The battery is analogous to the                Sequential Tubes of
           vacuum pump, current is analogous to gas               Passages
           flow and the resistor is analogous to pipe.
FIGURE 2. Rate of flow of a gas Q through tube with applied       If two different diameter pipes with
                                                                  different conductance values are
pressure differential ∆P = P1 – P2 (P1>P2). (See analogous        connected in series as in Fig. 4a, the total
electric circuit of Fig. 3.)                                      conductance of the connection between
                                                                  extreme ends decreases (resistance
            Section 2                         Section 1           increases). From Eq. 6, the conductance of
                                                      P1          the pipe between Sections 1 and 3 may be
            P2                                                    expressed as in Eq. 7:
To vacuum
                       Tube conductance = C                       (7) C13 =          Q
      pump               Tube resistance = R                                     P1 − P3
                                                     From vacuum
                                                     chamber
                       Gas flow rate                              ( ) ( )(8) P1 − P3 = P1 − P2 + P2 − P3
                       Gas flow rate Q = (P1 – P2)C               (9) P1 − P2 =     Q
                                                                                   C12
                                                                  or
           Pressure differential ∆P = P1 – P2 = QR = Q/C                                 Q
                                                                                        C 23
                                                                        P2 − P3 =
FIGURE 3. Electrical analogy of vacuum pumping pipe               Now, by combining Eqs. 7, 8 and 9, the
conductance system of Fig. 2. G is the electrical                 relationship for C13 becomes:
conductance, the reciprocal of electrical resistance R, so that
G = 1/R. ER = Eb – EL = E1 – E2 = IR = I/G.                       (10) C13 =             Q
                                                                                  Q +Q
                                       R = 1/G                                   C12 C23
                                                                  or, in its reciprocal form:
        –              i                                                   1     Q +Q
Eb                                                   EL Load                     = C12         C 23
                                                                  (11)
        +                                                               C13 Q
                                                                                 = 1+1
                                                                                      C12 C23
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In its general form, Eq. 11 may be written        division is not equal but depends on the
              as Eq. 12:                                        conductance of each component. From
                                                                Eq. 6, the gas load in each parallel pipe
              (12) I = 1 + 1                                    may be written in the form of Eq. 14:
                       CT C1 C2
                              + 1 +…+ 1                         (14) QA = CA × ∆ P
                                   C3 Cn                        and
              In Eq. 12, the subscript T denotes the            Qb = Cb × ∆P
              total conductance of a number of
              conductances C1, C2, C3 ... Cn connected          The total conductance between points 1
              in series.                                        and 2 is
                  In the case of only two conductances          (15) C12 =                   Qa + Q b
              connected in series (Fig. 4b), Eq. 12                                               ∆P
              should be written in the form of Eq. 13:
                                   C1 × C2                      Substituting from Eq. 14, Eq. 15 gives:
                                   C1 + C2
              (13) CT           =                               (16) C12      =              Ca ∆P + Cb ∆P
                                                                                                      ∆P
              This case is analogous to the special case        Simplifying, Eq. 16 becomes:
              of two electrical resistors connected in
              parallel.                                         (17) C12 = Ca + C b
              Gas Conductance for Pipes                         In its general form, the total conductance
              or Tubes Connected in                             for a number of pipes connected in
              Parallel                                          parallel is equal to the sum of the
                                                                individual conductances, as given by
              Figure 5 shows two lengths of pipe                Eq. 18:
              connected in parallel. In this connection,
              the total gas load (throughput) flowing           (18) CT = C1 + C2 + C3 + … + Cn
              from the vacuum chamber divides
              between the two pipes as shown. The               FIGURE 5. Electrical analogy of two gas conductances in
                                                                parallel: (a) connection of two parallel gas conductances;
FIGURE 4. Electrical relationship of two conductances in        (b) electrical circuit analogous to two gas conductances in
series: (a) pipe conductances in series; (b) connection of two  parallel.
electrical resistances.
                                                                (a)                                                                P1
                                                                                                       Ca
                                                                                         P2
(a)                                P2          P1                                                      Qa Pipe 1
                                                                                                       Cb
                To P3   C23            C12                      To turbomolecular
       turbomolecular                                           or diffusion pump                        Qb Pipe 2
          or diffusion                                              QT = Qa + Qb
             pump
                          Q              Q     Vacuum                                                                                  From
                        Pipe 2         Pipe 1  chamber                                                                                 vacuum
                                                                                                                                       chamber
—1 = —1 + —1
C13 C12 C23
(b)                     R2 R1                                   (b)                                    R1
                             I                                     EB –                                         I1
                                                                (pump)                                 R2
   EB   –                                      Load
(pump)  +                                                                  +                                    I2
                                       EL      (vacuum                                                                           Load
                                               chamber)                                                             EL (vacuum
                                                                                             EB
                                                                                                                              chamber)
                                                                                                                      Leak Testing of Vacuum Systems 221
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Pumping Speed                                         throughput Q is the product of the speed
                                                              S and pressure P where each is measured
        In operating a vacuum system, there is an             at the same point, such as at the pump or
        interest in how fast gases are removed                chamber. Throughput at the pump is
        from the system. The rate of removal of               therefore expressed as Eq. 21:
        gases is measured by pumping speed S.
        From Eq. 4, pumping speed is defined as               (21) Q p = S p Pp
        the ratio of the throughput Q to the
        pressure P at the point in the system.                and pressure as:
        Mathematically, this relation is given by
        Eq. 19 (m3·s–1):                                      Pp            =   Q
                                                                                Sp
        (19) S = Q
                            P
        If the inlet to a vacuum pump were                    At the chamber being evacuated,
        connected directly to a vacuum vessel,                throughput is expressed as:
        then the pumping speed at the vessel
        would be the same as that at the pump                 (22) Qc = Sc Pc
        inlet. Because it is physically impossible to         and pressure as:
        join the pump and vessel without
        introducing a connector the pumping                   Pc =             Q
        speed at the vessel will be lower than that                            Sc
        at the pump. Pumping speed loss depends
        on the magnitude of the conductance                   Substituting Eqs. 21 and 22 into Eq. 20
        that causes a loss in pressure or creates             results in the relation of Eq. 23:
        differential pressure between pumps and
        vessel. Figure 6 is used to help establish a                    Q      –Q        =Q
        relationship between the net pumping                  (23) Sc                Sp        C
        speed at the vacuum chamber, pumping
        speed at the port of a vacuum pump and                Rearranging terms:
        the conductance between them. Although
        the connection is shown as a pipe in                            Q      =Q        +Q
        Fig. 6, it could be a combination of any              (24)                   Sp       C
        number of vacuum components, each
        contributing a value of conductance. The                        Sc
        flow of gas is from the chamber to the
        pump. From Eq. 5, the pressure drop is                and multiplying by 1/Q:
        given by Eq. 20:
        (20) ∆ P = Pc − Pp  =           Q                     (25) 1 = 1 + 1
                                        C                               Sc S p C
        In Eq. 20, the subscripts c and p refer to            In the general case, the net speed Sn at
        the chamber and pump, respectively. The               any point in a vacuum system is related
FIGURE 6. Net pumping speed relationship applicable to        to the pump speed Sp and the total
                                                              conductance Ct between that system point
conductance C between vacuum pump and chamber being           and the vacuum pump by Eq. 26:
evacuated. Pressure at vacuum chamber (inlet to               (26) 1 = 1 + 1
                                                                        Sn S p Ct
conductance C ) is Pc , and pumping speed Sc = Q/Pc.
Pressure at vacuum pump (outlet of conductance C) is Pp       Analysis of Eq. 25 shows that, except for
and pumping speed is Sp = Q/Pp. Because vacuum pump           the case of an infinite conductance (zero
pressure Pp is lower than chamber pressure Pc , whereas Q is  resistance), the net speed will always be
the same at each end of conductance C, the pumping speed      less than the pump speed. How much less
                                                              depends on the value of the tube
is different at inlet and outlet of C.                        conductance.
Diffusion   C
 pump                             Vacuum
                                  chamber
S—n  =  Qn  Q               Qc  =  —Sc
Pn                                 Pc
Sp   =  —Q                  Sc  =  —Q
        Pp                         Pc
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PART 2. Principles of Operation of Vacuum
Systems and Components
                                             atomic mass unit (u); and T is the
Introduction to Vacuum                       absolute temperature of gas within the
Pumping
                                             evacuated container (kelvin). A similar
To attain vacuum in a container, some
means of pumping must be used. A pump        expression can be given for a mass of gas
cannot reach into the system and extract
molecules, but must simply wait for          (kilogram) striking a unit area (square
molecules to wander through the natural
exit in the container and into the pump      meter) of the evacuated container wall per
for isolation and discharge. When the
pressure in the vacuum system becomes        unit time (second):
so low that there is no longer a net
movement of molecules into the pump,         ( )R’ = 43.8 × 10−4  P
the base pressure of the system has been
reached under those conditions. How low                           MT
this ultimate pressure is will be
determined by conditions such as (1) the     where R is rate of gas mass impact with
leak tightness of the vacuum system,         wall (kg·m–2.s–2); P is absolute pressure
(2) the nature and condition of materials    within evacuated chamber (pascal); M is
within the vacuum system that might          molecular weight of gaseous particles, in
cause outgassing and (3) the operating       unified atomic mass unit (u); and T is
characteristics of the pumps in              absolute temperature of gas within
combination with the specific vacuum         evacuated container (kelvin).
system.
                                                 If a hole of unit area were cut through
Molecular Conditions                         the container wall, those gas molecules
Limiting Rates of Pumping                    that would have collided with the
of Vacuum Systems                            container wall in the area of the hole and
                                             rebounded within the container will now
To evacuate a closed system initially at     pass through the hole at the rate given by
atmospheric pressure, numerous gaseous       Eq. 27a. If these escaping gas molecules
molecules must be removed from within        are now prevented from reentering the
the closed system. The fewer the gas         container through that hole, the net effect
molecules remaining, the lower the           would be that of reducing the number of
absolute pressure of gas within the          molecules within the container and thus
system. However, the common concept          reducing the internal gas pressure. This is
that vacuum pumps draw out the air like      the basic concept of vacuum pumping,
a vacuum cleaner is wrong. Molecules in      namely, to provide a natural exit for gas
the gaseous phase are in constant motion     molecules and to isolate the escaping gas
and collide with each other and with the     molecules so that they cannot reenter the
walls of the container. A certain number R   container being evacuated. The vacuum
of molecules strike each unit area of the    pump cannot extract gas molecules from
container wall per unit time. The number     within the evacuated container; it merely
of gaseous molecules striking a unit area    aids those molecules that pass through
(square meter) of the container wall per     the hole in the wall to naturally escape
unit time (second) is given by Eq. 27:       being reinjected into the vacuum
                                             container through that same hole. It is
                                             impossible to pump any gas out of an
                                             evacuated container at any rate faster
                                             than that at which internal gas molecules
                                             strike the hole area by their random
                                             kinetic motions.
( )(27) R = 2.63 × 1024  P                   Example of Limitations on Vacuum
                                             Pumping of Gaseous Nitrogen
                         MT
                                             For gaseous nitrogen with a molecular
where R is rate of molecular impact with     weight M = 28 at room temperature,
the wall in molecules per square meter per   298 K (25 °C or 77 °F) and atmospheric
second; P is absolute pressure in evacuated  pressure, 101 kPa (1 atm), Eq. 27a
chamber (pascal); M is the molecular         indicates that the number of molecules
weight of gaseous particles, in unified      striking each square meter of container
                                             wall during each second would be
                                             calculated as:
                                                                                                                      Leak Testing of Vacuum Systems 223
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R=  ( )2.63 × 1024 × 101 000                 Operation of Mechanical
                                             Pumps for Vacuum
                28 × 298                     Systems
= 2.92 × 1027                                The mechanical pump is an essential
                                             component used in vacuum systems to
Similarly, if the mass (kilogram) of         evacuate a chamber from atmospheric
nitrogen gas striking the unit area (square  pressure to about 0.1 Pa (10–3 torr)
meter) per second were to be determined,     absolute pressure. Of the various types of
Eq. 27b indicates that this mass would be:   mechanical pumps, the rotary oil sealed
                                             vacuum pump shown in Fig. 7 is most
    ( )R’ = 43.8 × 10−4 × 101 000            common. The pump consists of a
                                             stationary housing, an eccentrically
× 28                                         mounted rotor with two spring loaded
        298                                  vanes, an inlet port and a discharge port.
                                             Air enters the pump from the vacuum
= 136                                        chamber through the inlet port. This air is
                                             trapped, compressed and ejected into the
The volume flow rate corresponding to        atmosphere through the discharge port by
                                             means of the rotor arrangement. Sealing
the above mass flow rate would be equal      of the eccentric rotor vacuum pump is
to 136 × 0.8714 = 118 m3·s–1·m–2             done by an oil film between the two
(7.08 × 103 ft3·min–1·ft2).                  sliding spring loaded vanes that make
                                             contact between the rotor and the
    For the case of molecular nitrogen (N2)  housing. Oil is used as the pump sealant.
at 298 K (77 °F) and atmospheric pressure,   Close tolerances must be maintained to
the conversion factor is 0.8714 m3·kg–1.     prevent leaks and by passing of gases.
                                             Consequently, care must be taken to
Thus, for gaseous nitrogen molecules         prevent solid particles from entering the
                                             pump. Each rotation of the rotor
(each of which contains two nitrogen         discharges two volumes; each volume is a
                                             certain percentage of the volume to be
atoms), the volumetric rate of exit of gas   evacuated. This would indicate that even
                                             a perfect pump could never evacuate to a
through a hole in the evacuated container    vacuum linearly but could only approach
would be 118 m3·s–1·m2 or 11.8 L·s–1·cm2     this condition as an exponential function
(7.08 × 103 ft3·min–1·ft2). This is the      of pumping time.
maximum rate at which nitrogen can be
                                             FIGURE 7. Rotary mechanical vacuum pump with eccentric
pumped from a container whose internal       rotor and spring loaded vanes. Pump oil provides a sealing
                                             film at points of vane contact with stator housing.
pressure was 101 kPa (1 atm). As system
pressure decreases, the molecular or mass
rate of pumping drops proportionally.
Conditions Limiting Rate                     Outlet                         Inlet
of Pressure Reduction by                                           Oil
Pumping                                              Rotor
Pumping times greater than expected for                      Vane
reduction of pressure to desired levels can
result from system contamination or                  Spring
system leaks. System contamination can
be caused by processing of so-called dirty                         Housing
work materials or by allowing excessive
time without thorough cleaning of the
vacuum equipment. Contamination of
this type results in many layers of various
compounds, organic or otherwise, which
build up on interior surfaces. The
contaminated surfaces then outgas at such
rates that the pump capacity may be
unable to reduce pressure to desired levels
within acceptable pumping times. Water
vapor adsorbed to chamber walls is a
common contaminant. Dirty walls are
subject to more severe water adsorption. It
is also possible for mechanical pump oil
to become contaminated, which alone
can cause poor pumping characteristics.
    If pumping is slowed by system leaks,
thorough mass spectrometer leak
detection tests inspection should be
performed and leaks repaired.
224 Leak Testing
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At low chamber pressures, air may leak   closed because there is usually very little
back into the evacuated volume. This can     water vapor present. The minimum
be minimized by putting two pumps in         pressure obtainable is also slightly higher
series so that the discharge from the first  with the ballast valve open. (Because of
pump chamber is not directly to              the higher pressure in the chamber during
atmosphere but to some intermediate          compression with the ballast valve open,
pressure maintained by the second (or        there is more leakage back into the
backing) pump.                               vacuum system.) Some pump
                                             manufacturers recommend operating the
Pump Oil Used in Rotary Vacuum               pumps with the ballast valve open once
Pumps                                        each week for about 20 min to drive out
                                             any water vapor that may have
The operating fluid in any type of pump      accumulated in the pump oil.
is called the pump fluid or pump oil.
With rotary pumps, normally a good           Ultimate Pressure
quality light petroleum oil, with the high   Attainable in Rotary Pump
vapor pressure factions removed, is used     Vacuum Systems
to provide pump sealing and lubrication
between the rotor vanes and stator           The limiting absolute pressure approached
housing. The oil for lubricating and         in a vacuum system, after sufficient
sealing is contained in an oil reservoir.    pumping time establishes that further
The arrangement of the reservoir differs     reductions in pressure will be negligible, is
from manufacturer to manufacturer. In        called the ultimate pressure. The range of
some small pumps, the pump chamber is        ultimate pressures of commercial rotary
actually immersed in the reservoir,          vacuum pumps extends from about 3 mPa
whereas for the larger pumps the reservoir   to 1 kPa (20 µtorr to 5 torr). The low
is usually separated from the pump           pressure of 3 mPa is reached only under
chamber, often being mounted above the       the most ideal conditions. The ultimate
pump itself.                                 pressure will be determined by:
Prevention of Condensate                      1. outgassing of the pump,
Contamination of Pump                         2. the seal between rotor and stator,
Oils                                          3. contamination of pump oil and
                                              4. the vapor pressure of the oil used.
Contamination of pump oil is one of the
main difficulties with rotary pumps. As      A high vapor pressure pump oil will
the gases and vapors are compressed, the     evaporate at a greater rate, which will
vapors will tend to condense and             create gas loads that saturate the pump
contaminate the oil. Degassing of vapors     and limit the ultimate pressure attainable.
from pump oil can limit the ultimate
vacuum attainable. Pumps are available           A disadvantage of any oil sealed and
with a gas ballast valve incorporated,       lubricated pump is the backstreaming of
which minimizes the condensation of          oil vapors from the pump inlet when inlet
vapors in the pump oil. The gas ballast      pressures drop below or approach 70 Pa
valve is a small valve that can be opened    (0.1 torr). This has become a major
manually to admit a controlled amount of     concern to many industries, such as
air to the pump cylinder during part of      semiconductor producers, for whom
the compression cycle. This will dilute the  backstreaming causes contamination of
vapors to the point where they do not        their products with oil vapors. As a result,
condense during compression. The violent     several new pump designs classified as dry
agitation of the oil by the additional air   or relatively free of this problem have
rushing through the pump causes              been available since the early 1980s. Two
reevaporation and exhaust of water that      of these are called scroll pumps and hook
may have been pumped from the vacuum         and claw pumps.
system in vapor form and condensed in
the pump oil. To effect the removal of       Rotary Dry Mechanical
moisture when the surrounding air is         Pumps
saturated with moisture, connect a dry
nitrogen gas supply to the gas ballast. Be   Unlike the rotary vane pump, which
careful to select a nitrogen flow rate and   requires a low vapor pressure oil to
pressure that will not apply overpressure    lubricate and seal the internal surfaces,
to the casing of the pump. The extent of     two commonly used pumps are designed
use of the ballast valve is determined by    with very small clearances between the
the amount of such vapors handled by         moving and fixed surfaces and no need
the pump. In normal high vacuum              for oil. As a result, the contamination
service, the ballast valve is usually kept   caused by vapors entering the evacuated
                                             space at low pump inlet pressures is
                                                                                                                      Leak Testing of Vacuum Systems 225
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eliminated. A slight disadvantage is that                                        pumping, gas is drawn in one side of the
                 these pumps cannot quite reach the same                                          claws and compressed on the other as the
                 low pressure as the lubricated pumps.                                            claws rotate. During rotation, the right
                 Ultimate pressures for dry pumps is in the                                       claw opens the intake slot, allowing gas to
                 range of 2 to 3 mPa (20 to 30 µtorr).                                            be drawn into the chamber.
                                                                                                  Simultaneously, the left claw opens the
                 Rotary Scroll Mechanical Pumps                                                   exhaust slot letting compressed gas
                                                                                                  escape. On completion of the
                 A scroll is a free standing involute spiral                                      compression cycle, the claws pass through
                 with a solid base on one side. A scroll set,                                     a neutral position and cycle begins again.
                 the fundamental element of a scroll
                 vacuum pump, is made up of two                                                   Pumping Speeds of Rotary
                 identical right and left hand involutes.                                         Mechanical Vacuum Pumps
                 When assembled, one scroll is indexed
                 180 degrees with respect to the other, to                                        Apart from the ultimate absolute pressure
                 allow the scrolls to mesh (Fig. 8).                                              that can be achieved by an particular
                                                                                                  pump, there is an interest in how fast the
                     In operation, one scroll is fixed and the                                    pump can reduce the pressure in a
                 other is attached to an eccentric, driven                                        vacuum system to the operating level.
                 by an electric motor. The pump inlet is at                                       Manufacturers normally specify the
                 the periphery of the scrolls. As the                                             pumping speeds of their mechanical
                 moving scroll orbits (but does not rotate)                                       pumps at atmospheric pressure. In
                 about the fixed scroll, the entering gas is                                      general, rotary pumps start pumping at
                 trapped in two diametrically opposed,                                            atmospheric pressure and, as the pressure
                 crescent shaped pockets bounded by the                                           is reduced, the pump becomes less
                 involutes and base plates of both scrolls.                                       efficient. It then is pumping the same
                 The pockets shrink as they follow the                                            volume, but at lower pressure. Eventually,
                 involute spiral toward the center,                                               the pumping speed becomes zero at the
                 compressing the gas. The compressed gas                                          ultimate minimum pressure.
                 exhausts to atmosphere through the
                 discharge port at the center of the fixed                                            Figure 9 is a plot of pressure as a
                 scroll.                                                                          function of pumping speed for a
                                                                                                  400 L·min–1 (15 ft3·min–1) mechanical
                 Rotary Claw Mechanical Pumps                                                     pump. It is seen that at atmospheric
                                                                                                  pressure, the pump is rated at
                 The hook-and-claw mechanism consists of                                          400 L·min–1; at 0.1 Pa (1 mtorr), the
                 several inline stages. The claw devices do                                       pumping speed is 200 L·min–1 at 0.01 Pa
                 not make contact with each other or with                                         (0.1 mtorr), the pumping speed is
                 the chamber walls, obviating oils. Each                                          16.7 L·s–1 (35 ft3·min–1). The pump speed
                 rotation of a claw pair consists of three                                        reduces to zero at 10–3 Pa (10 µtorr), the
                 cycles: a start cycle, compression cycle                                         ultimate pressure attained by this pump.
                 and a finish cycle. The two claws, which                                         At this point the gas handling capacity
                 divide the pump chamber, turn in                                                 has been saturated by the gas load from
                 opposite directions and, in so doing, open                                       the pump, thereby reducing its effective
                 and close the intake and exhaust slots                                           pumping speed to zero.
                 through which the gases pass. During
                                                                                                  Blower Pump or Booster Pump
FIGURE 8. Position of orbiting scroll shown before
compression cycle.                                                                                The blower or booster pump (Fig. 10) is a
                                                                                                  high throughput, low compression pump.
                                                                     Orbiting scroll              This pump is usually used on systems
                                                                                                  where a large volume of gas must be
                 Pocket of gas                                                                    pumped. It is also used with a mechanical
                 isolated                                                                         pump to serve as the forepump for large
                                                                                                  diffusion pumps, turbomolecular pumps
                                                                                      Gas inlets  or even other blower pumps.
                                                                                      shown
                                                                                      closed          The pump consists of two figure eight
                                                                                                  shaped rotors or lobes mounted axially on
     Gas inlets                                                                                   parallel shafts, as shown in the drawing
shown closed                                                                                      below. These rotors are synchronized by
                                                                                                  gears to prevent physical contact and
                                                                                                  damage and rotate in opposite directions.
                                                                                                  This rapidly displaces gas from the inlet to
                                                                                                  the outlet.
Exhausts at      Fixed scroll
      center
   opening
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How the Pump Works                                                                   Vacuum System Operation
These rotors are designed so that, while                                             Operating procedure consists of turning
spinning, they approach each other and                                               the mechanical pump on, then the blower
the housing within several thousandths of                                            (Fig. 11). Usually the mechanical pump
an inch. (See Fig. 10.) Rotor speeds vary                                            has lowered the pressure sufficiently for
from 40 to 60 s–1 (2500 to 3500 rotations                                            the blower to begin pumping by the time
per minute). Because of the high speeds                                              the blower has reached operating speed. A
and close tolerances of the rotating lobes,                                          bypass valve around the blower is
booster pumps are usually not started                                                sometimes used for high pressure
until roughing pressures of about 1.3 kPa                                            roughing.
(10 torr) have been reached. The typical
blower windmills at atmospheric pressure,                                                Blowers are commonly used where
producing much heat and very little                                                  large volumes of gas need to be pumped.
pumping action.                                                                      They are used when the lowest pressure
                                                                                     needed is 10–2 to 10–3 Pa (75 to 7.5 µtorr).
    Blower or booster pumps are most                                                 They also are used to help the mechanical
useful in the 0.1 to 0.01 Pa (1.0 to                                                 forepump or backing pump maintain a
0.1 mtorr) pressure range. They are always                                           low pressure and help reduce the
backed by a mechanical pump as a result.                                             possibility of oil backstreaming.
Operating at high pressures will cause
heating and expansion of the lobes. This                                             Turbomolecular Vacuum
can result in damage to the pump. No oil                                             Pumps
is used to seal the gap between stator and
rotor. Oil is used in the forevacuum                                                 The turbomolecular pump serves as an
section of the pump to lubricate the gears                                           alternative to the diffusion pump and
and bearings located there.                                                          must also be backed by a forepump. Its
FIGURE 9. Mechanical pump speed as a function of gas pressure for a pump rated at 6.7 L·s–1
(14 ft3·min–1) at atmospheric pressure.
Pump speed, L·s–1 (ft3·min–1)  7 (14.8)                                                         Atmospheric pressure
                               6 (12.7)
                               5 (10.6)
                               4 (8.5)
                               3 (6.4)
                               2 (4.2)
                               1 (2.1)
                                         10–3                   10–2    10–1    100     101     102     103           104  105
                               (10–7)                           (10–6)  (10–5)  (10–4)  (10–3)  (10–2)  (10–1)        (1)  (10)
                                                                                Pressure, Pa (lbf·in.–2 × 1.45)
FIGURE 10. Blower pump operation: (a) at beginning of cycle; (b) after eighth of cycle; (c) after fourth of cycle; (d) after three
eighths of cycle.
(a) (b) (c) (d)
Inlet Outlet to
                                                      forepump
                                                                                                                      Leak Testing of Vacuum Systems 227
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principle advantage over the diffusion       dimensions of the grooves at the inlet
pump is that it provides an essentially      port must be such that the molecules
vapor free vacuum without baffles or cold    have a good chance of hitting the walls of
traps. Thus, for a system where the back     the groove or the blades without making
streaming of vapor from a diffusion pump     numerous collisions with other gas
is undesirable or intolerable, a             molecules (see Fig. 12). As the gas is
turbomolecular pump could be used. Its       compressed while passing through
main disadvantage is that it has high        successive stages of the turbine, it is
speed rotating parts whereas the diffusion   necessary to decrease the dimensions of
pump has not moving parts. It also           the air passages to keep them comparable
requires air gap tolerance on the order of   with the mean free path of the molecules.
2 to 5 µm (8 × 10–5 to 2 × 10–4 in.)         The system must already be evacuated by
between the high speed rotor and grooves     a forepump before a turbomolecular
in the stator. As with a diffusion pump, a   pump can start pumping. It can achieve
molecular pump cannot operate at             pressures as low as 1.0 to 0.1 µPa (10 to
pressures above 13 to 1.3 Pa (100 to         1.0 ntorr). Pumping speeds for air vary
10 mtorr) and must be backed by a            from about 70 to 9000 L·s–1 (1.5 × 102 to
mechanical forepump.                         1.9 × 104 ft3·min–1), depending on the size
                                             of turbomolecular pump selected.
    A turbomolecular pump (see Fig. 12) is   Pumping speeds for hydrogen and for
a mechanical vacuum pump that creates a      helium vary only slightly from those for
gas flow toward a suitable forepump by       air whereas the exhaust pressure is in the
imparting momentum or motion to gas          range from 1.3 Pa to 1.3 mPa (10 mtorr to
molecules by means of a rapidly rotating     10 µtorr). Higher exhaust pressures are
rotor with successive rings with inclined    achieved in compound turbomolecular
blades. These blades rotate with
circumferential speeds comparable to the     FIGURE 12. Turbomolecular pump: (a) schematic; (b) inlet
thermal motion of the molecules (speeds      port.
of 100 to 700 m·s–1 or 330 to 2300 ft·s–1).
Some molecules are struck by the rotor       (a)
blades and rebound in a favorable axial
direction toward the stator blades. The                                                                     Gas inlet
molecules rebound from these stator
blades in a direction favorable for their    Power source
being impelled by the next stage rotor           for motor
blades and so on as the process is repeated
through all successive stages of rotor and                         To forepump
stator blades. The series of impacts
statistically favor motion through the
turbine stages toward the discharge port
and constitute a pumping action with a
very high compression ratio.
    The seal between the individual stages
is achieved by very narrow air gaps. The
FIGURE 11. Vacuum system with blower
pump.
Chamber          Roughing valve
                                             (b)
    High                                     Stator
vacuum
   valve
    Blower pump
Mechanical pump
                                                            Rotor
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pumps. These follow the turbomolecular           These vapor streams are directed
                      stages with one or several molecular drag    toward the outer walls of the pump. The
                      stages, which further compress the gas       walls are typically cooled by water. When
                      through the effects of viscosity.            the vapor hits the cooled walls, it
                                                                   condenses back into a fluid. This fluid
              Operation of Vapor or                                then flows downward into the pump
              Diffusion Pumps for                                  boiler for reboiling.
              Vacuum Systems
                                                                       The actual pumping of gases happens
                      Although mechanical rotary pumps             when the large, heavy, high speed oil
                      sometimes attain pressure below 0.1 Pa       vapor molecules hit gas molecules. The
                      (10–3 torr), they are generally used in the  gas molecules are knocked downward and
                      100 to 0.1 Pa range. To obtain pressures     compressed by the movement of the
                      well below 0.1 Pa, the vapor pump was at     vapor jet stream.
                      one time the most commonly used.
                      However, in the 1990s it was largely             The gas molecules are thereby
                      replaced by turbomolecular pumps             compressed in several stages to higher
                      because of the backstreaming of vapors.      pressures. They are finally pumped away
                      The principle of operation of vapor          through the foreline by the mechanical
                      pumps is entirely different from that of a   pump (Fig. 14). When the oil drops to the
                      rotary oil sealed pump, where the gases      bottom of the pump, it is reboiled and the
                      and vapors are compressed by a rotating      cycle repeats.
                      mechanical member and exhausted to the
                      atmosphere.                                  Vacuum Limitations of
                                                                   Vapor Diffusion Pumps
                          The vapor pump, or diffusion pump,
                      operates in the molecular flow region. The       A diffusion pump (Fig. 14) cannot
                      basic principle involved is shown in         operate at pressures above 0.1 Pa (1 mtorr)
                      Fig. 13.                                     because the oil vapor jets cannot form in
                                                                   the viscous flow region. Therefore, the
                          The pump works by heating the pump       pump must start pumping in a chamber
                      fluid to its boiling point. The vapors       that is already under vacuum (such as
                      travel upward inside the jet assembly and    that attained with a rotary mechanical
                      exit through the jet nozzles. In fact, they  forepump). Oil is the most frequently
                      are accelerated downward through the jet     used diffusion pump fluid because of its
                      nozzles. The vapor molecules travel very     low vapor pressure at room temperature.
                      fast and can reach supersonic speeds.        Oil has a fairly steep curve relating its
                                                                   pressure to temperature. This is necessary
FIGURE 13. Principle of operation of high vacuum vapor             for proper operation of the pump boiler.
pump. Vapor forced through a narrow opening (nozzle)               The lowest attainable pressure of the
attains a high speed and is directed at a downward angle.          diffusion pump is determined in part by
Molecules of gas or vapor that wander along a path toward
the jet stream will be struck by vapor molecules. The gas          FIGURE 14. Construction of three-stage high vacuum vapor
molecule B has diffused into the path of the jet stream where      pump.
it is struck by the vapor molecule A. Molecule B is given a
generally downward motion.                                         Cold cap        Inlet             Cylindrical
                                                                                                     water cooled
                                              Flow from                Multistage                    body
                                         vacuum chamber              jet assembly
                                                                                                           Exhaust
       Nozzle                                                      Thermal                                           Baffles
                                                                    protect                                         Foreline
                                                                     switch
A Ejector
B Electrical connector
                                                                                                            Fill and
                                                                                                               drain
                                                                                                          assembly
Vapor  Vapor jet                                                             Oil reservoir (boiler)  Heater
                                                                                                                      Leak Testing of Vacuum Systems 229
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the vapor pressure of the oil at the          of gas, it should not sacrifice high
temperature of the available cooling          conductance because that would impair
water. Oils specified by pump                 the net pumping speed of the system.
manufacturers have vapor pressures,
under these conditions, of about 0.1 µPa      Operation of Cold Traps in
(1 ntorr). The popularity of the diffusion    Vacuum Pumping Systems
pump is due to its wide range of
operation, low cost, reliability and lack of  A cold trap placed above the baffle
moving parts. The pump heaters are            ensures that those few oil molecules that
usually mounted from the outside and          may get by the baffle will not get to the
can be replaced during operation.             vacuum chamber. A cold trap, therefore,
                                              stops back migration of pump oil vapors.
    Should the diffusion pump be suddenly     It is also very effective as a cryogenic
exposed to a burst of atmospheric             pump for pumping condensable vapors
pressure, the oil jet stream would collapse,  such as water vapor, the chief offender in
thereby destroying the pumping                most systems, as well as for grease vapors
capability of the vapor pumps and             and other undesired contaminants.
possibly acting to crack the oil. The term
cracked oil refers to a decomposition of          As a cryogenic pump, the cold trap
pump oil due to exposure to oxygen in         reduces system pressure by taking
the atmosphere while at or near the           molecules out of the gas or vapor phase
boiling point of the oil. Some fluids are     and trapping them on its surface. These
less susceptible to cracking than are other   molecules are not pumped out of the
diffusion pump fluids.                        vacuum system and discharged to
                                              atmosphere. The most common
Operation of Baffles and                      techniques used to obtain low
Traps in Vacuum Pumping                       temperatures for cold traps are mechanical
Systems                                       refrigeration, dry ice and liquid nitrogen.
One of the objections to diffusion pumps          Some common forms of optically dense
has been the possibility of contaminating     chevron and cold traps are shown in
the vacuum chamber work area with the         Fig. 16, which also shows thimble type
pump fluid. By providing suitable traps       traps used in mass spectrometer leak
and baffles between the pump and the          detectors. The reservoir is filled with
vacuum chamber, back diffusion of oil         liquid nitrogen through the filler tube.
and oil vapor can be minimized and            Use of liquid nitrogen requires that the
condensable vapors from the chamber           thimble type trap be kept essentially in a
may be trapped. As a general rule, the        vertical position.
pumping speed of the system goes down
as the trapping efficiency of baffles and     Characteristics Desired in Vacuum
traps goes up, due to decreased               Valves
conductance.
                                              Vacuum valves must (1) be free from
    The baffle or trap should normally be     leakage, (2) offer minimum flow
kept as cold as possible. However, the
temperature of surfaces of the first          FIGURE 15. Typical baffle designs used in oil diffusion vacuum
baffling state above a pump should be         pump systems.
cool enough to condense the oil vapors,
but not so cold as to freeze the pump oil                                                  Plate
and prevent it from flowing back into the
pump.                                                              Cooling coils
Characteristics Desired in                                                                 Cooling
Diffusion Pump Baffles                                                                     coils
A baffle is simply a cool surface that is                          Top view
placed above the diffusion pump in the                             of disk
path of gas flow. This baffle is of metal
with good thermal conductivity that                                                               Cooling
keeps its surface at a uniform temperature.                                                       coils
The refrigerant, usually cold water, is
passed through tubing that is brazed to                            Cooling coils
the baffle. A baffle should also be
optically dense, that is, there should be     Cooling coils                                Top view
no line of sight through it, to avoid back                                                 of chevrons
flow of molecules in molecular flow.
Fig. 15 shows some typical designs of         Cooled chevron trap
baffles. Because a baffle restricts the flow
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resistance and (3) contain materials that                cracking the bellows. Never completely
     do not outgas. The biggest problem in                    extend bellows when out of the valve.
     making leaktight valve is in sealing the
     operating shaft. Two types of valves that                Operation of Capture
     accomplish efficient sealing are the                     Vacuum Pump
     bellows sealed and diaphragm valves
     (Fig. 17). Usually preferred are brass or                Unlike the previously described pumps,
     stainless steel bellows, more movement                   which compress and exhaust gas either to
     being obtained with brass. The bellows is                atmosphere or into an attached forepump,
     brazed to the cover (bonnet) and dish, as                two commonly used pumps collect and
     shown in Fig. 17a. Figure 17b shows a                    store gases in the pump body until
     valve using a diaphragm that can be a                    eventually being released to atmosphere
     metal or elastomer. Compared to metal                    by a process called regeneration (for the
     diaphragms, an elastomer has                             cryopump) or until the pump is rebuilt as
     considerable flexibility but also has the                in the ion pump. These pumps are the
     disadvantages of outgassing and                          mechanical cryopump and the sputter ion
     permeability to various gases. On the                    pump.
     other hand, metal diaphragms are not as
     elastic but have better outgassing and                   FIGURE 17. Operating principles of vacuum valves:
     permeability characteristics.                            (a) bellows sealed valve; (b) diaphragm valve.
     Precautions in Disassembly of                            (a) Cover
     Bellows Sealed Valves
     Always open bellows valve before
     removing the stem assembly to prevent
FIGURE 16. Cold traps used in vacuum pumping systems to                                                   Bonnet gasket
condense vapor molecules: (a) combination baffle and trap
with optically dense chevrons; (b) thimble trap used in leak                                          Braze
detectors.                                                                                    Bellows
(a)                                                                                                       Body
      Liquid                                                       Seat Braze
   nitrogen                                                                                Vent hole
                                                                                                        Diaphragm
       Water
(b)                                                           (b)
     Liquid nitrogen
             To                                                    Braze and mechanical seal
     chamber                                                       if an elastomer diaphragm
                                               To diffusion
                                                  pump
                                                                                                                      Leak Testing of Vacuum Systems 231
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Operation of Cryopump                                                            relief valve. In the expander, high pressure
                                                                                                   helium is supplied by the compressor.
                      The cryopump is unique in that it pumps                                      This gas is expanded in two stages to
                      by getting the gases so cold that they                                       produce cryogenic temperatures. The
                      freeze and are stored, or captured, in the                                   actual operating temperatures will vary,
                      pump. It is extremely clean, using no oil                                    depending on the thermal and gas loads
                      and having no moving parts in vacuum.                                        that are imposed. The first stage operates
                      It also has a very high throughput and is                                    between 50 and 80 K (–370 and –315 °F)
                      used in the high vacuum range in                                             and the second stage between 10 and
                      industrial applications where                                                20 K (–440 and –420 °F). The cryoarrays
                      hydrocarbons cannot be tolerated.                                            are the pumping surfaces, cooled by the
                                                                                                   expander, on which gases from the
                          A cryopump (Fig. 18)2 is made up of                                      vacuum chamber are condensed or
                      two main components: a gaseous helium                                        adsorbed.
                      compressor and a pump consisting of an
                      expander, cold head (chilled surfaces) and                                       In cryopump operation, helium is
                      the pump body. These two components                                          compressed and gives up its heat to the
                      are connected by flexible hoses to form a                                    surrounding walls of the compressor. This
                      closed loop refrigeration system. Gaseous                                    heat is removed by water or air cooling.
                      helium is circulated between the                                             The cooled, compressed helium then goes
                      compressor and expander.                                                     to the pump cold head. The expander at
                                                                                                   the cold head valving system lets the
                          The pump module consists of the                                          helium expand. The expanded helium
                      expander module, the first and second                                        now absorbs heat from the cold head and
                      stage cryoarrays, the pump body, second                                      baffle array. This chills the cold head and
                      stage temperature monitors and a pressure                                    baffle array to about 12 K (–440 °F) and
                                                                                                   70 K (–335 °F), respectively. These chilled
FIGURE 18. Schematic of cryopump.                                                                  surfaces pump gases from the vacuum
                                                                                                   chamber in two ways. The gases are either
                                                                                               C   condensed or adsorbed on the arrays.
                                                                                                   That most gases will stick to a surface in
                                                                                               D   an icelike state at less than 20 K (–420 °F)
                                                                                               E   is very likely. At this temperature, the
                                                                                                   combination of partial pressures of most
                                                                                               F   gases is about 10–9 Pa (10–11 torr) or lower.
                                                                                               G       Most gases are condensed on the first
                                                                                                   and second stage cryoarrays. The first
                                                                                               H   stage array is cold enough to pump water
                                                                                                I  vapor and carbon dioxide by
                                                                                                   cryocondensation. The colder second
                       A                                                                           stage array pumps nitrogen, oxygen,
                                                                                                   argon and most other gases by
                                                                               J                   cryocondensation, but is not cold enough
                                                                                                   to condense helium, hydrogen and neon.
               B                                                                                   These three gases are pumped by the
                                                                                                   process called cryosorption; a surface
 Legend                                                                                            related phenomenon: the greater the
   A = Forevacuum port                                                                             available surface area at cryogenic
   B = Power connection                                                                            temperatures, the more likely that gas
   C = Inlet flange                                                                                molecules will stick to it. Although most
   D = Baffle                                                                                      gases are frozen or condensed between
   E = Second cold stage                                                                           12 and 20 K (21 and 36 °R), helium,
    F = Radiation shield                                                                           hydrogen and neon are still very actively
   G = Cryoplates                                                                                  in motion at these temperatures. If we did
   H = Relief valve                                                                                not remove them, their partial pressures
    I = First cold stage                                                                           would continue to rise, perhaps to a point
    J = Vapor pressure thermometer                                                                 where the total system pressure would be
                                                                                                   unacceptable.
                                                                                                       To solve this problem, activated
                                                                                                   charcoal is attached to the bottom side of
                                                                                                   the second stage (coldest) cryoarray where
                                                                                                   it is less likely to adsorb the easier to
                                                                                                   pump condensible gases. This reserves the
                                                                                                   charcoal for the helium, hydrogen and
                                                                                                   neon which are trapped in the maze like
                                                                                                   structures and surfaces of the charcoal.
                                                                                                   This is similar to a sponge soaking up
                                                                                                   water vapor at room temperature. This
                                                                                                   process is called cryosorption.
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Before chilling the cryoarrays, the      are accelerated toward the anode. This
pump volume must be rough pumped to          long path increases the probability of
remove most of the gas below a valve at      ionization and therefore the amount of
the pump inlet. During chilling, when the    useful pumping action that can be
second stage drops to less than 20 °K, the   performed by the pump.
pump is ready for use. During use, the
pump can absorb very large amounts of            Because of the action of the magnetic
condensible gas, but the second stage        field, the electrons do not easily come in
charcoal eventually saturates, usually with  contact with the anode. As a result, a
hydrogen and must then be turned off to      cloud of electrons is formed within the
warm up the pump (regeneration). To          anode space. This electron cloud becomes
speed up this process, dry nitrogen is       fairly stable during pump operation and is
applied to the purge tube, through a         dense enough for the efficient ionization
valve, which flushes the pump and expels     of gas molecules. The name for this
the previously stored gas out through the    process is cold cathode discharge. The
pressure relief valve. When the second       positively charged ions, which are
stage rises to room temperature, the pump    relatively heavy particles, are accelerated
is ready to be rough pumped and chilled      into the negatively charged titanium
again.                                       cathodes. This impact causes sputtering,
                                             or chipping away of the titanium cathode
    The cryopump is normally used in the     material.
pressure range of 10–1 to 10–6 Pa (10–3 to
10–8 torr) but when operated continually         Sputtered titanium deposits onto the
at the upper end of this range, the time     internal structure of the anode. Then,
between required regeneration cycles is      when gas molecules come in contact with
proportionately shorter; i.e. — more         these clean titanium deposits, chemical
downtime.
                                             FIGURE 19. Section through a cold cathode ionization gage
Operation of Ion Pump                        (Penning gage).
The ion pump (Fig. 19)2 is also a gas                       AH
capture pump but is not designed to
pump heavy gas loads. For this reason, it                 B                         I
is not generally used alone in high                                                 J
production applications. It is more often                 C                         K
used in research and analytical
applications where there is no need to                    D                         L
cycle the work chamber repeatedly and                     E                         M
rapidly from atmosphere to vacuum.                                                  N
                                                          F
    Ion pumps are clean operating
electronic devices which use no moving                    G
parts or oils within the vacuum pump. It
is possible to achieve pressures in 10–9 Pa  Legend
(10–11 torr) range with overnight bakeout      A = High voltage connection
of the system. The bakeout process drives      B = Hood
residual gas off the system walls, which is   C = Protective cap
then pumped by the ion pump. In               D = Vacuum tight cast iron housing
research and analytical applications, the      E = Permanent magnet
ion pump’s cleanliness, bakeability, low       F = Small flange connection
power consumption, and long life make it      G = Baffle
the pump of choice for most ultrahigh         H = Safety terminal
vacuum uses. They are available in various      I = Leadthrough (anode lead)
sizes and variations, but only the simplest     J = Compressed glass-to-metal seal
(diode) pump will be described here for        K = Ring anode
purposes of brevity.                           L = Ignition pin
                                              M = Fixing screw
    A stainless steel ion pump body           N = Cathode plate (exchangeable)
contains a multicell anode assembly
constructed of cylindrical parallel tubes
spaced between two flat titanium
cathodes. A very strong magnet is placed
outside the pump body. After the ion
pump is rough pumped to 1 Pa (10–2 torr)
or less, a voltage of 5 to 7 kV direct
current is applied between the cathodes
and the anode assembly.
    The magnetic field forces any free
electrons within the anode into long
helical paths instead of straight paths.
This increases the probability of electron
collision with molecules, as the electrons
                                                                                                                      Leak Testing of Vacuum Systems 233
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combination converts these gas molecules     the system. At lower pressures, ion pumps
                    to solid compounds such as titanium          have long lives. Once they begin
                    oxide or titanium nitride. This process is   pumping, they quickly lower the pressure
                    called chemical gettering and produces       to the long life region. As long as they are
                    the required pumping action. In addition,    not pumping against a leak, they will last
                    a second pumping action takes place.         for years. An example of this would be
                    Some of the ionized molecules impact the     that a pump working at a constant
                    cathodes with enough force to become         pressure of 10–5 Pa (10–7 torr) would have
                    buried in them, which prevents them          a useful life of 20 years.
                    from neutralizing and becoming a free gas
                    again. A third pumping action occurs         Procedures for Pumping
                    with hydrogen which diffuses directly        and Operating Complete
                    into and reacts with the cathode plate.      Vacuum Systems
                    Also, neutral particles such as the inert
                    gases can literally be buried or covered by  By combining the components previously
                    the sputtered cathode material. Complex      discussed with appropriate manifolding,
                    molecules may also be split apart in the     plumbing and gaskets (O-rings), a
                    discharge to smaller, more readily pumped    complete vacuum system may be built as
                    molecules. Because these actions are not     shown schematically in Fig. 20. The initial
                    equally efficient, the chemically reactive   conditions are:
                    gases such as hydrogen, nitrogen and
                    oxygen are pumped at much higher              1. mechanical pump running,
                    speeds than the inert gases. A                2. diffusion pump operating and working
                    modification of the cathode design can be
                    made to increase the efficiency for these         in high vacuum,
                    inert gases.                                  3. cold trap filled with liquid nitrogen,
                                                                  4. atmospheric pressure in bell jar
                        Another characteristic of the ion pump,
                    often referred to as a sputter ion pump, is       chamber,
                    that it is self-regulating. At higher         5. high vacuum valve closed,
                    pressures, where much ionization takes        6. vent valve open,
                    place, more current flows and at low          7. roughing valve closed and
                    pressures, less current flows. This           8. foreline valve open.
                    characteristic current drain can be used to
                    measure the pressure, or degree of vacuum    An operational cycle for this vacuum
                    achieved with the pump. This feature         system is as follows:
                    eliminates the need for an ion gage on
                                                                  1. Close access to bell jar chamber, vessel
FIGURE 20. Schematic diagram of a typical complete vacuum             or hood to be evacuated.
system.
                                                                  2. Close vent and foreline valves. The
       Pumping      Bell jar chamber                                  ballast tank permits the
              port  or                                                turbomolecular pump or diffusion
                    other process vessel                              pump to discharge to an expansion
Vent valve                                                            volume so that a high critical
                                                                      forepressure is not reached.
    High                     Roughing
vacuum                       valve 2                              3. Start the roughing cycle by opening
 valve 1                                                              the roughing valve. This allows the
                    Cold trap Foreline                                mechanical pump to evacuate the
Diffusion                                                             manifolding between the high vacuum
   pump             Baffle   valve 3                                  valve and the bell jar chamber.
                                                To                4. After the pressure has been reduced to
                                          atmosphere                  below 10 mPa (about 50 µtorr) or
                                                                      crossover point, close the roughing
                    Ballast                                           valve.
                     tank
                                                                  5. Open the foreline and high vacuum
                            Leak test                                 valves. This allows the diffusion
                                  port                                pumping system (cold trap, baffle and
                                                                      turbomolecular diffusion pump) to
                                          Mechanical pump             continue pumping until the desired
                                                                      operating pressure is reached and work
                                                                      in the chamber may commence.
                                                                     After completion of work in the bell jar
                                                                 or vacuum chamber, the system may be
                                                                 cycled to its initial condition by first
                                                                 closing the high vacuum valve and then
                                                                 opening the vent valve. This allows
                                                                 atmosphere to enter the bell jar chamber
                                                                 and system up to the roughing and high
                                                                 vacuum valves. The pressure equalization
                                                                 allows access to the chamber.
234 Leak Testing
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PART 3. Materials for Vacuum Systems
Outgassing of Materials in                      This set one limit on the lowest ultimate
Vacuum Systems                                  pressure that can be reached in a
                                                particular vacuum system. The usual
Adsorption refers to the condensation of        technique of overcoming this problem is
gas (vapor) on the surface of a solid. As       to degas the materials, usually by baking
the pressure is reduced in a vacuum             (raising the system to a high temperature
chamber, there is a spontaneous evolution       while pumping). The bake-out
of gas (and vapor) from materials in the        temperature will depend on the
vacuum; this is referred to as outgassing.      temperature at which the material begins
                                                to change its properties. consequently,
    In vacuum systems the materials in the      vacuum systems are degassed at fairly
vacuum region may release adsorbed gases        modest temperatures, say 300 to 400 °C
and vapors that increase the gas load of        (570 and 750 °F), for several hours while
the system, resulting in a much longer          being pumped. This will eliminate much
pumpdown time. This phenomenon is               of the adsorbed gases and vapors.
most prevalent in new vacuum systems,
unclean vacuum systems or vacuum                    The dissolved gas content of a metal or
systems that have been exposed to               alloy will depend on factors such as
atmosphere for some considerable time. It       (1) the nature of the metal, (2) the
will also occur when new materials or           metallurgical process used in the
new work jigs and fixtures are installed in     production of the metal and (3) the
a vacuum chamber. Knowledge of the gas          degreasing and cleaning to which a metal
adsorption properties of various materials      was subjected. In comparing metals such
and, therefore, their outgassing properties,    as stainless steel and aluminum, stainless
is very valuable in vacuum work.                steel is found to outgas at a much lower
                                                rate. A cast aluminum surface outgasses at
Technique for Releasing                         a rate about ten times higher than the
Adsorbed Gases by                               rate at which a stainless steel surface
Moderate Heating                                outgasses. Therefore, during vacuum
                                                pumping, stainless steel vacuum systems
    Most metals in vacuum give off              are capable of reaching a desired vacuum
adsorbed or dissolved gases as well as          in a shorter time than a comparable
gases resulting from the decomposition of       aluminum system with its higher rate of
oxide near the surface. To minimize this        outgassing. Results are strongly influenced
gas evolution, metals can be heated under       by the condition of a metal (its alloy,
vacuum before being used in vacuum              cleanliness, finish etc.).
systems. Gas adsorbed by exposure to
atmospheric pressure can easily be released     Functions of Elastomers as
by heating to moderate temperatures.            Gaskets and Seals in
When pumping to pressures below 0.1 mPa         Vacuum Work
(1 µtorr) where baking is not practical, great
care must be taken in choosing the various      Certain openings must be provided for the
materials in the system. This applies to        insertion, removal and sealing of
choice of vacuum greases, elastomers,           equipment or materials for a given
metals and various sealing compounds.           vacuum system. During the operation,
                                                these openings must be tightly sealed.
Factors Influencing                             Elastomers are the most widely used gasket
Adsorption and                                  material, where temperature and gas loads
Outgassing by Baking                            permit, because they offer reliable sealing.
Vacuum System Materials                         Elastomers are natural or synthetic rubbers
                                                that can be vulcanized to a state in which
Gases and vapors are adsorbed by vacuum         they have an inherent ability to accept
construction materials (metals and              and recover from extreme deformation.
elastomers) and are gradually released.
                                                    For high vacuum service, leaks must be
                                                entirely eliminated and the gas evolved
                                                from the gasket material itself must be
                                                negligible. Both natural and synthetic
                                                rubber satisfy these requirements as long
                                                                                                                      Leak Testing of Vacuum Systems 235
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as negligible surface area is exposed.         room temperature and at pressures near
Frequently, gaskets must be exposed to oil     1 mPa (10 to 1 µtorr). Because of its
or other gasket deteriorating substances       temperature tolerance, silicone rubber is
and sometimes rather high or low               commonly used for low and high
temperatures must be tolerated. Gasketed       temperature operation. The fluorinated
joints should be readily accessible for tests  elastomers are highly resistant to most
for leakage. In designing a gasket these       corrosive materials found in vacuum
factors must be considered and                 practice. Fluorocarbon resin is very good
specifications should be based on material     but suffers from cold flow under pressure
capabilities as well as vacuum system          at room temperature; suitable means for
operational requirements.                      containing the fluorocarbon resin (spring
                                               loaded gaskets etc.) will eliminate this
Selection of Gasket                            difficulty. In trying to reach very low
Materials and Design for                       pressures, the permeability of the elastomer
Vacuum Seals                                   as well as its outgassing characteristics must
                                               be considered. Permeability is the property
The choice of natural or synthetic rubber      that determines how readily gases will pass
for a vacuum application depends on the        through a material.
combined qualities desired. In the case of
rubbers, a wide range of characteristics is    Selecting Elastomers to Reach Low
acceptable. Perhaps the most important         Pressure Vacuums
single factor is that of allowable deflection
under compression. This is a function of       To reach low pressures at room
hardness and allowable permanent set.          temperature, elastomers with low vapor
These materials generally contain volatile     pressures and low permeabilities are
oils, plasticizers and coloring pigments       desirable. consequently, considerable work
that adsorb moisture and gases. Most of        has been done with fluorinated elastomers.
the chemicals used have low vapor              Baking an elastomer at a temperature that
pressure at room temperature. The              does not damage it will reduce pumpdown
outgassing rates for various elastomers        time; however, it will still release some
depend on factors such as (1) the              vapor after many hours of pumping.
formulation used, (2) the area exposed,
(3) the operating temperature and (4) the      Selection of Alloys for Use
treatment of the elastomer before use. As      in Vacuum System
a rule, there is no way to control the         Components
formulation of gasket materials because
this is determined by the manufacturer.        There are many alloys of copper, but only
However, it is feasible to inform the          brasses and bronzes are used in vacuum
manufacturer of intended service and ask       practice. Brasses are copper zinc alloys,
for minimum volatiles. Exposed gasket          whereas bronzes are copper tin alloys.
area becomes critical as the operating         However, many brasses contain various
pressure is lowered. Proper gasket groove      other metals. Brasses are widely used for
design can help considerably in reducing       vacuum parts, such as diffusion pump
exposed areas.                                 parts, chambers, base plates, valves and
                                               fittings in high speed dynamic vacuum
    Because the outgassing rate of             systems.
elastomers increases as the temperature is
raised, the ultimate pressure can be               Many commercial bronzes contain
reached more rapidly if the elastomer can      zinc. Alloys containing zinc, cadmium,
be heated. However, all elastomers are         lead, antimony or bismuth should not be
damaged when heated too much. Also,            used in vacuum systems that are to be
the compression set increases more             baked because of the high vapor pressures
rapidly with temperature.                      of these metals. Vacuum firing is likely to
                                               alter the composition and therefore the
    Because of these properties, elastomeric   properties of such alloys.
gaskets are not normally used in ultrahigh
vacuum systems. Such systems are baked         Properties of Austenitic Stainless
at temperatures well above the damage          Steels in Vacuum Systems
point of all known elastomers. In this
case, it becomes necessary to use joints       Stainless steels have come into fairly
and seals of metals and alloys such as         common use in vacuum practice for
aluminum, brass, bronze, copper, indium,       turbomolecular pumps, diffusion pumps,
lead, silver, stainless steel and others.      manifolds, chamber baseplates etc.
                                               Austenitic stainless steels (types 302, 303
Properties of Specific Elastomers              and 304) are commonly used in vacuum
for Vacuum Seals                               work and are often called 18-8 stainless
                                               steels because they contain about
Natural and synthetic rubbers are              18 percent chromium and 8 percent
commonly used in systems that operate at
              236 Leak Testing
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nickel. These steels are nonmagnetic and       Selection and Properties of
the melting points of austenitic stainless     Vacuum Greases and Oils
steels are over 1400 °C (2550 °F). Surfaces
of stainless steels remain smooth because      Vacuum greases are commonly used to
oxides and hydroxides do not occur as in       help attain seals and to lubricate devices
other types of metals. This means that the     such as stopcocks and gasketed joints
effective surface area is less and vapors are  (static, rotating and sliding). In some
adsorbed in smaller quantities. This leads     cases, vacuum oils are used, including
to much easier degassing and quicker           diffusion pump oils. Oils are generally not
pumpdown.                                      as satisfactory as greases for most types of
                                               seals, because they are more readily
Properties of Aluminum Alloys                  squeezed out, thereby leaving a dry seal.
Used for Vacuum System                         In general, vacuum greases should not
Components                                     have a vapor pressure of more than about
                                               10 mPa (0.1 mtorr) at 30 °C (86 °F) and
Aluminum is also being used in vacuum          should maintain adequate viscosity at this
systems. The alloys of aluminum are            temperature and can be used up to a few
generally readily worked in the shop           degrees below their melting point. In
without much difficulty, the workability       general, vacuum greases should be applied
depending on the composition. Surface          sparingly and surplus grease then wiped
hardening can be achieved easily by            off, because greases absorb gases and
anodizing and other processes. Parts may       vapors and are dirt catchers.
be joined together by using aluminum
solder. Cast aluminum alloy parts are used     Diffusion Pump Oils
for a variety of purposes such as valves,
turbomolecular pumps, diffusion pumps          The ultimate vacuum of many vacuum
(particularly jet assemblies), grooveless      systems is, in fact, limited by insufficient
flanges and gaskets. The design of the dies    trapping of gas molecules by the diffusion
is important to get vacuum tight               pump fluid. Certain desirable properties
aluminum die castings. Although                that a diffusion pump oil must have
aluminum is difficult to de-gas                include the following.
thoroughly, it is commonly used for
vacuum parts where good heat and                1. It should have low vapor pressure.
electrical conductivity is required.                Vapor pressures of typical diffusion
                                                    pump oil recommended by
Properties of Other Metal Seals in                  manufacturers of diffusion pumps are
Vacuum Systems                                      in the range from 10 to 0.01 µPa (100
                                                    to 0.1 ntorr).
Certain specialty metals have almost the
same coefficient of expansion as most           2. It should have low enough viscosity to
glasses and have excellent sealing                  flow back into the boiler.
characteristics. They are used with
vacuum flanges in the manufacture of            3. It should have high molecular weight
ionization gage tubes and in other                  relative to the pumped gases to
applications where metal-to-glass                   increase the efficiency of removal of
junctures and seals are necessary.                  gas from systems being evacuated by
                                                    the vapor jets. Molecular weight of oil
Applications and                                    commonly used is in the range of 300
Limitations of Soft Metallic                        to 500 unified atomic mass units (u).
Vacuum Gaskets
                                                4. Oil should be thermally stable to
Metal gaskets of some kind are used by              avoid decomposition with heat.
vacuum seals that must be maintained at             Decomposition often results in the
temperatures higher than about 125 °C               evolution of more volatile fractions
(257 °F) or in which rubber cannot be               caused by cracking of the oil due to
used because of outgassing. Small gaskets           frequent exposure to atmospheric
of lead, copper, aluminum, gold, silver or          pressures.
tin have long been used for higher
temperature vacuum services. Complete           5. The fluid should be chemically stable
sealing demands high stresses and                   and noncorrosive in the presence of
consequently the metal gaskets can only             common metals, glass, elastomer
be used once. They are not designed for             gaskets and the gases and vapors
applications where the seals are often              usually present in vacuum systems.
opened and then reclosed because the
metal gaskets will take a permanent set         6. It should be nontoxic.
and are not reusable in most applications.
                                               The recommended hydrocarbon oils
                                               represent a very satisfactory low cost fluid
                                               for the normal vacuum range down to the
                                               low 10 µPa (100 ntorr) region. Ultrahigh
                                               vacuum is best obtained with oils specified
                                               by pump manufacturers. These oils are
                                               extremely stable, showing little change in
                                               properties even if the pump is exposed to
                                               atmospheric pressure with the heater on.
                                                                                                                      Leak Testing of Vacuum Systems 237
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