constituents within a volume is called          A leak testing tracer gas with low
diffusion. Under fixed conditions, it is    diffusivity provides an advantage in
found that lighter gases diffuse more       detector probe leak detection techniques
rapidly than the heavier gases. Graham’s    because the concentration of the tracer
law of diffusion states, The rates of       gas builds up at the leak exit. This allows
diffusion of different gases are inversely  detection by a probe to locate the site of a
proportional to their individual molecular  leak. With low diffusivity, the tracer gas
masses. Graham’s law can be written         does not leave the leak location rapidly.
mathematically in the form of Eq. 12:
                                                A tracer gas of high diffusivity is
(12) D1 = M1                                needed for internal pressurization where it
         D2 M2                              is necessary to fill cul-de-sacs or blind
                                            passageways within a reasonable soak
where D1 and D2 are the rates of diffusion  time before testing. A low diffusion rate
of gases 1 and 2 and where M1 and M2 are    would not allow a tracer gas to traverse a
the respective molecular masses of these    tortuous leak passage, thus making leak
two different gases.                        detection by tracer gas an unreliable
                                            procedure. Table 2 lists the diffusivities of
                                            typical tracer gases in air at standard
TABLE 2. Diffusivities of tracer gases in air at standard temperature of 0 °C (32 °F) and
standard pressure of 100 kPa (760 torr). (Diffusion coefficient values are calculated from
an empirical equation, after Slattery.2)
                                            Molecular        Difffusion
                                               Mass          Coefficient
Gas                   Formula               (g·mol–1)  mm2·s–1  (ft2·h–1)
Acetylene             C2H2                   26.0      14.2     (0.55)
Ammonia               NH3                    17.0      17.0     (0.66)
Argon                 Ar                     39.9      14.7     (0.61)
Benzene                                      78.1               (0.30)
Butane                C6H6                   58.1       7.7     (0.33)
Carbon dioxide        C4H10                  44.0       8.5     (0.52)
Carbon disulfide      CO2                    76.1      13.4     (0.36)
Carbon monoxide       CS2                    28.0       9.3     (0.67)
Carbon tetrachloride  CO                    154.0      17.3     (0.28)
Dichloromethane                              84.93      7.2     (0.29)
Ethane                CCl4                   30.1       7.4     (0.49)
Ethyl alcohol         CH2Cl2                 46.1      12.6     (0.38)
Ethylene              C2H6                   28.0       9.8     (0.52)
Refrigerant–11        C2H5OH                137.0      13.4     (0.30)
Refrigerant–12        C2H4                  121.0       7.7     (0.32)
Refrigerant–21        CCl3F                 103.0       8.3     (0.33)
Refrigerant–22        CCl2F2                 86.5       8.5     (0.37)
Refrigerant–112       CHCl2F                204.0       9.5     (0.25)
Refrigerant–114       CHClF2                171.0       6.5     (0.28)
Refrigerant-134a      CCl2F–CCl2F           102.0       7.2     (0.28)
Helium                CClF2–CClF2                       7.2     (2.70)
Hydrogen              C2H2F4                   4.0     69.7     (2.60)
Hydrogen sulfide      He                       2.0     67.1     (0.53)
Krypton                                      24.1      13.7     (0.51)
Methane               H2                     83.8      13.2     (0.72)
Neon                  H2S                    16.0      18.6     (1.10)
Nitric oxide          Kr                     20.2      28.4     (0.70)
Nitrogen                                     30.0      18.1     (0.68)
Nitrous oxide         CH4                    28.0      17.5     (0.52)
Oxygen                Ne                     44.0      13.4     (0.68)
Propane                                      32.0      17.5     (0.39)
Sulfur dioxide        NO                     44.1      10.0     (0.42)
Sulfur hexafluoride                          64.1      10.8     (0.28)
Water                 N2                    146.0       7.3     (0.85)
Xenon                 N2O                    18.0      21.9     (0.42)
                      O2                    131.0      10.8
                      C3H8
                      SO2
                      SF6
                      H2O
                      Xe
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conditions of 100 kPa (1 atm) pressure             collide elastically with each other and
and a temperature of 0 °C (32 °F). The             with the walls of their container.
diffusion coefficient values in Table 2 are    4. In any collection of gas molecules,
calculated and converted from an                   individual molecules have different
empirical equation.2                               speeds. However, their average speed
                                                   (including many molecules over a
Brownian Motion of Gases                           significant period of time) is
                                                   dependent on the absolute
One aspect of gaseous behavior that gives          temperature (kelvin or rankine
the strongest clue to the nature of gases is       degrees). The higher the gas
the phenomenon known as Brownian                   temperature, the higher the average
motion. This motion, first observed by the         molecular speed.
Scottish botanist Robert Brown in 1827, is
the irregular motion of extremely minute      Kinetic Theory Explanations of
particles suspended in a fluid. Brownian      Gaseous Pressure, Volume and
motion can be observed by focusing a          Temperature
microscope on a particle of illuminated
cigarette smoke in a glass tube. The          The kinetic theory of gases postulates that
particle does not settle to the bottom of     a gas consists mostly of empty space in
the container but continues to move           which billions of tiny points representing
randomly in all directions. The smaller       molecules are moving randomly. The
the suspended particle under observation,     molecular particles collide with each other
the higher the temperature of the fluid,      and with the walls of the container. The
the more vigorous is the particle’s           volume of a gas sample is the volume of
movement. The existence of Brownian           its container. Pressure is exerted by gases
motion suggests that the molecules of         because the molecules collide with the
gaseous matter are constantly moving. A       walls of the container. Each collision
visible small particle seems to be jostled    produces a tiny push or impulse as the
by its neighboring invisible particles. The   molecule rebounds from the wall. The
motion of the visible smoke particle thus     sum of all of these molecular pushes or
indirectly reflects the motions of the        force impulses of impact constitute the
smaller invisible particles of matter. This   pressure of the gas on its containment
provides powerful support for the idea        walls. The temperature of a gas is a
that gaseous or fluid matter consists of      measure of the average speed or kinetic
extremely small particles or molecules in     energy of the particles.
constant motion. The theory of moving
molecules of gases is the kinetic molecular   Kinetic Theory Explanations of the
theory of matter. Its basic postulates are    Gas Laws
these.
                                              The kinetic molecular theory of gases can
 1. The molecules of gaseous matter are in    be used to explain the observed behavior
     motion.                                  of gases as described by the gas laws.
 2. Heat causes this molecular motion.        Boyle’s Law. The pressure exerted by a gas
                                              at a given temperature depends only on
The kinetic theory of gases can be used to    the number of impacts of gas molecules
explain many of the properties and            with the walls of the container. If the
characteristics of tracer gases used in leak  volume is reduced as sketched in Fig. 4,
testing.
                                              FIGURE 4. Example of Boyle’s law. Doubling of gas pressure
Assumptions Underlying                        concentrates gas molecules and doubles number of
the Kinetic Theory of Ideal                   molecular impacts per unit area on chamber walls and piston
Gases                                         in given time period.
The kinetic theory of gases applies only to   Force = F      Force = 2F
ideal or perfect gases that behave in
accordance with the following                 Volume = 1 m3  Volume = 0.5 m3
assumptions.
 1. Gases consist of tiny molecules so
     small and so far apart that the actual
     volume of the gas molecules is
     negligible compared to the empty
     space between them.
 2. There are no attractive forces between
     gaseous molecules.
 3. The molecules of gases travel in
     random straight-line motion and
                                                                                                                            Tracer Gases in Leak Testing 39
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the molecules are more confined. This             constituents present (see Fig. 6.)
increases the frequency of molecular              Therefore, the partial pressure of a gaseous
collisions with the walls. These more             constituent in a gas mixture is not
numerous impacts are observed as a                changed by the presence of other gases in
greater pressure.                                 the container. The total pressure exerted
                                                  on the walls of the container (or on the
Charles’ Law. If the temperature of a gas         diaphragm of a pressure measuring gage)
rises, the average molecular energy and so        is equal to the sum of the partial pressures
the average speed of the gas molecules            exerted by the individual constituents of
rises. As the molecules move more                 the gaseous mixture.
energetically, they collide with the walls
of the container more frequently and with         Determining
greater momenta, thus producing greater           Concentration of Tracer
pressure. (Force is equal to the time rate of     Gas in Gas Mixtures from
change of momentum and pressure is the            Partial Pressures
force per unit area.) As shown in Fig. 5, if
the temperature is raised, the balloon            In many leakage measurements, it is
responds to the increased pressure by             desirable or necessary to dilute the tracer
stretching and expanding its diameter.            gas being used for leak testing. Use of
                                                  diluted tracer gas might be dictated by
Dalton’s Law. According to the kinetic            practical considerations such as:
theory of ideal gases, there are no
attractive forces between the molecules of         1. high expense of pure tracer gas filling
gases. On the average, the molecules of                large volumes or attaining high
each constituent of a gaseous mixture will             pressures;
strike the walls of their container the
same number of times per second and                2. attainment of a more nearly linear or
strike with the same impact forces as they             more stable instrument response at a
would if there were no other gases                     lower concentration of tracer gas;
FIGURE 5. Example of Charles’ law. Raising         3. pure tracer gas providing a much
gas temperature increases molecular                    higher leakage sensitivity than needed;
velocities and increases gas pressure on
container wall. Under constant atmospheric         4. danger of fire or explosion with a
pressure, impacts by higher velocity                   flammable tracer gas (in some cases, a
molecules cause increase in gas volume                 dilute gas mixture lowers the danger
within elastic balloon.                                of explosions); and
                                     Heated        5. inability to completely evacuate the
                                     balloon           test object or test system before filling
                                                       with tracer gas. As a result, residual gas
Cooled                                                 dilutes the tracer gas added during
balloon                                                pressurizing.
                                                      Concentration of the tracer gas in a
                                                  test system containing mixed gases
                                                  depends on the partial pressure of the
                                                  tracer gas. Dalton’s law (Eq. 4) shows the
                                                  contributions of each gaseous constituent
                                                  to the total gas pressure. The fractional
                                                  concentration of the tracer gas T is given
                                                  by the term NT in Eq. 13:
FIGURE 6. Example of Dalton’s law: (a) oxygen; (b) nitrogen; (c) nitrogen and oxygen
combined. Partial pressure of each gaseous constituent is not changed by presence of other
gases in the same container. Pressure is exerted on container walls by impacts of individual
molecules of all gas species.
(a)                             (b)           N2       (c)
                 O2  P=5                                         N2 and O2
                                                  P=7                       P = 12
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(13) NT   = PT                                               that in the atmosphere at sea level.
               P total
                                                             Helium is present in the earth’s
          = PT                                               atmosphere in the proportion of 5 µL·L–1.
               P1 + P2 + P3 + … + Pn                         With mass spectrometer types of helium
                                                             leak detectors, even this small proportion
                                                             of helium can be readily sensed.
    This fractional concentration is given                   Mean Free Paths of Gas
by Eq. 13 in terms of the number of                          Molecules
molecules of tracer gas as a fractional part
of the total number of molecules in a                        The mean free path is the average
gaseous mixture. The percentage                              distance a gas molecule travels between
concentration by mass would depend also                      successive collisions with other molecules
on the molecular masses of each gaseous                      in the gas or vapor state. The mean free
constituent. The partial pressure PT of                      path is important in leak testing because
tracer gas required to provide a specific                    it determines the type of gas flow that will
percentage of tracer gas molecules,                          occur through leaks or other passageways
percent T, is given in terms of total                        traversed by tracer or pressurizing gases.
system pressure Ptotal by Eq. 14:                            The mean free path can be calculated
                                                             from the pressure, temperature and
(14) P T  =  %T × Ptotal                                     molecular properties by means of Eq. 15:
                   100
Partial Pressures of Gaseous                                 (15)  λ = 116.4 n            T
Constituents of Earth’s                                                                P  M
Atmosphere
                                                             where λ is mean free path (meter) under
The composition of atmospheric air is                        static pressure; n is gas viscosity (pascal-
78 percent nitrogen, 21 percent oxygen,                      second); P is absolute pressure of gas
0.9 percent argon and about 0.1 percent                      (pascal); T is absolute gas temperature,
of other gases and vapors (including water                   (kelvin); and M is molecular mass of gas,
vapor, whose concentration varies with                       (g-mol–1).
the temperature and relative humidity of
the atmosphere). The partial pressures of                        Table 4 lists the mean free paths of
atmospheric constituents at sea level,                       common gases at 20 °C (68 °F) and
where the total pressure of 100 kPa                          1.0 mPa (7.6 µtorr).
(1 atm) is equal to that of 760 torr, are
given in Table 3.                                            Simple Approximation Formula
                                                             for Mean Free Path of Common
    The partial pressure in kilopascal is                    Gases
about the same as the percentage of each
constituent gas, at standard atmospheric                     An easily remembered relation for
pressure. The partial pressures of                           approximating the mean free paths of
atmospheric constituents at an altitude of                   common gaseous molecules is presented
3600 m (12 000 ft), where the total                          in Eq. 16:
pressure is equal to 64.4 kPa (9.3 lbf·in.–2
absolute), are given in Table 2.                             (16) λ = NF
                                                                                 P
    The percentage composition of
atmospheric air changes very little until                    where λ is mean free path length (meter),
very high altitudes are reached. When test                   P is gas pressure in pascal and NF is a
systems are pressurized with air pumped                      numerical factor (meter-pascal) given in
from the atmosphere, the percentage                          Table 5. An NF value of 6.8 × 10–3 permits
composition is also not changed from
TABLE 3. Partial pressures of atmospheric constituents at sea level, 100 kPa (1 atm).
                          kPa at                                   (torr at  kPa at          (torr at
Gas            Percent    sea levela                         sea level)a 3.6 km           12 000 ft)b
Oxygen (O2)     21.0       21.28                             (159.6)         13.52        (101.4)
Nitrogen (N2)   78.0       79.03                             (592.8)         50.22        (376.65)
Argon (Ar)
Other             0.9        0.91                               (6.84)        0.58           (4.35)
Total air         0.1        0.10                               (0.76)        0.06           (0.45)
               100.0      101.325                            (760.00)        64.4         (483.0)
a. Atmospheric pressure at sea level = 101.325 kPa (1 atm).
b. Percentage × atmospheric pressure of 64.4 kPa.
                                                                                                                            Tracer Gases in Leak Testing 41
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TABLE 4. Mean free path lengths of                              Relation of Mean Free Path
     various atmospheric gases at 20 °C                              Lengths to Viscosity and
     (68 °F) and at absolute pressure of                             Molecular Mass of Gas
     1.0 mPa (7.6 µtorr).
                                                                     The ratio of mean free path lengths for
                                    __M__e_a_n__F_r_e_e__P_a_t_h___  two different gases at the same
             Gas m (in.)                                             temperature and pressure are given by
                                                                     Eq. 17:
                     Air                    6.8   (268)              (17)  λ1  =  n1  M2
                     Argon (Ar)             7.2   (284)                    λ2     n2  M1
                     Carbon dioxide (CO2)   4.5   (177)
                     Hydrogen (H2)         12.5   (492)                  In Eq. 17, n indicates the gas viscosity
                     Water (H2O)            4.2   (165)              and M indicates its molecular mass. The
                     Helium (He)           19.6   (771)              subscript 1 indicates the first gas and
                     Nitrogen (N2)          6.7   (264)              subscript 2 indicates the second gas. (This
                     Neon (Ne)             14.0   (551)              relationship is derived from Eq. 15 when
                     Oxygen (O2)            7.2   (284)              T and P are held constant.) For a leak or
                                                                     an orifice across which there is a sizable
     use of Eq. 16 for estimating the mean free                      pressure differential, the mean free path
     path lengths for air, argon, nitrogen and                       length within the orifice is typically
     oxygen molecules. Table 5 lists the                             estimated from the average pressure in the
     numerical factors used in the numerator                         orifice (the mean value of inlet and outlet
     of Eq. 16 for several other common gases.                       pressures).
     However, it is seldom necessary to know
     mean free path lengths to precisions                            Effective Viscosity of Mixtures of
     better than one order of magnitude. For                         Gases
     example, the molecular mean free path at
     20 °C (68 °F) at atmospheric pressure is of                     In a mixture of various species of gases,
     the order of 30 to 300 nm. At a pressure                        the effective viscosity nmixture is assumed
     of 1 Pa (1.5 × 10–4 lbf·in.–2), the mean free                   to be proportional to the sum of the
     path is in the range from 3 to 30 mm                            products of viscosity and concentrations
     (0.12 to 1.2 in.).                                              for each individual gaseous constituent, as
                                                                     indicated by Eq. 18:
TABLE 5. Physical properties of common gases used in leak testing.
                                                  Numerical                       Diffusivityd
                                                                                     in Air at
                                           Densitya Factorb for      Dynamic                         Thermal
                                                                                  0 °C (32 °F)   Conductivitye
                              Molecular at        Mean Free Viscosityc            and 101 kPa
                                                                                                at 20 °C (68 °F)
                              Mass 100 kPa        Path at 20 °C (68 °F)              (m2·s–1)     (W·m–1·K–1)
Gas                  Formula (g·mol–1) (g·L–1)    (m·Pa)             (µPa·s)
Airf                 Mixture   29.0        1.21    6.8 × 10–3        18           13.9 × 10–6    26.2
Argon                          40          1.79    7.2 × 10–3        22           15.8 × 10–6    17.9
Carbon dioxide       Ar        44          1.97    4.5 × 10–3        15                          16.0
Refrigerant-12                121          5.25                      13           63.4 × 10–6
Helium               CO2                   0.179  19.6 × 10–3        19                            9.8
Hydrogen             CCl2F2      4.0       0.090  12.5 × 10–3                     17.8 × 10–6   149.0
Krypton              He          2.0       3.74                       9           23.9 × 10–6   183.0
Neon                           84          0.90    5.36 × 10–6       25
Nitrogen             H2        20          1.25   14.0 × 10–3        31                            9.4
Oxygen               Kr        28          1.43                      18                          48.0
Sulfur hexafluoride            32          6.60    6.7 × 10–3        20                          25.6
Water Vaporg         Ne       146          0.83    7.2 × 10–3        15                          26.2
Xenon                          18          5.89    2.5 × 10–3                                    13.0
                     N2       131                  4.2 × 10–3         9                          18.7
                     O2                            3.8 × 10–3        22
                     SF2                                                                           5.5
                     H2O
                     Xe
a. Density in oz·ft–3 = g·L–1 = mg·cm–3 at 20 °C (68 °F) and 100 kPa (1 atm).
b. Numerical factor for calculating mean free path using Eq. 16. Mean free path in meters at 20 °C (68 °F).
c. Independent of pressure under conditions for viscous flow.
d. Diffusivity in m2·s–1 in air at 0 °C (32 °F) and 101 kPa (1 atm).
e. Thermal conductivity in W·m–1·K–1 at 20 °C (68 °F). Thermal conductivity is independent of pressure under conditions for viscous flow.
f. N2, 78 percent; O2, 21 percent; argon, 0.9 percent; others, 0.1 percent.
g. Vapor pressure of H2O at 20 °C (68 °F) is 2.3 kPa (17.5 torr).
               42 Leak Testing
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(18) nmixture = N1 n1 + N2 n2                             masses of common gases and some vapors
                                                          are tabulated in Table 6.
                       + … + Nk nk
                                                              Vapors resulting from evaporation of
where n1 is viscosity of the first gaseous                liquid hydrocarbon compounds have
constituent and N1 is fractional                          molecules containing relatively large
concentration of the first gaseous                        numbers of atoms. Molecular masses of
constituent, as defined by Eq. 14.                        such organic chemical compound vapors
                                                          increase as the macromolecules increase
Molecular Masses of Gases                                 in complexity and contain more atoms.
and Vapors
                                                          Stratification of
Any combination of atoms in a chemical                    Constituents in Mixtures of
compound is called a molecule. The                        Gases
molecular mass equals the total number
of nucleons in the atoms forming the                      If a tracer gas is added to air already
molecule. Most elements in the gaseous                    within a vessel or system under test, a
state form diatomic molecules that consist                uniform mixture of gases is often difficult
of two atoms of that element loosely                      to achieve. The tracer gas will settle
bound by electronic forces. The molecular                 toward the top or toward the bottom of
mass of diatomic gases is twice the atomic                large containers, depending on the
mass. For example, the element oxygen O                   density of the tracer gas relative to the
has an atomic mass of 16; gaseous oxygen                  density of the air or other pressurizing
O2 has a molecular mass of 32. Exceptions                 gases within the system. This stratification
to this diatomic arrangement in gases                     of mixed gases is more pronounced with
include most metallic vapors and the                      high molecular mass gases and with gases
noble gases. The noble gases (argon,                      with low diffusion coefficients.
helium, neon, krypton, radon and xenon)                   Precautions should be taken to avoid or
have extremely stable electronic structures               correct stratification effects during leak
and typically do not combine with any                     testing by (1) premixing of tracer gas with
other atom species. The molecular masses                  diluent gases before injection, during
of the monatomic gases are identical to                   pressurization of the test system or
their atomic masses.                                      enclosing hood or chambers and
                                                          (2) providing some means for circulating
    In chemical compounds containing                      and mixing the gases within large volume
different elements (for example, carbon                   chambers or test systems.
dioxide) the molecular mass is the sum of
the atomic masses of the constituent                          Usually, there should be no problems
atoms. One carbon atom (atomic mass 12)                   with pooling or stratification inside test
combines with two oxygen atoms (atomic                    systems, if precautions are taken to mix
mass 16 each) to form CO2 with a                          the tracer gas thoroughly with the diluent
molecular mass of 44. The molecular                       gas in pressurization of the test system.
                                                          However, if the test pressure is to be about
TABLE 6. Viscosity and molecular masses                   atmospheric pressure in the test system,
of typical gases and vapors used in leak                  the system should first be evacuated to
testing.                                                  remove air at atmospheric pressure and to
                                                          replace it by the thoroughly mixed
     Viscosity at          Relative                       combination of tracer gas with diluent
                                                          gas.
     15 °C (60 °F) Molecular
                                                          Equilibrium Distribution
Gas              (µPa·s)a  Mass (u)b                      Law for Gas Concentration
                                                          Ratios with Gravity Effect
Hydrogen          8.7       2.02
Helium           19.4       4.00                          The preferred technique is that in which
Methane          10.8      16.0                           both the tracer and diluent gases used in
Ammonia vapor              17.0                           pressurization of test systems are
Water vapor       9.7      18.0                           premixed or added simultaneously
Neon              9.3      20.2                           through a screened aperture or rake so as
Nitrogen         31.0      28.0                           to be mixed rather uniformly from the
Air              17.3      28.7                           start. There should then be no problem of
Oxygen           18.0      32.0                           pooling of denser constituents inside the
Hydrogen         20.0                                     system under test, provided that
                           36.5                           precautions are taken to mix the tracer
 chloride vapor  14.0      39.9                           thoroughly with diluent gas in the
Argon            21.9      44.0                           pressurization of the system. The
Carbon dioxide   14.5                                     equilibrium distribution law of Eq. 19
a. One µPa·s = 10 micropoise.
b. One unified atomic mass unit (u) ≅ 1.6605 × 10–27 kg.
                                                                                                                            Tracer Gases in Leak Testing 43
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gives the ratio Ch of tracer as
                   concentration at the top of a tank relative
                   to the concentration Co of the same
                   gaseous constituent at the bottom of the
                   tank:
                                                            − Mgh
                   (19) Ch = Co e RT
                   where M is molecular mass of gaseous
                   constituent, h is height of interior volume
                   of tank, R is universal gas constant, T is
                   absolute temperature and g is local value
                   of acceleration due to earth’s gravity.
                        From Eq. 19, it is evident that with a
                   specific tracer gas in equilibrium
                   distribution, the concentration of tracer
                   gas diminishes exponentially as height
                   within the chamber increases. The
                   greatest concentration of the gaseous
                   constituent is at the bottom of the tank
                   and the lowest concentration exists at the
                   top of the tank. However, this effect takes
                   no account of the relative densities of the
                   tracer gas and diluent gas. If the tracer gas
                   were lower in density than the diluent gas
                   (as with helium tracer gas in air),
                   stratification effects could have a
                   predominant effect, with helium
                   collecting at the top of the tank after a
                   period of time. If the tracer gas were
                   higher in density than the diluent gas (as
                   with refrigerant-12 gas in air),
                   stratification effects could also
                   predominate and the denser tracer gas
                   would tend to collect at the bottom of the
                   tank after a period of time. In large test
                   chambers or enclosing hoods, it would be
                   desirable to provide constant internal
                   circulation and mixing of the internal
                   contents of tracer gas and diluent gas, as
                   with a fan.
44 Leak Testing
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PART 2. Mechanisms of Gaseous Flow through
Leaks
Modes of Gas Flow                             Depending of the material and the type of
through Leaks of                              gas, a rubber O-ring usually represents a
Restrictions                                  permeability of about 5 × 10–7 Pa·m3·s–1
                                              (5 × 10–6 std cm3·s–1) for every 100 kPa
To clarify the problem of leakage, it is      (760 torr) of pressure differential per
necessary to consider gas flow through        linear centimeter of exposed O-ring
small restrictions. It is extremely           surface. This permeability does not have
important to know something about the         to be taken into consideration during
basic modes of flow: viscous, transitional    routine leak testing if the leakage
and molecular. Viscous flow may be            measurement occurs in a time too short
further divided into laminar flow or          to permit the saturation and mass transfer
turbulent flow. Other special modes of        of gas through the O-ring.
leakage or flow are permeation and
choked flow. The factors that influence       Mean Free Path of
gaseous flow through leaks are (1) the        Gaseous Molecules
molecular mass of the gas, (2) the
viscosity of the gas, (3) the pressure        Molecular flow occurs when the mean
difference causing the flow, (4) the          free path of a tracer gas is greater than the
absolute pressure in the system and           cross section dimension of the leak. The
(5) the length and cross section of the       mean free path is the average distance a
leak path.                                    molecule travels between successive
                                              collisions with other molecules in vapor
    An understanding of leakage               state. The mean free path is of some
mechanisms and controlling factors is         importance in leak testing because it
vital to the proper interpretation of leak    establishes the type of gas flow that will
tests. A simple description of gaseous flow   occur. The mean free paths of several
through leaks is presented here for leak      gases are given in Table 4.
testing operators and supervisory
personnel, followed by a theoretical              In flow systems encountered in leak
approach to leakage.                          testing, knowing the mean free path
                                              allows one to know, or at least estimate,
Permeation of Gases through                   the type of flow occurring. Table 4 shows,
Solids                                        in general, the relationship of mean free
                                              path to pressure and the information may
Permeation is the passage of fluid into,      be used as a guide to determine the nature
through and out of a solid barrier having     of the flow.
no holes large enough to permit more
than a small fraction of molecules to pass    Characteristics of
through any one hole. The process also        Molecular Flow of Gases
involves diffusion through a solid and
may involve many phenomena such as            It should especially be noted that in
adsorption, dissociation, migration and       molecular flow the leakage rate is
desorption.                                   proportional to the difference of the
                                              pressures. Molecular flow occurs quite
    The first implication of permeation is    often in vacuum testing applications. In
that if the system is to be relatively        molecular flow, molecules travel
leaktight, the materials of construction      independently of each other. It is possible
have to exclude leakage by permeability.      for random molecules to travel from a
As an example, the permeation rate at         part of a system at low pressure to
room temperature of a natural rubber          another part of the system at a higher
gasket (2.5 mm thick, with a 2.5 mm wide      pressure. When an ultrahigh vacuum
rim and a 125 mm diameter) with a             system is being tested by a mass
100 kPa (1 atm) hydrogen pressure             spectrometer leak detector, the mass
differential is 1.6 × 10–6 Pa·m3·s–1          spectrometer leak detector operates at a
(1.6 × 10–5 std cm3·s–1). In some uses, this  pressure of about 10 µPa (0.1 µtorr)
permeation might represent an                 whereas the ultrahigh vacuum system
unacceptable leakage rate.                    might be operating at a pressure of
    Another similar example of this type of
permeation involves a rubber O-ring.
                                                                                                                            Tracer Gases in Leak Testing 45
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0.1 µPa (1 ntorr). When a tracer gas enters    measured are in the laminar flow range,
the ultrahigh vacuum system through a          the simplest means of increasing test
leak, it will eventually travel from the       sensitivity is by an increase of pressure
0.1 µPa (1 ntorr) vacuum system to the         across the leak.
mass spectrometer operating at 10 µPa
(0.1 µtorr) by the process of molecular        Viscous Flow of Gases
flow. This does not imply that the total       through Leaks
flow is from a system at low pressure to
one at high pressure. The mass                 Laminar flow is one of the two classes of
spectrometer operating at 10 µPa               viscous flow; the other class is turbulent
(0.1 µtorr) sends some gas molecules into      flow. Because turbulent flow is rarely
the system at the lower pressure.              encountered in leaks, the term viscous flow
However, when summing flows, total net         is sometimes incorrectly used to describe
flow is from the high-pressure to the low      laminar flow in leak testing. Viscous flow
pressure region. The high pressure system      implies that the flow occurs when the
is contributing gas molecules to the           mean free path of the gas is smaller than
ultrahigh vacuum system. The tracer gas        the cross section dimension of the leak. It
flow in the direction opposing the major       should especially be noted that the
flow of molecules is possible because of       viscous flow leakage rate is proportional
the random mode of molecular flow. The         to the difference of the squares of the
gas molecules, when traveling from one         pressures. Viscous flow leakage occurs in
system to the other, do not come in            high pressure systems, such as are
contact with molecules traveling in the        encountered in detector probe leak tests.
other direction.                               It is often related with the Reynolds
                                               number. The dimensionless Reynolds
Characteristics of                             number is the ratio of the inertial to the
Transitional Flow of Gases                     viscous forces acting on the medium. In
                                               the case of tubes (or leak paths), the
Transitional flow occurs when the mean         Reynolds number NRe is expressed by
free path of the gas is about equal to the     Eq. 20:
cross section dimension of the physical
leak. It occurs under conditions               (20) N Re  =  vd
intermediate between laminar and                              η
molecular flow. The transition from
laminar flow to molecular flow is gradual.     where v is velocity (m·s–1), d is diameter of
The mathematical treatment of this             opening (meter) and η is kinematic
region is extremely difficult; however, a      viscosity (m2·s–1). However, any set of
treatment of this region is necessary          consistent units may be used in this
because leakage from an enclosed volume        equation. Above a critical value of the
to a vacuum necessarily involves a             Reynolds number (about 2100 in the case
transition from laminar to molecular flow.     of circular tube flow), flow becomes
                                               unstable. This results in innumerable
Characteristics of Laminar                     eddies or vortexes in the flow. The partial
Flow of Gases                                  path in turbulent flow leaks is very erratic.
                                               In laminar flow, the particles flow nearly
The laminar flow of a fluid in a tube is       straight line paths.
defined as a condition in which there is a
parabolic distribution of the fluid velocity   Characteristics of Choked
in the cross section of the tube. The two      (or Sonic) Flow of Gases
most important characteristics of laminar
leaks are (1) the flow is proportional to      Choked flow, or sonic flow as it is
the square of the pressure difference          sometimes called, occurs under certain
across the leak and (2) the leakage is         conditions of leak geometry and pressure.
inversely proportional to the leaking gas      Assume there exists a passage in the form
viscosity. Table 1 shows that the viscosity    of an orifice or a venturi, and assume that
of most gases varies by less than one order    the pressure upstream is kept constant. If
of magnitude. Changing the tracer gas          the pressure downstream is gradually
will not markedly increase the sensitivity     lowered, the velocity through the throat
of the leak test unless this change of gas     or orifice will increase until it reaches the
implies a change of instrument sensitivity.    speed of sound through the fluid. The
However, increasing the pressure               downstream pressure at the time the
difference across the leak by a factor of a    orifice velocity reaches the speed of sound
little over three will increase the flow rate  is called the critical pressure. If the
through this leak by a factor of ten.          downstream pressure is lowered below
Obviously then, when the leaks to be           this critical pressure, no further increase
                                               in orifice velocity can occur, with the
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TABLE 7. Composition and partial pressures of dry air at sea level (101.325 kPa or
1.00 atm). Note the similarity of partial pressures with the percentages. When less
precision can be tolerated, use percentages × 103.
                     Content                             Partial Pressure
                     ________________________  ________________________________
Constituent          Percent      µg·g–1             Pa (torr)
Nitrogen             78.084        ——          7.9119 × 104  (4.9343 × 102)
Oxygen               20.946        ——          2.1224 × 104  (1.5919 × 102)
Argon                              ——          9.460 × 104
Carbon dioxide        0.934        ——          3.34 × 101    (7.10)
Neon                  0.033       18.18                      (2.50 × 10–1)
Helium                1.8 × 10–3   5.24        1.84          (1.38 × 10–2)
Krypton               5 × 10–4     1.14        5.3 × 10–1    (3.98 × 10–3)
Xenon                 1 × 10–4     0.087       1.16 × 10–1   (8.66 × 10–4)
Hydrogen                           0.5         8.8 × 10–3    (6.61 × 10–5)
Methane                 ——         2.0         5 × 10–2      (3.80 × 10–4)
Nitrous oxide (N2O)     ——         0.5         2 × 10–1      (1.52 × 10–3)
                        ——                     5 × 10–2      (3.80 × 10–4)
                        ——
consequence that the maximum mass              be used. Table 7 lists the standard
flow rate has been reached. This condition     composition of dry air at sea level.
is known as choked or sonic flow.
                                                   The physical properties of gases and
Leaks Dependent on a Critical Gas              vapors are also important, including the
Temperature or Pressure                        molecular mass, the molecular diameter
                                               and the viscosity. The gas streaming
Both pressure dependent leaks and              through a narrow bore tube experiences a
temperature dependent leaks have been          resistance to flow so that the velocity of
observed, but in extremely limited             gas flow decreases uniformly from the
number. Pressure dependent or temperature      center outwards until it reaches zero at
dependent leaks denote a condition where       the walls. Each layer of gas parallel to the
no leakage exists until a critical pressure    direction of flow exerts a tangential force
or temperature is reached. At this point,      on the adjacent layer, tending to decrease
the leakage appears suddenly and may be        the velocity of the faster moving layers
appreciable. Further changes in pressure       and to increase that of the slower moving
or temperature cause the leakage to vary       layers. The property of a gas or liquid by
in the prescribed manner. When the             virtue of which it exhibits this
pressure or temperature is reversed, the       phenomenon is known as internal
leakage follows the prescribed course to       viscosity.
the critical point at which leakage drops
to zero. No adequate explanation for this          The internal viscosity is directly
phenomenon is advanced, but in view of         proportional to the velocity gradient in
the very few times this occurs, such leaks     the gas. Furthermore, the viscosity must
can generally be ignored. Temperature          depend on the nature of the fluid. In a
and pressure are not normally applied in       more viscous fluid the tangential force
the course of leak testing for the purpose     between adjacent layers for constant
of locating such leaks. Instead, they are      velocity gradient will be greater than in a
used to force existing discontinuities to      less viscous fluid. For any gas at constant
open, so as to start or increase the leakage   temperature, the gas viscosity is
rate to a point of detection.                  independent of the pressure. However, gas
                                               viscosity increases as gas temperature
Physical Properties of                         rises. Conversely, the viscosity of all
Tracer Gases Used in Leak                      ordinary liquids decreases with increased
Testing                                        temperature.
When performing any leak test it is
important to have some knowledge of the
residual gases present in the test area
because this will have a bearing on the
choice of tracer gas and test technique to
                                                                                                                            Tracer Gases in Leak Testing 47
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PART 3. Practical Measurement of Leakage
Rates with Tracer Gases
Principles of Leakage                         Criteria to Determine Type
Measurement                                   of Gas Flow through Leaks
All leak detection with tracer gases          The type of flow that occurs through leaks
involved their flow from the high pressure    depends on the factors listed earlier. In
side of a pressure boundary through a         flow systems encountered in leak testing
presumed leak to the lower pressure side      with gases, the length of the mean free
of the pressure boundary. When tracer         path of the gaseous molecules can be used
gases are used in leak testing, instruments   to estimate the type of flow occurring
sensitive to tracer gas presence or           through leakage paths. (The mean free
concentration are used to detect outflow      path lengths for various gas molecules can
from the low pressure side of the leak in     be calculated by means of Eq. 15 or 16.
the pressure boundary.                        Tables 4 and 5 give data on mean free
                                              path lengths for several gases and pressure
    Where leak tests involve measurements     ranges.) When determining the nature of
of change in pressure or change in            flow of gases through leaks, use is made of
volume of gas within a pressurized            two parameters: (1) the mean free path
enclosure, the loss of internal gas pressure  length λ is determined by using the
or volume indicates that leakage has          average pressure in the leak flow system.
occurred through the pressure boundary.
When evacuated or low pressure test               The criteria that determine the mode of
systems or components are surrounded by       gas flow through leaks, given in terms of
higher pressure media such as the earth’s     the mean free path length λ and the leak
atmosphere, or a hood or test chamber         dimensional constant d, are as follows.
containing gases at higher pressures,
leakage can be detected by loss of pressure    1. When the ratio λ·d–1 is less than 0.01,
in the external chamber or by rise in              the gas flow is viscous.
pressure within the lower pressure system
under test.                                    2. When the ratio λ·d–1 has values
                                                   between 0.01 and 1.00, the gas flow is
Modes of Gas Flow                                  transitional.
through Leaks
                                               3. When the ratio λ·d–1 is greater than
For each type of leak test, it is essential        1.00, the gas flow is molecular.
that the test operator have a basic
understanding of the types of flow that       In molecular flow, the mean free path
might occur in a leak. Different basic laws   length is greater than the largest linear
relate leakage rate to pressure difference    dimension of the cross section of the leak.
across the leak, the range of absolute
pressure involved and the nature of the       Relation of Viscous
gaseous fluid escaping through the leak.      Leakage Flow to Pressure
There are three basic types of gas flow       Differential across Leaks
through leaks.
                                              Viscous flow occurs when the mean free
 1. Viscous flow typically occurs in probing  path length of the gas is significantly
     applications with gases leaking at       smaller than the cross section of a leak.
     atmospheric or higher pressures.         This condition is implied by the first
                                              criterion above, where λ is at least 100
 2. Molecular flow usually occurs in leaks    times smaller than the leak’s cross
     under vacuum testing conditions.         sectional diameter d. Viscous flow occurs
                                              in high pressure systems such as in
 3. Transitional flow occurs under test       probing applications where tracer gases
     conditions intermediate between          leak into air at atmospheric pressures.
     vacuum and pressures higher than         With viscous flow through leaks, the flow
     atmospheric pressure.                    rate or leakage Q is proportional to the
                                              difference in the squares of the pressures
Figure 7 shows the range of conditions of     acting across the leak. This relationship is
gas pressure and leak radius under which      shown by Poiseuille’s law for viscous flow
each of these types of flow is typically      through a cylindrical tube, in Eqs. 21 and
encountered, for leakage flow of air.         22 for the leakage rate Q:
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( )π r 4                                                  in the discussion above. Molecular flow
                                                                    usually occurs through leaks in vacuum
(21) Q = 8 n l Pa P1 − P2                                           systems or systems that have vacuum
                                                                    applied to the lower pressure side of the
or                                                                  pressure boundary for purposes of leak
                                                                    testing. With molecular flow through
( )(22) Q = π r4                                                    leaks, the leakage rate Q is proportional to
                   16 n l                                           the difference in pressures applied across
                                            P12 − P22               the leak. This relationship is shown by
                                                                    Knudsen’s law for molecular flow through
where Q is gas flow rate (Pa·m3·s–1), r is                          a cylindrical tube, neglecting the end
                                                                    effect, as shown in Eq. 23 for the leakage
radius of leakage tube (meter), l is length                         rate, Q through a tubular leak with
                                                                    molecular flow:
of leakage tube (meter), n is viscosity of
                                                                    (23) Q = 3.342 r3
leaking gas (Pa·s), P1 is upstream gas                                                             l
pressure (pascal), P2 is downstream
pressure (pascal) and Pa is average pressure
within leak path, (P1 + P2)/2 (pascal).
                                                                                                          RT  (P1 − P2 )
                                                                                                          M
Relation of Molecular                                               where Q is leakage rate (Pa·m3·s–1), r is
Leakage Flow to Pressure
Differential across Leaks                                           radius of leakage tube (meter), l is length
Molecular flow occurs when the mean                                 of leakage tube (meter), M is molecular
free path length of the gas molecules is
greater than the largest cross sectional                            weight of gas (kilogram per mole), P1 is
dimension of a physical leak. This                                  upstream pressure (pascal), P2 is
condition is implied by the third criterion                         downstream pressure (pascal), T is
                                                                    absolute temperature (kelvin); and gas
                                                                    constant R = 8.315 J·mol–1·K–1.
FIGURE 7. Types of flow characteristics of tracer gases though leaks as function of leak channel
radius and gas pressure. Graph illustrates air at 25 °C (77 °F).
          105 (4 × 103)
                          104 (4 × 102)
                          103 (4 × 101)                                                          Viscous
                          102 (4 × 100)
Radius of tube, mm (in.)  101 (4 × 10–1)                                       Transition
                          100 (4 × 10–2)
                          10–1 (4 × 10–3)                           Molecular
                          10–2 (4 × 10–4)
                          10–3 (4 × 10–5)
                          10–4 (4 × 10–6)
                          10–5  (4 × 10–7)
                                            10–4  10–3  10–2  10–1  100        101         102 103            104        105
                                                                                                                         (15)
                                ( 1.5×10–8)(1.5×10–7)(1.5×10–6)(1.5×10–5)(1.5×10–4)(1.5×10–3)(1.5×10–2)(1.5×10–1) (1.5)
                                                              Absolute pressure, Pa (lbf·in.–2)
                                                                                                                            Tracer Gases in Leak Testing 49
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If this value is substituted for R in      ( )(29) Q = 3.342 r3    RT
Eq. 23, the leakage rate in SI units is given                             lM
by Eq. 24:                                                                 P1 − P2 FT
( )(24) Q = 9.637 r3       T                       For Eq. 28 and 29, the symbols are
                               lM
                              P1 − P2          explained below Eq. 23, with the
                                               exception of the mean free path length λ,
If the molecular mass M is given in units      which is determined at the average
of grams per mole. All other quantities are
in SI units as listed above. The leakage       between upstream and downstream
rate in SI units of Pa·m3·s–1 is given by Eq.
25:                                            pressures acting across the leak, namely
                                               (P1 + P2)/2, from Eq. 15 or 16 and Tables 4
                                               and 5.
( )(25) Q = 304.8 r3       T
                               lM
                              P1 − P2          Analogy between Electrical
                                               Conductance and Gaseous
    In cgs (centimeter-gram-second) units,     Conductance
with tube radius and length given in
centimeter and molecular weight in gram        Conductance is a term describing the
per mole, the rate of leakage (L·s–1) is       property of a gas flow system that permits
given by Eq. 26:                               gas to flow. It is defined analogously to
                                               electrical conductance G, the reciprocal of
( )(26) Q = 30.48 r3       T                   electrical resistance R. Ohm’s law for
                               lM              direct current flow i through a
                              P1 − P2          conductance or resistance is stated in
                                               Eq. 30:
This flow rate is related to the flow rate Fo
for zero thickness orifice:
(27) F   =  8  r  Fo                           (30) i = V = V G
            3  l                                                  R
where both F and Fo are flow rates (L·s–1).        In Eq. 30, the quantity V equals the
                                               voltage drop across the resistance R or
Relation of Transitional                       conductance G. Electrical conductance
Leakage Flow to Mean                           could be described as the property of an
Free Path Length of Gas                        electric circuit that permits current to
and to Pressure                                flow. In steady state direct current circuits,
Differential Applied across                    the conductance G is the ratio of the
Leak Path                                      current i flowing in the resistive element
                                               to the drop in electrical potential (or
                                               electrical pressure) across the resistive
                                               element, as in Eq. 31 for the electrical
                                               conductance G:
Transition flow occurs when the mean           (31) G = 1 = i
free path length of the gas molecules is                           RV
about equal to the cross-sectional
dimension of the leak. Transitional flow           With gas flow through the
occurs under leakage conditions                conductance of a leak path, for example,
intermediate between those for viscous         the flow rate Q is analogous to the electric
flow and those for molecular flow. For         current i. The pressure drop (P1 – P2) is
transitional flow, Knudsen’s law (see          analogous to the voltage drop V. Leak
Eqs. 23 to 27) for molecular leakage is        conductance C is analogous to the
modified by an additional term that            electrical conductance G. The electrical
depends on the ratio R equal r/λ or            current could be considered as the leakage
leakage tube radius r to the mean free         of electrical charge through a resistive
path length λ that applies for the average     element such as a length of wire of given
pressure (P1 + P2)/2, existing within the      diameter and specific conductivity. The
leakage path. This correction term for         gaseous conductance of a tubular
transitional flow in leakage paths is given    passageway permits the leakage of a
as the factor FT, defined by Eq. 28 where      gaseous constituent when a pressure drop
Rt = r/λ:                                      exists between the ends of the tubular
                                               hole. The gaseous conductance is the
(28) FT  =  0.1472 R t  +  1 + 2.507 Rt        reciprocal of the resistance of the leak
                           1 + 3.095 Rt        passageway, as indicated by Eq. 32 for the
                                               gaseous conductance C:
The leakage rate Q in SI units of Pa·m3·s–1
is given by Eq. 29:                            (32) C = 1 =                Q
                                               R gas                   P1 − P2
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The equivalent of Ohm’s law for a gas         The conductance for molecular flow of
conductance would be the linear               gases through a long cylindrical tubular
relationship of Eq. 33 for the rate Q of      leak channel can be calculated from
leakage or of gas flow:                       Eq. 36:
( )(33) Q = P1 − P2 =                         (36) C = 3.342 r3                   RT
                       R gas                                                l     M
                                  P1 − P2 C
However, Eq. 33 is only true for the case         The conductance of a leak that can be
of molecular flow, as shown in Eqs. 23        approximated by an ideal orifice subject
to 27.                                        to molecular flow at low pressure is
                                              calculated by Eq. 37:
    It is very important to keep in mind
that, by definition, the relationships of     (37) C = 3.613 r 2 T
gaseous conductance calculations always                                            M
include a term describing a property of
the flowing gas. This property usually is         The conductance of a long tubular leak
the gas viscosity that influences viscous     with transitional gas flow can be
flow through leaks or is the gas molecular    calculated from Eq. 38:
mass that influences molecular flow
through leaks.                                (38) C = 3.342 r 3                  T
                                                                            P     M
                                                                                      FT
Equations for Calculating                     In Eq. 38, the factor FT is the correction
Conductances of Leaks                         term for transitional flow defined earlier
with Various Modes of
Flow                                          by Eq. 28.
The following equations give basic            Gas Conductance with Two Leaks
relationships required to calculate leak      in Series
conductances under various conditions of
leak geometry and of modes of gas flow        If two different diameter leaks with
and to estimate variations of leakage rate    different conductance values are
with different gas pressures.                 connected in series as in Fig. 8, the total
                                              conductance of the connection between
    The conductance of a leak exhibiting      extreme ends decreases (resistance
viscous flow of gas can be calculated by      increases). From Eq. 33, the conductance
Eq. 34, assuming that the physical leak       of the leak between the outer ends of
channel approximates a straight,              sections 1 and 3 may be expressed as in
cylindrical tube: The viscous conductance     Eq. 39:
C of a tube is expressed as follows:
                                              (39) C1−3  =      Q
                                                            P1 − P3
           πr4
(34) C  =  8nl  Pa                                The total pressure drop across the two
                                              leaks in series is given by Eq. 40:
    In Eqs. 34 through 38 for calculating
                                              FIGURE 8. Diagram of typical leak paths connected in series.
the conductance of leaks, C is gas
conductance (m3·s–1), r is radius of bore of                                      Wall of
                                                                                  system
tube (meter), l is length of tubular leak
                                                      Inside                      P2 chamber             Atmosphere
passageway (meter), n is viscosity of         P1 of                                                      P3
leaking gas in Pa·s, P1 is upstream pressure         system                                   C23
(pascal), P2 is downstream (pascal), Pa is
average gas pressure within leak channel                          C12
(pascal), Pa = (P1 + P2)/2, M is molecular               Tracer                                  Outer
mass of gas g·mol–1 and T is absolute                                                         capillary
                                                                    Inner
temperature (kelvin).                                               capillary
    If viscous leakage occurs through an
ideal orifice where the ratio P2/P1 of
downstream to upstream pressures is
smaller than or equal to 0.52, the
approximate conductance for viscous flow
through an ideal orifice can be calculated
by the empirical Eq. 35:
(35) C = 6.4 r 2               T              Legend
                    1 − P2     M
                           P1                   C = channel connecting points
                                                P = point where fluid is present
                                                                                                                            Tracer Gases in Leak Testing 51
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( ) ( )(40) P1 − P3 = P1 − P2 + P2 − P3       ( )(46) Qa = Ca P1 − P2 = Ca ∆ P
    The pressure drop across each             ( )(47) Q b = Cb P1 − P2 = Cb ∆P
individual leak is shown in Eq. 41:
(41) P1 − P2   =    Q,                            The total conductance through the
                  C1−2                        pressure boundary between Points 1 and 2
                                              is given by Eq. 48:
      P2 − P3  =    Q                         (48) C1−2  =  Ca ∆ P + Cb ∆ P
                  C 2 −3                                             ∆P
Now, by combining Eqs. 39 to 41, the          Simplifying Eq. 48 gives Eq. 49:
conductance C13 for the two leaks in          (49) C1−2 = Ca + Cb
series is given by Eq. 42:
(42) C13 =            Q                           In its general form, the total
               Q +Q                           conductance for n individual leaks
               C1−2          C 2 −3           connected in parallel is given by the sum
                                              of the individual conductances as in
or, in its reciprocal form,                   Eq. 50:
               Q +Q                           (50) CT = C1 + C2 + C3 + … + Cn
(43) 1 = C1−2                C 2 −3
      C13 Q
          = 1+1                               Graphical Determination
               C1−2          C 2 −3           of Conductance for
                                              Molecular Flow through
In its general form, Eq. 43 may be written    Tubes and Orifices
as Eq. 44:
                                              The preceding equations give the
(44)   1  = 1 + 1 +…+ 1                       relationships required to calculate
      CT       C1 C2                 Cn       conductance under various conditions. In
                                              practice, calculation of the exact
where the subscript T denotes the total       conductance often is not required in leak
                                              testing. Also, it has been found that most
conductance of a number of conductances       needed conductance values are for
                                              molecular flow through cylindrical tubing
C1, C2, C3 … Cn connected in series.          and orifices. Figures 10 and 11 have been
    In the case of only two conductances      provided to allow quick determinations.
                                              Note that the curves are plotted for air at
connected in series, Eq. 44 should be         20 °C (68 °F) and values must be corrected
                                              if another gas or temperature is used.
written in the form of Eq. 45:
(45) CT   = C1 × C2
               C1 + C2
This case applies for two successive leak     FIGURE 9. Diagram of typical leak paths connected in
conductances connected in series. This is     parallel.
analogous to the case of two electrical
resistors connected in parallel or of two
electrical conductances connected in series.
Leak Conductance for Two                      Inside of       Wall of system         Atmosphere
Leaks Connected in                              system                               P2
Parallel                                              P1    Ca
                                                                                 Cb
Figure 9 shows the case of two leaks
connected in parallel. With this situation,   Legend
the total leakage through two parallel
leaks divides between the two leakage           C = channel connecting points
paths from the high pressure side to the        P = point where fluid is present
low pressure side of the pressure
boundary. The division of flows depends
on the conductance of the individual
leaks as indicated in Eqs. 46 and 47:
52 Leak Testing
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Improvement of Viscous                       Effect of Variations in
Flow Leak Test Sensitivity                   Tracer Gas Concentration
by Increasing Pressure
Differential                                 Under viscous flow conditions, which are
                                             usually encountered when leak testing
The change in leakage rate obtained by       pressurized systems, the flow rate increase
                                             resulting from higher pressure differentials
increasing the pressure applied to a leak    may also be used to conserve tracer gas. In
                                             a mixture of two gases such as helium and
to atmosphere is used to great advantage     nitrogen, each gas will flow through a
                                             leak at the same rate regardless of their
in leak testing under conditions where the   concentrations in the mixture. Thus, if a
                                             10 percent tracer gas in 90 percent carrier
leakage flow is viscous in nature, as        gas mixture is used, the test sensitivity
                                             will be 10 percent of what it would be if
illustrated in Fig. 12. For example,         100 percent tracer gas were used at the
                                             same working pressure. To bring the test
suppose that the leakage rate is             sensitivity back to a leakage rate increase
1 × 10–8 Pa·m3·s–1 (1 × 10–7 std cm3·s–1)    ratio of 1, the pressure would have to be
from a system with an internal gage          raised enough to increase the flow by a
                                             factor of 10. Suppose that a tank must be
pressure of 1 atm (absolute internal         brought to an absolute pressure of 10 MPa
                                             (1.5 × 103 lbf·in.–2) and leak tested with
pressure of 200 kPa or 2 atm), as indicated  helium. To save money, it is desired (1) to
                                             use the smallest amount of helium that
by point P1 in Fig. 12. It is desired to     will give adequate sensitivity and (2) to
determine the new absolute internal
pressure P2 needed to make the leakage
rate 50 times higher, or 5 × 10–7 Pa·m3·s–1
(5 × 10–6 std cm3·s–1). From Fig. 12, the
new flow rate at Point P2 is seen to be
obtained with an absolute internal
pressure of 1.23 MPa (12.3 atm), as shown
on the horizontal scales.
FIGURE 10. Conductance of cylindrical tubes of different lengths and inside diameters for air
at 20 °C (68 °F). 1 L = 1 dm3 = 0.028 ft3.
                        Conductance (L·s–1)
10–2           10–1  1                       10 102 103
0.01
       0.02
               0.04
                    0.06
                       0.08
                          0.1
                                 0.2
                                         0.4
                                             0.6
                                                 0.8
                                                   1.0
                                                           2.0
                                                                   4.0
                                                                       6.0
                                                                          8.0
                                                                             10
                                                                                    20
                                                                                            40
                                                                                                60
                                                                                                    80
                                                                                                      100
                                                                                                              200
                                                                                                                     400
                                                                                                                          600
                                                                                                                             800
                                                                                                                                 1000
20             Inside1do00if8a9tmmu7mbme5temem6(5s4r20(sm3immn.53(.mm3)8i.n0m((.2)2imn..502.)5(ii2nn1m2...)5)mm2in0m1.()61m(.m00m1.3mi8n(71m.0)5(0.07mi.m5n6.(2im)0n5..56)(in0im.n.)3.m5)75m(0imn4.2.)m5(0m3i.n1m.8()08m.1in6(0.)i.n1.2)5 in.)     1000
Length of tube (m)10                                                                                                                                                                                                                                 800
                                                                                                                                           Length of tube (in.)                                                                                      600
 5                                                                                                                                                                                                                                                   400
               10–4  10–3                    10–2  10–1
 2                                                                                                                                                                                                                                                   200
 1
 0.5                                                                                                                                                                                                                                                 100
                                                                                                                                                                                                                                                       80
 0.2                                                                                                                                                                                                                                                   60
 0.1                                                                                                                                                                                                                                                   40
 0.05
                                                                                                                                                                                                                                                       20
 0.02
 0.01                                                                                                                                                                                                                                                  10
 0.005                                                                                                                                                                                                                                                   8
 0.0025                                                                                                                                                                                                                                                  6
                                                                                                                                                                                                                                                         4
         10–5
                                                                                                                                                                                                                                                         2
                                                                                                                                                                                                                                                         1.0
                                                                                                                                                                                                                                                         0.8
                                                                                                                                                                                                                                                         0.6
                                                                                                                                                                                                                                                         0.4
                                                                                                                                                                                                                                                         0.2
                                                                                                                                                                                                                                                         0.1
                                                                                                                                                                                                                                                100
                     Conductance (m3·s–1)
                                                                                                                            Tracer Gases in Leak Testing 53
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FIGURE 11. Conductance of orifices for air at 20 °C (68 °F), molecular flow. For curve A read
left vertical scale; for curve B read right vertical scale (1 m3 = 35 ft3).
10–1                                                              100
Conductance (m3·s–1)10–2       A                    B                                                                                10
                                               Read left scale10–3                                                                    1.0
                                                                                  Read right scale
                                                                                                                 Conductance (m3·s–1)
10–4                                                                                                                                 0.1
10–5                                                                                                                                 0.01
                 2.5                        25              250   2000
                 (0.1)                    (1 . 0 )          (10)  (100)
                               Orifice diameter, mm (in.)
FIGURE 12. Viscous leakage rate as function of internal pressure of system leaking to
atmosphere when pressurizing with 100 percent gas. For curve A read left vertical scale, for
curve B read right vertical scale.
                 Internal absolute pressure (atm) at 1 atm
          1                       10 100 1000
100                                                                                               100 000
50 P2 = 1.23 MPa (12.3 atm)
                            A
10
Leakage rate increase ratio                                 B
                                                                                                                  Leakage rate increase ratio10 000
1.0                                                               1000
                    P1 = 200 kPa (2 atm)
0.1                                103                104                 100
                                  (147)             (1470)
    102 2 × 102                                                     105
   (14.7)                                                         (14 700)
      Internal pressure, kPa (lbf·in.–2), outside of part at 100 kPa (1 atm)
54 Leak Testing
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pressurize the rest of the way with            Effect of Increasing
                                               Pressure Differential across
nitrogen. The minimum detectable               Molecular Leak Flow
leakage should be at least                     Figure 14 shows the effect of changing the
1 × 10–8 Pa·m3·s–1 (1 × 10–7 std cm3·s–1) at   pressure differential across a leak when
100 kPa (1.0 atm) pressure differential. It    the flow conditions are molecular. As
                                               would be predicted by Eq. 23, the increase
is desired to calculate the percentage of      of gas flow is a linear function of pressure.
                                               Under conditions of molecular flow, the
helium that should be used after reaching      amount of tracer gas flowing through a
                                               leak is not a function of the total pressure.
an absolute pressure of up to 10 MPa           It depends only on the partial pressure of
(1.5 × 103 lbf·in.–2).                         the tracer gas. Therefore, there would be
                                               no advantage in raising the total pressure
    The specified minimum detectable           difference without raising the tracer gas
leakage rate of 1 × 10–8 Pa·m3·s–1             pressure.
(1 × 10–7 std cm3·s–1) requires that the leak
test sensitivity be standard or the same as    Conversions between
                                               Leakage Rates with
it would be if 100 percent tracer was used     Different Tracer Gases
at 100 kPa (1 atm) pressure difference.        Many occasions will arise where it will be
                                               necessary to express a leakage rate (flow
From Fig. 12 it is seen that an absolute       rate) or conductance in terms of a
                                               particular tracer gas when it has been
pressure of 10 MPa (100 atm) results in a      measured using a different tracer gas. For
leakage rate increase factor of 3300. Thus,
the helium concentration after pressuring
up should be 1/3300 or 0.03 percent.
Figure 13 is very similar to Fig. 12 and is
used in the same manner. The difference
is that Fig. 13 is plotted for conditions
where high vacuum is on the low pressure
side of the pressure boundary. Figure 13
still assumes viscous flow conditions.
FIGURE 13. Viscous leakage rate as function of pressure differential during vacuum testing,
pressurizing with 100 percent tracer gas. Read left vertical scale for curve A and right vertical
scale for curve B.
          1  Internal absolute pressure (atm)          1 000
                  10 100                                     1 000 000
1 000
 800                                                           500 000
 600
 400
Leak rate increase ratio
200
                                           Read left scale
                                                                                      Read right scale100
                                                                                                                   Leak rate increase ratio
80           A                                                                  100 000
60
                                                                                  50 000
40                                             B
20
10 10 000
 8
 6
                                                                                                            5 000
 4
 2
1                103                             104                1 000
                (147)                          (1470)
   102                                                    105
 (14.7)                                                (14 700)
             External pressure, kPa (lbf·in.–2 ) inside part at high vacuum
                                                                                                                            Tracer Gases in Leak Testing 55
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example, a specification may state that a          n2 is viscosity (same units as gas 1) for
                                   certain part cannot leak more than a               gas 2.
                                   given amount for air, but helium tracer
                                   gas is used in testing. To be able to              Conversion of Viscous
                                   convert a measured helium leakage rate to          Conductance between Different
                                   an equivalent air leakage rate, the type of        Gases
                                   flow must first be identified. After the
                                   flow type is determined, the conversion            Dividing both sides of Eq. 51 by the
                                   may be made. Also, many times the                  pressure drop will give conductance C
                                   conductance for a piece of tubing or other         rather than flow Q. Any two conductances
                                   item must be determined. Conductance is            C1 and C2 will then have a relationship
                                   the part of the flow equations that                given in Eq. 52:
                                   contains the term describing either
                                   molecular mass or viscosity of the gas that        (52) C2  =  n1  C1
                                   is flowing. The conductance of a given                         n2
                                   system will be quite different for two
                                   gases having different properties. In leak         where C1 is conductance (any units) for
                                   testing work, this situation is encountered        gas 1, C2 is conductance (same units as
                                   where the pumpdown time of a system                gas 1) for gas 2, n1 is viscosity (any units)
                                   for air must be determined and then                for gas 1 and n2 is viscosity (same units as
                                   response and cleanup times for helium              gas 1) for gas 2.
                                   must be determined.
                                                                                          A few comparisons that may be used
                                   Conversion of Viscous Flow Rates
                                   between Different Gases                            for converting higher conductance or flow
                                                                                      from helium flow rates to flow rates for
                                                                                      other gases are shown in Table 8.
                                   If a flow rate has been identified as              TABLE 8. Comparison of viscous flow rates
                                   viscous for one gas, the viscous flow for          of other gases with helium flow rates.
                                   any other gas may be determined using
                                   the expression given in Eq. 51:
                                   (51) Q2  =  n1  Q1                                 To Convert to       Multiply Helium
                                               n2                                                              Flow by
                                   where Q1 is flow rate (any units) for gas 1,       Q of argon              0.883
                                   Q2 is flow rate (same units as gas 1) for gas      Q of neon               0.626
                                   2, n1 is viscosity (any units) for gas 1 and       Q of hydrogen           2.23
                                                                                      Q of nitrogen           1.12
                                                                                      Q of air                1.08
                                                                                      Q of water vapor        2.09
FIGURE 14. Molecular leakage rate as function of pressure                             Conversion of Molecular Flow
differential in vacuum leak testing, pressurizing with                                Rates between Different Gases
100 percent tracer gas.
                                                                                      If molecular flow occurs, the flow rate for
         1000                                                                         one gas may be compared to the flow rate
           800                                                                        for any other gas by Eq. 53:
           600
           400
                          200                                                         (53) Q2 =   M1      Q1
                                                                                                  M2
Leak rate increase ratio  100
                           80                                                         where Q1 is flow (any units) for gas 1, Q2
                           60                                                         is flow (same units as gas 1) for gas 2, M1
                                                                                      is molecular mass for gas 1 and M2 is
                           40                                                         molecular mass for gas 2.
                          20
                          10                                                          Conversion of Flow Rates for
                           8                                                          Molecular Conductance
                           6
                           4                                                          The conductance under conditions of
                                                                                      molecular flow for one gas may be
                           2                                                          compared to the conductance for another
                                                                                      by using the expression of Eq. 54:
                          1                 1.0 10 100
                              0.1
                                   (10)                (100)                  (1000)              M1
                              (1)                                                                 M2
                                   Absolute external pressure inside of part          (54) C2 =           C1
                                           at high vacuum, MPa (atm)
56 Leak Testing
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where C1 is conductance (any units) for      Test Variables Limiting
gas 1, C2 is conductance (same units as      Leak Testing Sensitivities
gas 1) for gas 2, M1 is molecular mass for
gas 1 and M2 is molecular mass for gas 2.    Some factors that prevent leak testing
                                             devices from attaining their ultimate
    A few comparisons that may be used       sensitivities include geometry, sampling
                                             efficiency, tracer economy and noise (or
for converting either conductance or flow    contamination). Geometry enters the
                                             picture because any instrument should
are given in Table 9.                        and must respond only to local
                                             conditions at its sampling inlet. Two
TABLE 9. Comparison of molecular flow        things are of interest in the leak
rates of other gases with helium flow        evaluation process: the space coordinates
rates.                                       of the leaking orifice and the mass rate of
                                             leakage. The effects of leak location and
To Convert to     Multiply Helium            leakage rate on the concentration of tracer
                       Flow by               at the instrument depend on convection
                                             and diffusion of the tracer gas.
Q of argon            0.316
Q of neon             0.447                      Sampling efficiency may be thought of
Q of hydrogen         1.410                  both as a measure of how nearly all of the
Q of nitrogen         0.374                  quantity to be measured is used in
Q of air              0.374                  making the measurement and as a
Q of water vapor      0.469                  measure of how well extraneous responses
                                             can be excluded. Many leak detectors
Effect of Temperature on Gas                 must operate with their active parts in a
Conductance with Molecular Flow              partial vacuum. This limits the rate at
                                             which samples of the surrounding air can
The effect of temperature on conductance     be ingested for analysis. Other leak testing
when the flow is molecular should not be     instruments may take in the sample so
overlooked. As can be seen in Eq. 35 and     violently that extra turbulences are
36, the conductance changes in direct        created near the sampling point. The
proportion with the square root of gas       sampling problem is somewhat
temperature. The expression of Eq. 55 is     interrelated with the noise and
for a variation in gas conductance           contamination problem.
resulting from a change in temperature
only, with pressure and dimensions               The ultimate sensitivity of most leak
remaining constant:                          testing instruments is quoted on the basis
                                             of 100 percent tracer concentration in the
(55) C2 =  T2     C1                         system or, equivalently, on the amount of
           T1                                tracer leaking. In a practical situation this
                                             concentration is necessarily kept down for
where C1 is conductance at temperature       reasons of safety or economy and
T1; C2 is conductance at temperature T2;     sometimes because of corrosiveness of the
T1 is starting temperature, kelvin; and T2   tracer. With reduced tracer concentration,
is new temperature in kelvin. T1 and T2      the leakage sensitivity is reduced
must be absolute temperatures.               proportionately. With 1 percent tracer
                                             concentration the sensitivity figure is
Relative Sensitivities of                    correspondingly reduced by a factor of
Leak Testing Techniques                      100.
When choosing a test technique it is         Control of Ambient
advantageous to have an insight into the     Concentrations of Tracer
relative sensitivities of the various        Gases
techniques. Obviously, the test sensitivity
does not equal the published ultimate        Changes in tracer gas concentration due
sensitivities of the various detecting       to leaks are self obscuring in the presence
devices because of many variables.           of random variations in the ambient
Table 10, showing relative sensitivities,    tracer gas concentration. Background
may be used to assist in choosing            levels of tracer gas in the atmosphere
potentially satisfactory leak testing        disturb the predicted gas concentration
techniques.                                  pattern. The problem of distinguishing
                                             leaks from increasing and randomly
                                             varying background contamination may
                                             reduce instrument sensitivities by orders
                                             of magnitude or even destroy test
                                             sensitivity altogether.
                                                                                                                            Tracer Gases in Leak Testing 57
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TABLE 10. Relative ultimate leakage sensitivities of various leak testing methods under
ideal conditions with very high concentrations of tracer gases. (These numbers are not
intended to be used as guides in practical leak testing.)
                                             ______________L_e_a__k_a_g_e__R_a_t_e________________
Minimum Detectable Leakage Test Technique    Pa·m3·s–1      (std cm3·s–1)
Pressure drop using liquids                  Depends on volume tested and gage range
Pressure drop using gases
Pressure rise                                       Depends on volume tested
Ultrasonic leak detector
Volumetric displacement (gas flow meter)            Depends on volume tested
Gas discharge
Ammonia and phenolphthalein                  10–2           (10–1)
Ammonia and bromocresol purple
Ammonia and hydrochloric acid                10–3           (10–2)
Ammonia and sulfur dioxide
Halide torch                                 10–3           (10–2)
Air bubble in water
Air and soap or detergent                    10–3 to 10–4   (10–2 to 10–3)
Thermal conductivity
Infrared                                     10–3 to 10–4   (10–2 to 10–3)
Hydrogen Pirani technique
Hot filament ionization gage                 10–3 to 10–4   (10–2 to 10–3)
Mass spectrometer detector probe
Halogen diode detector                       10–3 to 10–4   (10–2 to 10–3)
Hydrogen bubbles in alcohol
Palladium barrier detector                   10–4           (10–3)
Mass spectrometer envelope
Radioactive isotopes                         10–4 to 10–5   (10–3 to 10–4)
                                             10–4 to 10–5   (10–3 to 10–4)
                                             10–5           (10–4)
                                             6 × 10–4 to 6 × 10–5 (6 × 10–3 to 6 × 10–4)
                                             10–7           (10–6)
                                             10–7 to 10–8   (10–6 to 10–7)
                                             10–6 to 10–8   (10–5 to 10–7)
                                             10–7 to 10–9   (10–6 to 10–8)
                                             5 × 10–7       (5 × 10–6)
                                             10–8 to 10–9   (10–7 to 10–6)
                                             10–10          (10–9)
                                             10–9 to 10–13  (10–8 to 10–12)
    Any gas tracer system, no matter how     gas concentration that are caused by
sensitive, that responds to the simple       accumulated leakage or by venting tracer
absolute level of concentration will soon    gases. The need for controlled
become incapable of detecting leakage        environment and ventilating systems is
when the ambient tracer concentration        minimized. The reference intake of the
rises to the level capable of giving         differential detector is prevented from
spurious signals. This is the major failing  sampling in the immediate area of the
of the simple halogen leak detector.         leak to avoid fast transients and confusing
                                             indications. However, the differential
    Two solutions to the background          detector leak sensor is less sensitive than
problem immediately present themselves:      either the heated anode halogen leak
(1) keep the ambient concentration low       detector or the helium mass spectrometer
and (2) use a gradient sensor (differential  leak detector.
detector). One such instrument actually
has two separate detection cells
(Chambers where the temperature
compensator detects are mounted). Each
cell has an individual intake port. The
dual detectors continually compare the
thermal conductivity of the sample gas
(from potential leakage sources) with that
of the ambient atmosphere. When the
sample cell intake is not near a leak, the
two detection cells are sampling the same
gas concentration and their combined
output is zero, giving no output reading.
Only when the leak area is encountered
by the leakage sample intake does the
instrument respond.
    The differential detector prevents
interference from gases in the atmosphere
and working area. It eliminates the need
for selectivity to any particular gas. Leak
testing can be performed in areas of high
58 Leak Testing
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PART 4. Mathematical Theory of Gas Flow
through Leaks
Mechanisms of Mass                           Because turbulent flow is rarely
Transfer in Gas Flow                         encountered in leaks, the term viscous
                                             flow is sometimes incorrectly used to
Mass transfer attributed to leakage can      describe laminar flow in leak testing work.
occur in two modes: pneumatic flow and
permeation. Pneumatic flow occurs when           The most familiar laminar flow
leakage is by passage of fluid through       equation was developed by Poiseuille.
finite holes. Permeation is passage of a     Poiseuille’s equation for laminar flow
fluid into, through and out of a solid       through a straight tube of circular cross
barrier having no holes large enough to      section is given in Eqs. 21 and 22.
permit more than a small fraction of the     Poiseuille’s equation has been
molecules to pass through any one hole.      substantially verified experimentally and
                                             is applicable where the length and
Leakage Rates for                            diameter of the flow passage are known.
Different Modes of                           This is not the case for most leaks.
Pneumatic Flow of Gas in                     Equation 21 can be rewritten in the form
Leaks                                        of Eq. 56:
Pneumatic gas flow in leaks may be           (56) Q  =   K Pa  P1  −  P2
placed in five categories: turbulent,                              n
laminar, molecular, transition and choked
leakage flows. The approximate ranges of     K represents the constants of the two
flow rates for various pneumatic modes of    geometry factors of length l and diameter
gas flow follow.                             d of the tubular leak passage, as shown in
                                             Eq. 57:
 1. Turbulent flow occurs with leakage
     rate above 10–3 Pa·m3·s–1               (57) K = πr4
     (10–2 std cm3·s–1).                                          8l
 2. Laminar flow occurs with leakage rates       Laminar flow takes place when the
     in the range from 10–2 to 10–7          Reynolds’ number of flow is lower than
     Pa·m3·s–1 (10–1 to 10–6 std cm3·s–1).   the defined critical value. The Reynolds’
                                             number is a unitless quantity that defines
 3. Molecular flow is most probable with     the flow conditions and is given by
     leakage rates below 10–6 Pa·m3·s–1      Eq. 58:
     (10–5 std cm3·s–1).
                                             (58) N Re   =  d ρF
 4. Transition flow occurs in the gradual                     n
     transition from laminar to molecular
     flow.                                   where NRe is Reynolds’ number, p is fluid
                                             density, n is gas viscosity, F is average flow
 5. Choked flow occurs when the flow
     velocity approximates the speed of      velocity across a plane in the tube and d is
     sound in the gas.
                                             diameter of the leak (compare with
Laminar and molecular flows are the
predominant modes of leakage flow in the     Eq. 20).
range of leakage rates of interest in most
leak testing.                                Reynolds’ Number for Ideal Gas
Characteristics of Laminar                   By substituting the ideal gas equation (see
(or Viscous) Flow                            Eq. 9) into Eq. 58, the expression for the
                                             Reynolds’ number for an ideal gas
The laminar flow of a fluid in a tube is     becomes Eq. 59:
defined as a condition where the velocity
distribution of the fluid in the cross       (59)  N Re  =  Q 4M
section of the tube is parabolic. Laminar                   d πn RT
flow is one of the two classes of viscous
flow, the other class being turbulent flow.  where M is molecular mass, R is molar gas
                                             constant, T is absolute temperature, Q is
                                             leakage rate, d is leak diameter and n is
                                             gas viscosity.
                                                 The critical value of Reynolds’ number
                                             has been shown to depend on the
                                                                                                                            Tracer Gases in Leak Testing 59
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entrance conditions, roughness of the          will increase the flow rate through this
walls of a tube and shape of the flow          leak by a factor of ten. Obviously then,
path. In general, for smooth tubes with        when the leaks to be measured are in the
well rounded entrances, the critical value     laminar flow range, the simplest way to
is about 1200.                                 increase leakage sensitivity is by an
                                               increase of pressure across the leak.
Equation for the Viscosity
of a Gas                                       Equations for the Mean
                                               Free Path of Gaseous
The kinetic theory of gases states that the    Molecules
viscosity of a gas is given by the
relationship of Eq. 60:                        The mean free path length is the average
                                               distance that a molecule travels between
(60) n =  m Fa                                 successive collisions with the other
                                               molecules of an ensemble. The mean free
          3 2 π σ2                             path λ of gas molecules is given by Eq. 64:
where Fa is a average velocity of the          TABLE 11. Mean free paths at 25 °C (77 °F), molecular
individual molecules, m is molecular           diameters, and viscosities for gases and vapors used in
                                               leak testing.
mass, σ is molecular diameter and n is
viscosity of gas. The average velocity of a
gas molecule is given by Eq. 61:
(61) F =  8RT                                                       Mean Free Molecular
          πM
                                                                    Path     Diameter Viscosity
The mass m of the individual molecules is      Gas                  (mm·Pa)  (pm)                                                                       (µPa·s)
given in terms of the molecular mass M of
a specific gas:                                Acetylene                                         9.2
                                               Air                                             16.9
(62) m = M                                     Ammonia               7.23
                     N                         Argon                 1.53                        9.4
                                               Benzene               4.49    358 20.8
In Eq. 62, N is Avogadro’s number, i.e.,       Carbon dioxide                765 6.9
number of molecules per mole.                  Carbon disulfide      3.21    465 13.5
Substituting Eq. 61 and 62 into Eq. 60         Carbon monoxide
results in Eq. 63 for the viscosity of a gas:  Dichloromethane      19.5                         8.9
                                               Ethane               12.2                       17.1
                     2 M RT                    Ethyl alcohol
(63) n =                                       Ethylene              5.27    537 8.5
                                               Refrigerant–11        1.86                        8.2
                   3 π3 N σ2                   Refrigerant–12        1.51                        9.3
                                               Refrigerant–21        1.31
Equation 63 shows that the viscosity of a      Refrigerant–22       13.70                      10.3
gas is independent of pressure and is          Refrigerant–113                                 11.8
proportional to the square root of             Refrigerant–114       6.99                      10.8
absolute temperature.                          Refrigerant–134a      2.32                      12.0
                                               Helium
Characteristics of Laminar                     Hydrogen              4.23                        9.8
Gas Leaks                                      Hydrogen sulfide
                                               Methane                       218 17.8
The two most important characteristics of      n–Butane                      275 8.3
laminar leaks shown by Eq. 21 and 22 are       n–Pentane
(1) the flow is proportional to the            n–Hexane                                        11.8
difference between the squares of the          Neon                          419 10.0
pressures upstream and downstream of           Nitric oxide                  706 10.0
the leak and (2) the leakage is inversely      Nitrogen                      782
proportional to the leaking gas viscosity.     Nitrous oxide                 842
Table 11 shows that the viscosity of most      Oxygen                        260
gases is similar. Therefore, a change of       Propane
leaking gas will not markedly increase the     Sulfur dioxide                                  17.8
sensitivity of the leak testing technique      Sulfur hexafluoride                             16.8
unless this change of gas implies a change     Water                                           13.3
of instrument sensitivity.                     Xenon                         364 19.1
                                                                             632 7.7
    However, as shown in Fig. 15,                                                              11.6
increasing the pressure difference across
the leak by a factor of a little over three                                  468 8.8
                                                                                               21.0
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(64) λ =                   1                          The molecular diameters and mean free
                                                                    2 π n1 σ2                  paths of typical leak testing gases and
                                                                                               vapors are listed in Table 11. As a
                                             where n1 is number of molecules in 1 cm3          convenient calculation guide, the mean
                                             volume and σ is molecular diameter. The           free path, in meters, of air at room
                                                                                               temperature is given by Eq. 67:
                                             molecular density n1 of gaseous molecules
                                             per unit volume is given by Eq. 65:               (67)  λ air  =  6.8 × 10−3
                                                                                                                      P
                                                                    mN
                                             (65) n1             =  MV                         The pressure P is expressed in pascal in
                                                                                               Eq. 67 (compare with earlier Eq. 16).
                                             where m is mass of gas, M is molecular
                                                                                               Equation for Molecular
                                             mass of gas, N is Avogadro’s number, i.e.,        Flow of Gases
                                             6.023 × 1023 molecules per mole; n1 is
                                             number of gaseous molecules per unit              Molecular flow is flow through a duct
                                                                                               under conditions where the mean free
                                             volume; and V is volume containing the            path is greater than the largest dimension
                                                                                               of a transverse section of the duct. In such
                                             gas. Replacing the volume V in Eq. 65 by          a flow, each atom moves independently
                                                                                               by random movement. Net flow is from a
                                             its value mRT/P from the ideal gas law of         volume of high concentration to one of
                                                                                               low concentration. The original
                                             Eq. 9 and substituting it in Eq. 64 results       mathematical derivations of molecular
                                                                                               flow are attributed to Knudsen (see
                                             in the equation for the mean free path            Eqs. 23 to 27). The rate of gas flow in a
                                             length λ of Eq. 66:                               long tube is given by Eq. 68:
                                             (66) λ =                MRT
                                                                    2 πPN σ2
                                             which shows that at constant pressure the         (68) Q =        d3( )2π RT
                                             mean free path is proportional to absolute                        6lM
                                             temperature. However, if the amount of                                P1 − P2
                                             gas in a volume is kept constant, the
                                             mean free path is independent of
                                             temperature, as indicated in Eq. 64. In
                                             Eq. 66, R is the specific gas constant and
                                             MR equals the molar gas constant.
FIGURE 15. Relation of leakage to pressure differential with                                   where d is diameter of the tube, l is length
laminar flow of helium gas in typical hardware leak.                                           of the tube and P2 and P1 are pressures at
                                                                                               the two ends. For the formula of Eq. 68 to
                                                             Pressure across leak (lbf·in.–2)  apply, the tube must be of a circular cross
                                                                                               section. For tubes and ducts of a
                                                       1  2         5 10 20    50 100          noncircular cross section, the conductance
                                             (10–1)                                            is less than for tubes of circular cross
                                       10–2                                                    section and equal area. Equation 68
                                                                                               applies only if the tube is much longer
                                                                                               than its diameter. Any difficulty
                                                                                               experienced by a molecule in entering the
                                                                                               tube must be negligibly small compared
                                                                                               to the difficulty in transversing its length.
Leakage rate, Pa·m3·s–1 (std cm3·s–1)  10–3 (10–2)                                             Equation for Free
                                                                                               Molecular Entry of Gases
                                       10–4 (10–3)                                             into a Small Aperture
                                                                                               If gas molecules experience difficulties in
                                                                                               entering a small leak opening, the kinetic
                                                                                               theory shows that the rate of free
                                                                                               molecular escape of gas from the
                                                                                               container into a small aperture of area A is
                                                                                               given by Eq. 69:
                                                                                               (69) Q =        ( )RT
                                                                                                               2πM
                                                                                                               A P2 − P1
                                       10–5 (10–4)
                                                          10 20     50 100 200 500 1000        In the case of an aperture, the leak
                                                                                               opening does not have to be circular for
                                                             Pressure across leak (kPa)        this equation to apply.
Legend
             = Theoretical values
             = Measured values
                                                                                                                            Tracer Gases in Leak Testing 61
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Flow Characteristics of                       1. the flow is not turbulent in any part of
Molecular Leaks                                   the pipe and
The conductance of lines and apertures in     2. the pressure difference between the
molecular flow is independent of pressure.        ends is not so great that the
Calculations may be made of the effect of         mechanism of the flow, i.e., laminar or
turns, apertures and change in tube               molecular, changes along the pipe.
diameter to calculate the overall flow in a
leak.                                            Although the first of these conditions
                                             is usually satisfied in the leak, the second
    Equations 23 to 27, 68 and 69            generally is not: that is, the transition
demonstrate the general form of relations    from laminar to molecular flow does take
for molecular flow through leaks. They are   place within a leak. Equation 70 at low
not applicable in most leakage situations    pressures becomes an equation of
because the leak length and diameter are     molecular flow, whereas at high pressure
not known. The molecular flow of each        this equation reduces to one of strictly
individual species in a gas mixture is       laminar flow.
inversely proportional to the square root
of the individual masses. Therefore, a           Knudsen used Eq. 70 to represent his
certain amount of separation of gaseous      experimental data. This equation has the
species takes place during flow through a    effect of molecular flow added to the
leak. In molecular flow, the gas molecules   effect of laminar flow; consequently, it is
travel independently of each other. Thus,    not an actual representation of the flow
it is possible for random molecules to       mechanism taking place in the leak. The
travel from a part of a system at low        phenomenon is better visualized by
pressure to another part of the system at a  realizing that both are occurring at the
higher pressure.                             same time.
                                             Burrows Equation for Transitional
                                             Flow
Knudsen Equation for                         Burrows combined Eq. 23 to 27 for
Transition Flow                              laminar flow with that of Eq. 68 for
                                             molecular flow to obtain the general
The transition from laminar flow to          relation for transitional flow given in
molecular flow is gradual. The               Eq. 71:
mathematical treatment of this region is
extremely difficult, but is necessary           π   d4    Pa
because a leak from a volume to a vacuum        8   2   nl
necessarily involves a transition from       =( )(71) Q
laminar to molecular flow. Equation 68                          P1 − P2
shows that the conductivity of a passage
in molecular flow is proportional to the           2π RT    d3
cube of the passage diameter and                     M      6l
independent of pressure. Conversely,         ( )+
Eq. 21 and 22 show that the conductivity                        P1 − P2
of the same passage in laminar flow is
proportional to the pressure.                In a way, Eq. 71 accurately represents the
                                             events occurring in the leak. Both laminar
    Knudsen derived a semiempirical          and molecular flow always occur in a leak.
formula for the conductance of gas           However, laminar flow is insignificant at
flowing through long tubes in the            low pressures. The molecular flow mode
transition flow region:                      contributes little to total flow at high
                                             pressures.
(70) C = Cviscous + ZCmolecular
                                                 Equation 71 is not completely accurate
=  π        d 4  Pa                        because of a slipping of molecules in
   8       2   nl                        transition flow. In laminar flow, the
                                             velocity of the molecular layers is
+  1        2 RT      d3                    proportional to their distance from the
                M      l                    wall, the first layer being stationary. In
     6                                      the transition region, slipping of the gas
                                             over the walls of the tube occurs; that is,
         1+        M   Pa  d                the flow velocity at the walls is not zero.
                   RT      n                At pressures below the viscous limit, the
×                                           slip correction becomes an appreciable
                                            contribution to the total conductance.
   1 + 1.24            M   Pa  d  
                       RT      n                 With further reduction in pressure, the
                                             dependence of flow conductance on
In this case, the gas flow rate Q =          pressure becomes more complex. The flow
                                             characteristics begin a progressive change
C(P1 – P2), where C is defined by Eq. 70.    from those of viscous slip flow to those of
Equation 70 is valid providing that:         molecular flow, where the conductance
                                             becomes independent of the pressure. The
                                             complete transition from viscous to
                                             molecular flow takes place over roughly
               62 Leak Testing
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two orders of magnitude change in                                                      γ
pressure. This effect of slip can change the
predicted flow rate by at least 20 percent.    (73) rc  =  P2       =      2  γ −1
Because of this effect, Eq. 70 better                      P1              γ + 1
represents flow in the transition region
but cannot handle the total transition         The term γ is the ratio of specific heats
region.                                        defined by Eq. 75 below. The velocity of
                                               sound through a gas can be written as in
    Other authors have attempted to derive     Eq. 74:
equations to represent this phenomenon
of transition from one type of flow to         (74) Fc  =    2γ            RT1
another. One simple way is to calculate                    γ +1            M
laminar flow through one section of the
tube, calculate molecular flow through         where Fc is velocity of sound and T1 is
another and approximate the region             absolute temperature upstream of the
between them.                                  orifice where the velocity is low. The ratio
                                               of specific heat at constant pressure to
Characteristics of                             that at constant volume is described by
Turbulent Flow of Gases                        gamma (γ), the ratio of specific heats
                                               defined in Eq. 75:
In viscous flow above a critical value of
the Reynolds’ number (about 2100 in the        (75) γ = C p
case of circular pipe flow), flow becomes                         Cv
unstable, resulting in innumerable eddies
or vortexes in the flow. Any particle in       where Cp is heat capacity at constant
turbulent flow follows a very erratic path,    pressure and Cv is heat capacity at
whereas in laminar flow the particle           constant volume.
follows a smooth line. Turbulent flow
occurs only in rather large leaks because it       The mass flow rate under a choked
requires relatively high velocity.
                                               flow condition is given by Eq. 76:
    The laws for turbulent flow are quite
different from the laws for laminar flow.                      πd 2 P1Co
The equation relating mass flow rate Q in
units of pressure × volume/time may be         (76) Q   =              4M
written as Eq. 72:
                                                              RT1  γ     2     γ +1
                                                                        + 1  γ −1
                                                                       γ
(72) Q = π d5  ( )RT P12 − P22                 where d is orifice diameter, P1 is upstream
                                               pressure and Co is orifice discharge
                    16f Ml                     coefficient.
The friction factor f depends on                   The value of γ for an ideal monatomic
roughness of the channel walls and can         gas is 1.67. For polyatomic molecules, the
be considered a constant in fully
developed turbulent flow.                      heat energy supplied is used for increasing
Theory of Choked (or                           not only the kinetic energy of translation
Sonic) Flow of Gases
through Leaks                                  but also the kinetic energy of rotation and
The phenomenon of choked flow (also            vibration. Because the same amount of
known as sonic flow) of gases is described
above. Two conditions required for             extra energy is required at both constant
choked flow to occur are:                      pressure and constant volume, γ decreases
                                               with molecular complexity. Characteristic
 1. The flow passage must be in the form       values of γ are listed in Table 12.
     of an orifice or venturi in which only
     negligible fractional losses occur        TABLE 12. Specific heats of gases at constant pressure Cp,
     upstream of the orifice or throat of the  at constant volume Cv, and as the ratio γ of Cp·Cv–1, in
     venturi.                                  joule per mole of gas at 25 °C (77 °F) and 100 kPa
                                               (1 atm) pressure.
 2. The ratio of downstream to upstream
     pressure must be below a certain               Gas Cp Cv Cp·Cv–1 = q
     critical value.
                                               Argon                20.8                  12.5  1.67
The critical ratio rc of downstream            Helium               20.8                  12.5  1.67
pressure P2 of upstream pressure P1            Hydrogen             28.8                  20.5  1.41
required for choked flow is given by           Oxygen               29.5                  21.1  1.40
Eq. 73:                                        Nitrogen             29.0                  20.7  1.40
                                               Carbon dioxide       37.5                  28.9  1.29
                                               Ammonia              36.1                  27.5  1.31
                                               Ethane               53.1                  44.5  1.19
                                               Propane              73.6                  65.2  1.13
                                                                                                                            Tracer Gases in Leak Testing 63
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Because of the stringent requirements,    (82) N Re > 2100
choked flow is rarely encountered as the
predominant flow mode except in very          for turbulent flow,
large leaks.
                                              (83) N Re < 1200
Criteria for Distinction
between Modes of Gas                          for viscous flow and
Flow in Leaks
                                              (84) 1200 < N Re < 2100
Equations have been presented for the
various possible modes of flow that can be    for either turbulent or viscous, depending
encountered in a leak. The following rules    on duct conditions.
may be used to predict the mode most
likely to occur. In distinguishing between        Choked flow takes place when the
laminar and molecular flow, the size of       pressure ratio between outlet and inlet
the passage and the mean free path are        reaches a certain minimum value. This, of
the two important parameters. The             course, depends on other characteristics,
distinction may be specified by a             such as aperture dimension. The formula
dimensionless parameter called the            for the critical pressure ratio for choked
Knudsen number. The Knudsen number is         flow depends on the ratio r defined in
defined as the ratio of the mean free path    Eq. 73. The critical ratio below which
of the molecule to a characteristic           choked flow takes place is given by
dimension of the channel through which        Eq. 73. Choked flow cannot take place
the gas is flowing. The Knudsen number is     when P1 is so low that molecular flow
defined by Eq. 77:                            exists.
(77) NK    =  λ                               General Formula for
              d                               Gaseous Permeation Flow
                                              Rate
where NK is Knudsen number, λ is mean
free path and d is channel diameter.          Permeation is passage of a fluid into,
                                              through and out of a solid barrier having
    The type of flow encountered in the       no holes large enough to permit more
various Knudsen number ranges is              than a small fraction of the molecules to
described by Eqs. 78 to 80:                   pass through any one hole. The process
                                              always involves diffusion through a solid
(78) λ < 0.01                                 and may involve other phenomena such
         d                                    as adsorption, solution, dissociation,
                                              migration and desorption. The general
for laminar flow,                             formula for permeation is given by Eq. 85:
(79) λ > 1.00                                           A ∆P      SD A ∆P
         d                                                  l               l
                                              ( )(85)q=Kp      =
for molecular flow and
(80) 0.01 > λ > 1.00                          where Kp = SD; q is rate of mass flow
                        d                     (Pa·m3·s–1·m2); S is solubility coefficient;
for transition flow.                          D is diffusion coefficient; Kp is permeation
    Flow in the viscous region is             rate constant (per second); A is area
                                              normal to flow (square meter); ∆P is
determined by the Reynolds’ number            pressure drop along the flow path
described earlier in Eq. 58 and 59 and
repeated in Eq. 81:                           (pascal); and l is length of flow path
                                              (meter). The ∆P in Eq. 85 does not
(81) N Re  =  d ρF      =  Q 4M               represent absolute pressures, but the
                n          d πnRT
                                              difference in partial pressure of the
                                              leaking fluid between the two sides of the
                                              barrier.
where d is channel diameter, ρ is fluid       Permeation of Helium through
density, F is flow velocity, n is gas         Rubber
viscosity, Q is leakage rate, M is molecular
mass, R is gas constant and T is absolute     Permeation presents a problem in leak
temperature.                                  testing equipment where the construction
                                              materials have a high permeability to the
    The distinction between laminar and       tracer gas. For example, if a component
turbulent flow is shown by the numerical      containing a rubber diaphragm 1 mm
criteria of Eqs. 82 to 84:                    (0.04 in.) thick and 650 mm2 (1.0 in.2) in
                                              surface area is leak tested using helium
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gas, a leakage of about 1 × 10–6 Pa·m3·s–1                                                                            material to be saturated with gas. This
      (1 × 10–5 std cm3·s–1) will be measured                                                                               is only possible if the material is
      across the diaphragm.                                                                                                 relatively thick. For example, a rubber
                                                                                                                            diaphragm will rapidly saturate and
          This leakage is due to permeation of                                                                              almost immediately show leakage. On
      helium through the diaphragm and not to                                                                               the other hand, O-rings are relatively
      any actual holes. It represents the                                                                                   thick and will not saturate rapidly
      maximum sensitivity of helium leak                                                                                    enough to give a reading within a
      testing that can be performed on this                                                                                 reasonable period of time (5 min). If
      component. However, if the component is                                                                               the diffusivity and solubility of the
      to be used with another fluid to which                                                                                fluid in the material are known, it is
      the membrane is impermeable, the                                                                                      possible to calculate the rate of
      apparent leakage due to permeation                                                                                    increase of leakage. However, in many
      measured during the leak testing has little                                                                           cases (where the leakage path is long),
      meaning under operating conditions.                                                                                   this calculation is not necessary.
                                                                                                                            Rather than calculations, experimental
          Another example of this type of false                                                                             results can determine very quickly if
      reading is a rubber O-ring. Depending on                                                                              leakage through a thick gasket is
      material, a rubber O-ring usually                                                                                     inconsequential for short time periods.
      represents a permeability of about                                                                                2. The maximum permeability of all
      5 × 10–7 Pa·m3·s–1 per centimeter of O-ring                                                                           components and the resulting mass
      surface exposed for every 100 kPa                                                                                     transfer produced by permeability
      (14.5 lbf ·in.–2) of differential pressure.                                                                           during leak testing may be calculated
      Figure 16 is an example of the permeation                                                                             (refer to Eq. 85, below). In this way,
      rates of O-ring of various materials. This                                                                            the permeability value will be known
      permeability does not have to be taken                                                                                and only leakage above this value will
      into consideration during routine leak                                                                                be considered as leakage flow.
      testing if leakage measurement occurs in a                                                                        3. The last and most difficult way is to
      time too short to permit the saturation                                                                               quantitatively measure the leakage at
      and mass transfer of helium through the                                                                               various pressure differentials. If gas
      O-ring.                                                                                                               leaks through a hole in the
                                                                                                                            component so that the leak being
      Procedures for Reducing Gas                                                                                           measured is pneumatic and laminar,
      Permeability Effects during Leak                                                                                      the flow is proportional to the square
      Testing                                                                                                               of the pressure differential across the
                                                                                                                            leak. However, if the flow is strictly
      To reduce permeability as a factor in                                                                                 due to permeation, then the flow
      leakage measurement, three procedures                                                                                 through the leak will be directly
      may be used:                                                                                                          proportional to the difference in tracer
                                                                                                                            gas concentration across the leak. In
       1. The leakage measurement may be                                                                                    this way, the presence of holes in the
           taken rapidly, not allowing the                                                                                  component can be differentiated from
                                                                                                                            permeation.
FIGURE 16. Permeation rate of helium at differential pressure
of 100 kPa (1 atm) through O-rings of 4 × 4 mm (0.16 ×                                                                 General Guide to Estimating Gas
0.16 in.) cross section, per 25 mm (1 in.) of length at 25 °C                                                          Flow Rates through Leaks
(77 °F) in units of pascal cubic meter per second (left vertical
scale) and torr liter per second (right vertical scale).                                                               Table 10 lists the theoretical ultimate
                                                                                                                       leakage sensitivities of various leak testing
      Silicone (composition: 20 percent)                                                                               techniques under ideal conditions with
                                                                                                                       very high concentrations of tracer gas. It
10–6                                          10–5                                                                     is derived from the various flow equations
10–7                                                                                                                   presented in the text. As may be seen
Permeation rate (Pa·m3·s–1)10–8                                                                                        from Tables 8 to 10, the influence of
                                                                                         permeation rate (torr·L·s–1)  varying the gas is not so great as that of
           Natural (composition: 10 percent)  10–6                                                                     varying the flow mode. Once the flow
      Hydrocarbon (composition: 10 percent)                                                                            mode is determined, the conversion to
                                                                                                                       another gas should be relatively easy to
      Synthetic rubber (composition: 10 percent)                                                                       make, providing the relationships in Table
                                                                10–7                                                   10 are in fact correct. The major difficulty
                                                                                                                       is identifying the predominant flow
10–9                                          10–8                                                                     mode.
      0 30 60 90 120 150 180 200                                                                                           The data necessary for the conversion
                                   Time (min)                                                                          of leakage rates between various gases are
                                                                                                                       relatively easy to obtain. For example, the
                                                                                                                       viscosity of many gases is published. Even
                                                                                                                       if the viscosity is not known,
                                                                                                                       approximation should not produce a large
                                                                                                                            Tracer Gases in Leak Testing 65
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error. As shown in Table 11, the viscosity        1. If pressure is increased, correlate as
of gases at constant temperature varies by            laminar.
less than half an order of magnitude
between the most viscous and the least            2. If pressure is decreased, correlate as
viscous.                                              molecular.
    For molecular flow, data on the               3. If gas is changed, correlate as
molecular mass of the gases is easily                 molecular.
available and should cause no problem in
the conversion (see Table 5). If choked              Correlation should be performed so
flow does occur, the gamma of Eq. 75,            that, if an error is made, actual leakage
necessary for conversion of choked flow          will be no greater than that predicted in
leakage, is 1.67 for monatomic gases and         the correlation. Correlation of leaks
rapidly approaches 1 as the complexity of        resulting from increased pressure across a
the gas molecule increases.                      leak is not recommended. An actual
                                                 measurement should be made whenever
Effect of Leak Size on Mode of                   possible to verify leakage rate.
Gas Leakage Flow
                                                 Equation for Gas Leakage
By working with a variety of leaks of            Flow Rate in Laminar Flow
different sizes and under different
conditions, some of the flow modes may           Assuming the flow mode has been
readily be eliminated. For example, if the       identified, the following are sample
leakage rate is small, it is relatively easy to  calculations for correlation of flow rates
assume that no turbulent flow will take          with the use of different gases and
place. If the leakage goes from high             pressure. The first sample calculation is
pressure to a slightly lower pressure, but       for laminar flow. The general equation for
not to a vacuum, it is likely that               laminar flow of gases is given by Eq. 86:
molecular flow is not the flow
mechanism. In this case, the flow may be             π    d4
of a laminar nature and therefore                   8nl   2 
conversion to a second flow pressure is          ( )(86) Q=
relatively easy. Choked flow is rarely                            Pa  P1 − P2
encountered in small leaks.
                                                 where Q is leakage (mass flow in units of
    Another example is that of converting        pressure × [volume/time]), d is average
the leakage rate for gas flowing into a          diameter of leak hole, P2 is pressure on
vacuum to an anticipated rate for a              the entrance side of the leak, P1 is
different pressure driving gas into the          pressure on the exit side of the leak,
same vacuum. If the leak is of relatively        average leak inlet and leak outlet pressures
small size, 10–6 Pa·m3·s–1 (10–5 std cm3·s–1)    Pa = (P1 + P2)/2, n is viscosity of the
or less, molecular flow will play a major        leaking fluid or fluid mixtures and l is
role in such a leak. However, should the         leak length. Note that Eq. 86 is equivalent
leak be relatively large, 10–4 Pa·m3·s–1         to Eq. 21 given earlier.
(10–3 std cm3·s–1) or greater, the leakage
will be predominately laminar. If one can            The leak dimension of d and l are
accurately predict the type of flow that         usually not known. An apparent
will predominate in a leak, one could            conductance C may be calculated by the
therefore make accurate conversions to a         formula, where this apparent conductance
different set of conditions. Unfortunately,      is the product of π(d/2)4/8 l and any unit
the state of the art is such that these          conversion factors. From this calculation,
predictions are usually not possible.            an apparent leak geometry factor can be
                                                 calculated from Eq. 87:
Estimating Mode of Gas
Leakage Flow from                                (87) C = π d4
Leakage Rate and Pressure                                           128 l
Many authors have predicted the following            If C is calculated only for conversion
predomination flow modes in leaks of             from one flow to another, the constant
various sizes: turbulent flow, 10–3 Pa·m3·s–1    does not have to be in compatible units,
(10–2 std cm3·s–1); laminar flow, 10–2 to        providing that the same units are used
10–7 Pa·m3·s–1 (10–1 to 10–6 std cm3·s–1);       both in solving for C and using the C in
transition flow, 10–5 to 10–7 Pa·m3·s–1 (10–4    correlation equations.
to 10–6 std cm3·s–1); molecular flow,
10–7 Pa·m3·s–1 (10–6 std cm3·s–1) . When             Using the apparent conductance C
there is doubt about the correctness of flow     calculated above, the flow of any gas at
identification, the following procedure is       operating pressure may be predicted by
recommended.                                     using Eq. 88:
                                                 ( )(88) QC
                                                 =  n    P12 − P22
                                                     A similar apparent conductance may be
                                                 calculated for other flow modes using the
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equations given earlier in this section.                leak cannot be seen below a critical
             Such calculations are correct only if the               pressure.
             flow mode has been correctly chosen.
                                                                     Effects of Geometry Change in
             Categories of Anomalous                                 Leaks
             Leaks
                                                                     The shape of a leak may change with
             Four types of leaks have been encountered               changes in system pressure. As pressure
             that do not fit in the categories already               increases, the expansion of system parts
             discussed: (1) check valve leaks, (2) surface           resulting from stresses induced by the
             flow leaks, (3) geometry change leaks and               increased pressure can cause leakage rates
             (4) self-cleaning leaks.                                of known leaks to increase beyond the
             The errors in leak measurement because of               predictions of laminar flow theory. Figure
             these types of leaks could be greater than              18 illustrates this increase of leakage rate
             any errors inherent in the preceding                    with geometry change.
             equations for flow conversions.
                                                                     Effects of Self-Cleaning Leaks
             Effects of Check Valve Leaks
                                                                     If gaskets under compression are subjected
             Examples of check valve and geometry                    to a high helium pressure and the leakage
             change leaks have been found during                     rate is determined quantitatively, the
             studies of leakage phenomena. Figure 17                 slope of the pressure leakage line is found
             is a plot of the leakage-pressure                       to be greater than two. No flow regime
             differential obtained on a damaged needle               would produce such a slope. However,
             valve. It was observed that although the                these curves consist of a series of lines
             typical laminar flow curve was obtained at              with a slope corresponding to that for
             a high pressure differential, below this                laminar flow.
             pressure, the leakage abruptly stopped. On
             increasing the pressure, the leak                           Because the increase in leakage could
             reappeared. This phenomenon was                         result from a permanent deformation of
             repeatable. This type of leak would be                  the gasket, an experiment was run using
             particularly hard to detect because the                 an aluminum gasket too sturdy to be
                                                                     deformed. Figure 19 shows the data
                                                                     obtained during this experiment. During
                                                                     the original increase in pressure, the
                                                                     leakage increased at a rate greater than the
FIGURE 17. Check valve leakage effect in hardware leak.
                 Pressure across leak (lbf·in.–2)                    FIGURE 18. Effects on leakage of geometry changes in
                                                                     gasket.
             12               5 10 20 50 100                                                                                                                    Pressure across leak (lbf·in.–2)
                                                                                                                                                                              103 104
10–4 (10–3)
                                                                                                                                                           102
                                                                                                                                           10–6 (10–5)
10–5 (10–4)Leakage rate, Pa·m3·s–1 (std cm3·s–1)                                                                                           10–7 (10–6)              Broken lines indicate
10–6 (10–5)                                                                                         Leakage rate, Pa·m3·s–1 (std cm3·s–1)  10–8 (10–7)              theoretical laminar flow slopes
                              Leakage drops to less than                                                                                   10–9 (10–8)
                              10–4 Pa·m3·s–1 (10–3 std cm3·s–1)
10–7 (10–6)                                                                                                                                                     12  5 10 20  50 100
                       10 20
                              50 100 200                  500 1 000
                              Pressure across leak (kPa)                                                                                                            Pressure across leak (MPa)
                                                                                                                            Tracer Gases in Leak Testing 67
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square of the pressure increase. However,         solid provides binding sites for the gas
                                       on releasing the pressure, the leakage            atoms and the electronic structure of the
                                       decrease was proportional to the square of        solid permits the formation of a
                                       the pressure decrease. A second increase          chemisorption bond. The nature of the
                                       in pressure produced an increase that             binding sites, the bonds between the gas
                                       retraced the leakage encountered during           atoms and the surface all influence the
                                       the pressure decrease. It is believed that        degree of surface migration of the atoms.
                                       the original pressure increase cleaned the
                                       leakage passages. Further pressure cycling            The flow along a fine capillary or
                                       did not affect the maximum leakage. This          micropore is assumed to consist of two
                                       suggests that whenever possible, leak             mechanisms working simultaneously:
                                       testing should be done at the proposed            (1) molecular flow along the bore of the
                                       operating pressure, in order that potential       capillary, whereby molecules are supposed
                                       leaks may be formed and observed.                 to collide with the wall, reevaporate and
                                                                                         collide with the wall again without
                                       Characteristics of                                intermolecular collisions; and (2) surface
                                       Absorbed or Surface Flow                          flow along the wall of the capillary,
                                       Leaks                                             whereby molecules are adsorbed and
                                                                                         diffuse along the surface of the wall. Both
                                       The flow of gases and noncondensing               these mechanisms promote gas flow from
                                       vapors through fine capillaries and               regions of higher gas concentrations to
                                       micropores cannot be dealt with by                regions of lower gas concentrations.
                                       means of simple techniques analogous to
                                       those applicable to molecular and laminar         Factors Influencing Surface Flow
                                       flow. The narrow passages and large               of Gases
                                       surface areas involved cause surface
                                       adsorption and surface flow to become             For a given set of conditions, the
                                       important factors.                                proportion of molecules that follow the
                                                                                         mechanisms of adsorbed or surface flow
                                           The adsorption may be physical, where         leakage depends on a variety of factors,
                                       only relatively weak van der Waals                including (1) the sticking probability (the
                                       attractions are involved. However, the            probability that a molecule sticking the
                                       adsorption may also be regarded as                surface will become adsorbed), (2) the
                                       chemical. In this case, the surface of the        length of time the molecule remains
                                                                                         adsorbed (the mean surface lifetime of the
FIGURE 19. Leakage curves showing self-cleaning effects in                               gas molecules) and (3) the coefficient of
leaks.                                                                                   surface diffusion of the gas molecules.
                                                                                         These features are, in turn, influenced by
                                                    Pressure across leak (lbf·in.–2)     other characteristics, such as the number
                                                                                         of sites occupied by the adsorbed
                                                         10 20      50 100 200 500 1000  molecules or whether a complete
                                       10–5 (10–4)                                       monolayer is involved.
Leakage rate, Pa·m3·s–1 (std cm3·s–1)  10–6 (10–5)                                           The nearer the properties of a gas
                                                                                         approach those of a condensable vapor,
                                       10–7 (10–6)                                       the greater the proportion of surface flow.
                                                                                         Therefore, a reduction of temperature or
                                       10–8 (10–7)                                       an increase of pressure may sometimes
                                                                                         promote a total flow in excess of that
                                                    0.1 0.2 0.5 1.0 2.0 5.0 10           predicted by the laminar molecule theory.
                                                    Pressure across leak (MPa)               Although the final leakage rate
                                                                                         achieved with a condensable gas may be
Legend                                                                                   higher than predicted from flow theory,
                                                                                         there may be an initial delay of flow
                                       = Pressure decrease                               because of condensation of the tracer gas
                                       = Second pressure increase                        on the leak surfaces. This delay is
                                       = Initial pressure increase                       important if a tracer probe technique is
                                                                                         used for testing. For example, if butane, a
                                                                                         readily condensable gas, is used in the
                                                                                         tracer probe, some small leaks will be
                                                                                         missed because of the delay caused by the
                                                                                         adsorption. Two remedies can be
                                                                                         suggested to counter this problem: use of
                                                                                         a noncondensable gas and use of a
                                                                                         detector probe with condensable gases.
                                                                                         With use of a detector probe, the gas is
                                                                                         continually in contact with the leak and
                                                                                         equilibrium is established.
68 Leak Testing
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References
                         1. Nondestructive Testing Handbook,
                            second edition: Vol. 1, Leak Testing.
                            Columbus, OH: American Society for
                            Nondestructive Testing (1982).
                         2. Slattery, J.C. and R.B. Bird.
                            “Calculation of the Diffusion
                            Coefficient of Dilute Gases and of the
                            Self-Diffusion Coefficient of Dense
                            Gases.” AIChE Journal. Vol. 4, No. 2.
                            New York, NY: American Institute of
                            Chemical Engineers (1958): p 137-142.
                                                                                                                            Tracer Gases in Leak Testing 69
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3
                                                                   CHAPTER
                         Calibrated Reference
                                               Leaks1
                                                                                 Mark D. Boeckmann, Vacuum Technology,
                                                                                 Incorporated, Oak Ridge, Tennessee
                                                                                 Charles N. Sherlock, Willis, Texas
                                                                                 Stuart A. Tison, National Institute of Standards and
                                                                                 Technology, Gaithersburg, Maryland
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PART 1. Calibrated Reference Leaks
Terminology Applicable to                     specification requires some arbitrary
Reference, Calibrated or                      standard. However, if any doubt exists,
Standard Leaks                                one need only reduce the leakage of this
                                              arbitrary standard physical reference leak
Physical leaks suitable for checking leak     by a sufficient safety factor to ensure that
detector performance and leak test            test sensitivity meets the practical leakage
sensitivity are a vital component of          requirement within some estimated
instrumentation for leak testing. The         confidence interval.
terms reference, calibrated and standard
leaks have been used in the past to           Classification of Common
identify these physical leaks. To many        Types of Calibrated or
people, the term calibration implies the      Standard Physical Leaks
existence of a universally accepted
standard such as those at the National        Calibrated physical leaks are designed to
Institute of Standards and Technology.        deliver gas at a known rate. The most
                                              common use of such leaks is in the
    The National Institute of Standards and   measurement of sensitivity of leak
Technology has performed calibration of       detectors. However, calibrated leaks are
helium leaks (capillary and permeation)       also used to measure the speed of vacuum
over the range of 10–14 to 10–6 mol·s–1       pumps and to calibrate pressure gages. A
(2.3 × 10–11 to 2.3 × 10–3 Pa·m3·s–1) on a    standard physical leak makes feasible the
routine basis. The uncertainties in leak      establishment of leakage rate
rate vary from less than 1 percent at         requirements for specifications. It also
10–6 mol·s–1 (2.3 × 10–3 Pa·m3·s–1) to as     provides a uniform reference standard for
much as 5 percent at 10–14 mol·s–1            calibrating leak detectors at different
(2.3 × 10–11 Pa·m3·s–1). Additionally, the    locations where products are inspected.
National Institute of Standards and           This ensures more uniform agreement of
Technology will calibrate leaks with other    all tests.
gases over this range on a special test
basis. All of these calibrations are              Calibrated leaks may be divided into
performed while the gas is exhausted into     two distinct categories: (1) reservoir leaks
a vacuum. Leaks may also be calibrated by     that contain their own tracer gas supply
commercial companies that derive their        and (2) nonreservoir leaks to which tracer
measurement uncertainty from either of        gas is added during testing. Figure 1
two techniques. The first is that they        shows a classification of physical leaks
derive their measurements from leaks          used for reference, calibration or standard
calibrated at the National Institute of       leaks.
Standards and Technology and perform
calibrations using a comparison               Accuracies of Reservoir Calibrated
technique. The second technique uses          Leaks
secondary techniques that derive the leak
rate through measurements of pressure,        The uncertainty in the leak rate of fixed
volume, temperature and time with             reservoir leaks is due to a combination of
instruments whose calibration can be          calibration uncertainty, leak rate decay
traced to the National Institute of           because of calibration, temperature effects
Standards and Technology. The                 and leak instability. Of these, uncertainty
appropriate type of calibration will          in the stability of the leak is hardest to
depend on particular measurement              quantify. Changes in the leak rate may
requirements including the required           occur in capillary leaks because of partial
accuracy, traceability or regulatory issues.  blockage of the capillary. Changes in the
                                              leak rate of glass permeation leaks may
    In some cases, accuracy in leakage        occur because of the development of
measurement is not of prime importance.       microcracks in the glass. In general, these
Rather, most practical situations require     leaks are more stable than leaks without
that some particular leakage value not be     closed reservoirs, particularly for
exceeded. It need only be established that    calibrated leaks with values less than
no leakage in the tested system is greater    10–9 mol·s–1 (2.3 × 10–6 Pa·m3·s–1).
than this allowable maximum leakage
rate. This practical approach to leakage
72 Leak Testing
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Accuracies of Nonreservoir                     correction for pressure, temperature and
Calibrated Leaks                               other environmental factors. In the tracer
                                               probe mode of leak detection, tracer gas is
The nonreservoir type of leak provides         sprayed on the calibrated leak under the
only a hole or a series of holes and           same conditions that exist when the leak
passages that permit gas to pass through       detector is used to measure a leak in any
at a known rate. The users of this type        system or enclosure under test.
calibrated leak must provide gas at a
known concentration, purity and                    In the case of a leak containing a
pressure.                                      reservoir, the measured sensitivity of the
                                               leak detector is independent of the test
    The uncertainty in the leak rate of        gas pressure and of the tracer gas
nonreservoir leaks is due to a                 contamination of ambient air surrounding
combination of calibration uncertainty,        the leak testing area. If the calibrated leak
temperature effects, leak instability,         is to be used for the measurement of an
pressurizing gas purity and uncertain          absolute value, as in the case of the
measurements of gas pressures and              calibration of a pressure gage or
temperatures. Most if not all nonreservoir     measurement of the speed of a pump, a
leaks are physical leaks and are susceptible   leak carrying its own gas supply is
to plugging. Because of this it is very        desirable.
important that the input gas be free of
particulates and hydrocarbons. In              Basic Categories of
addition the output should be exposed to       Calibrated Gas Leaks
as little contamination as possible,
especially when the leak is not                Generally, leaks may be grouped into
pressurized. Nonreservoir type leaks are       either of two categories: (1) leaks that
typically used for higher leak rates, greater  depend on the permeation of some
than 10–9 mol·s–1 (2.3 × 10–6 Pa·m3·s–1),      materials by certain gases and (2) leaks in
where the depletion rate of reservoir leaks    orifices that permit the flow of any gas
becomes greater than 20 percent per year.      when a pressure differential is exerted
The temperature coefficients of leaks can      across the element.
be measured to account for changes in the
leak rate as a function of temperature.            Variation of the material composition,
                                               the membrane dimensions and the partial
Comparison of Standard Leaks                   pressure differential of gas across the
with and without Tracer Gas                    element permit the attainment of an
Reservoirs                                     almost infinite range of flow rates. The
                                               temperature coefficients of the
In proper leak testing practice, the           permeation leak systems are appreciable.
sensitivity of leak detectors is checked       This provides an additional means of
frequently by calibrated leaks of reservoir    extending the flow range, particularly
types with internal gas supply. For system     when the other parameters are fixed or
sensitivity checks, a calibrated leak          limited.
without a reservoir is preferable because it
closely imitates the behavior of an actual         Leaks that permeate through a
leak in the object or system under test.       fluorocarbon resin membrane are also
The calibrated leak without a reservoir is     available with properties similar to those
open to local atmospheric pressure;            of gas leaks. The second category of orifice
therefore, it requires no sensitivity          leaks permits the attainment of a wide
                                               range of flow rates by modification of the
FIGURE 1. Categories of artificial physical leaks commonly spoken of as “reference,”
“calibration” or “standard” leaks.
                                                                                         Leaks
                        Reservoir                             Nonreservoir
Permeation              Capillary              Porous  Capillary                                Porous
                                                plug                                             plug
Glass  Fluorocarbon
              resin  Fixed         Variable            Fixed  Variable
                                    value              value   value
                     value
       Fixed  Variable
       value   value
                                                                                                                              Calibrated Reference Leaks 73
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element dimensions and the pressure          reservoir standard leaks with low leakage
differential across the element.             rates of the order of 2 × 10–7 Pa·m3·s–1
Temperature is not as great a factor         (2 × 10–6 std cm3·s–1) or less.
because the temperature coefficients are
small with glass orifice standard leaks.         During manufacture of calibrated leaks,
                                             additional effort and weight can extend
Properties Designed in Calibrated            the upper limit of flow by as much as a
Gas Leaks                                    factor of 50 without allowing the
                                             depletion of the gas supply to cause a
The range of possible flow rates of          falloff in leakage rate greater than
calibrated leaks is rather severely limited  10 percent per year. Greater increases of
by practical considerations in the           the upper limit call for nearly linear
selection of parameters for the              increases in volume of the leak gas
construction of leaks for quantitative       reservoir and even greater increases in
standards. An ideal calibrated leak should   weight. These reduce the portability and
have the following properties.               ease of installation of standard leaks.
 1. The leakage rate should be constant      Limitations of Flow Rate
     and should remain unaffected by         Calibration of Standard Gas Leaks
     ambient conditions.
                                             The lower limit of flow rate that is
 2. The calibration should be accurate.      practical for direction calibration is about
 3. The physical size should be              10–11 Pa·m3·s–1 (10–10 std cm3·s–1). The
                                             degassing of the system becomes a
     convenient.                             problem as the size of the leak is decreased.
 4. The calibrated leak should not be too    In this range the changes of both true
                                             leakage and virtual leakage caused by
     delicate or fragile.                    pressure increase are nearly equal.
 5. The calibrated leak should have its
                                                 Two indirect techniques may be used,
     own gas supply.                         either separately or in combination, to
                                             calibrate with reasonable accuracy in the
Temperature Coefficients of                  low ranges; both techniques have been
Calibrated Leaks                             experimentally justified. The calibration
                                             may be made by comparison with a
Unfortunately, those parameters useful in    standard of greater flow rate by means of
extending the possible range of flows are    a mass spectrometer. The actual rate is
not conducive to constancy. The high         extrapolated (assuming linear response of
temperature coefficients of the membrane     the instrument). Alternatively, the leakage
leaks are particularly disturbing when the   rate may be increased in a manner in
changes in ambient temperatures are          which the response is predictable (i.e., the
frequent and there is no way of              pressure response of membrane leaks is
determining whether or not the               linear) and calibration made at the higher
equilibrium flow rate is reached at any      flow rate.
one temperature. Even the relatively small
temperature coefficients of orifice leaks    Limitations of Glass Membrane
are appreciable when the temperature         Standard Gas Leaks
varies over wide ranges.
                                             Construction of all-glass membrane leaks
    The National Institute of Standards and  that vary in flow range at ambient
Technology measures the temperature          temperatures from 0 to 50 °C (32 to
coefficients of leaks as a normal part of    122 °F) is rather simple. Larger flows
their calibration service over the range of  require either higher pressures or
0 to 50 °C (32 to 122 °F). Some              modification of membrane parameters
manufacturers of calibrated leaks may also   that tend to make them excessively
be able to measure temperature               fragile.
coefficients. Normally manufacturers
assume a linear temperature coefficient of       It is possible to combine a number of
3 to 4 percent per 1 °C (2 °F) for glass     the large leak elements in parallel to
helium permeation leaks. For the lowest      obtain greater flow when necessary.
uncertainties the temperature coefficients   Advantage has been taken of the relatively
should be measured.                          sturdy nature of glass tubing of very small
                                             cross section and correspondingly thin
Size, Weight and Portability of              walls. Elements have been made using
Calibrated Gas Leaks                         literally miles of such tubing in systems
                                             designed for use at relatively high
The convenience of the physical size is a    temperatures to separate low
property that would vary considerably,       concentrations of helium from natural
depending on the use to which the            gases. However, these elements do not
calibrated leaks is applied. In general,     seem suitable for use under high vacuum
complete and convenient portability of       conditions.
standard leaks is desirable and is usually
available in nonreservoir standard leaks.
Portability is easily attainable with
74 Leak Testing
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Limitations of All-Glass Orifice               Basic Characteristics of
Standard Leaks                                 Orifice Standard Leaks
All-glass orifice leaks are more difficult to  The orifice standard leaks share several
produce with flow rates smaller than           characteristics.
5 × 10–9 Pa·m3·s–1 (5 × 10–8 std cm3·s–1)
unless precautions are taken to maintain        1. They may be used with almost any gas
the pressure differential significantly             under conditions sufficiently removed
positive in the downstream direction                from liquidus conditions.
while the upstream pressure is made
subatmospheric.                                 2. They have relatively low temperature
                                                    coefficients.
    The upper limit in flow rate is
determined mainly by the maximum                3. They are relatively sturdy, being able
acceptable physical size. Glass reservoirs          to stand high pressure differentials, in
become bulky when they are of adequate              excess of 10 MPa (100 atm).
size to supply a leak of the order of
1 × 10–6 Pa·m3·s–1 (1 × 10–5 std cm3·s–1)       4. They have pressure responses that vary
without having the leakage rate fall off            from linear response for very small
more than 10 percent per year.                      leaks, about 1 × 10–9 Pa·m3·s–1
                                                    (1 × 10–8 std cm3·s–1), to direct
Improving Calibrated                                proportion to the square of the
Leakage Rate Stability by                           pressure for very large leaks, about
Increasing Envelope                                 5 × 10–4 Pa·m3·s–1
Pressure                                            (5 × 10–3 std cm3·s–1).
Stability of leakage rate may be improved       5. They are subject to plugging by solids
greatly without sacrificing compactness by          or by condensation of vapors of
enclosing the leak element in a metal               materials close to liquidus conditions.
envelope and filling the envelope to a
significantly greater pressure. Membranes      Precautions with
that leak 5 × 10–8 Pa·m3·s–1                   Calibrated Gas Leaks
(5 × 10–7 std cm3·s–1) at a pressure
differential of 100 kPa (1 atm) will raise     For maximum accuracy in the use of
their leakage 20× to a rate of                 calibrated leaks, the following precautions
1 × 10–6 Pa·m3·s–1 (1 × 10–5 std cm3·s–1)      should be taken.
when used with a partial pressure
differential of 2 MPa (20 atm).                 1. Leakage rates should be defined as
                                                    mass units per unit time. When
    The leakage rate will fall off one              volume units are used, they must be
twentieth as much as that of a membrane             defined by specification of the
that will leak 1 × 10–6 Pa·m3·s–1                   temperature and pressure conditions
(1 × 10–5 std cm3·s–1) at atmospheric               under which they are to be measured.
differential, with the same volume
reservoir. Maximum envelope membrane            2. The temperature at which the
leak pressures are limited by their nature          calibration is made and the
to not more than 2.8 MPa (400 lbf·in.–2             temperature at which the calibrated
gage). Orifice leaks have been used with            leak is used should be specified. If they
maximum pressures in the envelope of                are not identical, the temperature
12 MPa (1700 lbf·in.–2).1                           coefficient should be used to correct
                                                    the leakage rate. For best results the
Basic Characteristics of                            leak should be calibrated and used
Membrane Standard Leaks                             under constant temperature
                                                    conditions.
Membrane standard leaks share several
characteristics.                                3. A considerably higher than ambient
                                                    temperature surrounding the element
 1. They are restricted to usable gases,            of the orifice leaks will tend to
     even at elevated temperatures.                 decrease the possibility of plugging by
                                                    condensation of liquid.
 2. They have relatively high temperature
     coefficients.                              4. If a leak is not equipped with an
                                                    integral gas supply, care should be
 3. They are relatively fragile when                taken to use dry gas with orifices and
     constructed with glass.                        to maintain a positive pressure
                                                    differential across the element in the
 4. They normally have a response linear            downstream direction if possible.
     with respect to reservoir                      Membrane leaks should be given
     concentration.                                 adequate time to reach an equilibrium
                                                    rate if the partial pressure differential
 5. They are almost impossible to plug.             of the tracer gas is changed.
                                                                                                                              Calibrated Reference Leaks 75
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Design and Construction                       leakage temperature coefficient is large
                      of Permeation Physical                        (three percent or more per degree kelvin).
                      Leaks
                                                                    Permeation Leak for Helium
                      Permeation leaks use the principle of gas     Tracer Gas
                      diffusion through a thin wall. Tracer gas
                      permeates from the high leak reservoir        A common helium permeation leak is
                      concentration through the wall to air or      shown in Fig. 2. The helium permeation
                      vacuum. Leakage is governed by the            leak consists of a small helium filled metal
                      permeability of the thin membrane. The        or glass cylinder with an integral glass
                      major advantage of permeation leaks is        membrane at one end. Helium diffuses
                      that they deliver extremely small             through this glass at a measurable rate.
                      quantities of gas. The commercially           Each leak should be calibrated and labeled
                      available helium leak standard range          with the following information: (1) name
                      extends from 10–7 to 10–11 Pa·m3·s–1 (10–6    of manufacturer, (2) model number,
                      to 10–10 std cm3·s–1). Because a long period  (3) type of leak (glass permeation, orifice
                      of time is necessary to achieve permeation    etc.), (4) serial number, (5) composition of
                      equilibrium, these leaks usually come         fill gas, (6) leak rate, (7) calibration
                      with a self-contained gas supply. However,    temperature, (8) estimated uncertainty of
                      at small leakage rates, the leakage remains   leak rate, (9) date of calibration,
                      constant over a long period of time. The      (10) temperature coefficient and
                      two disadvantages of calibrated               (11) reservoir pressure, date of fill and
                      permeation leaks are (1) that they can        estimated depletion rate.2
                      only be made for gases that permeate
                      through membranes and (2) that their              The leak may contain two valves: a
                                                                    vacuum valve downstream of the leak
                                                                    element and a pressure (or reservoir
                                                                    valve). The reservoir valve is used for
FIGURE 2. Helium permeation leak with self-contained reservoir: (a) photograph of standard helium leak and
cut away model; (b) schematic cross section.
(a)
(b)                   Standard     Helium         Permeable               38 mm
                       vacuum     reservoir     glass/quartz             (1.5 in.)
           63 mm      coupling                   membrane           outside diameter
           (2.5 in.)                                                                  Filling
         maximum                                                                        port
                       32 mm
                      (1.26 in.)
                                  Leak shutoff
                                  valve
                                                280 mm
                                                (11.0 in.)
76 Leak Testing
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refilling of the leak reservoir. The vacuum    changed to change the leakage rate at
valve is used for briefly shutting off the     which tracer gas flows out of the physical
helium flow for purposes of zeroing a          reference leak.
helium leak detector during the process of
calibration. The vacuum valve should not       Variable Value Orifice Physical
be shut off for extended periods of time       Reference Halogen Leaks
(greater than 10 min) or the stability of
the leak may be affected severely.             The variable value physical halogen vapor
                                               leak shown in Fig. 4 is available for
Porous Plug Calibrated Leaks                   different ranges, such as 10–5, 10–6, 10–7
Providing Molecular Flow of Gas                and 10–8 Pa·m3·s–1 (10–4, 10–5, 10–6 and
                                               10–7 std cm3·s–1). A schematic flow
Porous plug calibrated leaks are not
commercially available but have                FIGURE 3. Reservoir variable rate physical orifice leak standard
frequently been cited in literature. They      (top) and fluorocarbon resin permeation leak standard
consist of a metal, ceramic or glass plug      (bottom) for calibration of detector probe instruments.
containing extremely fine pores. The
major advantage of this type of calibrated
leak is that molecular gas flow occurs
through the plug. Therefore, the change
of leakage flow resulting from a change of
tracer gas can be calculated from the
kinetic theory of gas flow. Porous plug
leaks can be either reservoir or
nonreservoir type, with the choice of
materials cited above.
Design and Characteristics                     FIGURE 4. Variable leak rate halogen refrigerant leak standard
of Capillary Calibrated or                     with physical (capillary) leak element: (a) photograph of leak
Standard Physical Leaks                        standard with internal reservoir of refrigerant gas and
                                               another of refrigerant liquid and (b) schematic flow
Another type of commercial calibrated          diagram.
leak is a single orifice in heat resistant
glass or metal, encased in a stainless steel   (a)
fixture. Tracer gas leaks through the
orifice at the rated leakage, when the leak    (b)                                Gage
is placed under a specified gage pressure
(relative to atmospheric pressure). Such                       (Pressure         Vapor     Calibrated
capillary leaks are available in two types,                    increase)        reservoir      leak Detector
fixed value leaks and variable value leaks,                                                              probe
as next described.                                   Liquid
                                                    reservoir   Vapor
Fixed Leakage Value Orifice                                    reservoir
Capillary Leaks                                                fill valve                  Vent (pressure decrease)
Capillary type calibrated leaks are made            Fill valve for
from constructed glass tubing or collapsed          liquid halogen/refrigerant
thin metal tubing. These orifice leaks can
be produced from large sizes down to
about 10–8 Pa·m3·s–1 (10–7 std cm3·s–1).
Although smaller leaks of this nature can
be made, they become extremely difficult
to handle because of leak clogging.
Capillary leaks can be calibrated to deliver
one or a variety of tracer gases. Some leaks
are to be used with an independent tracer
gas supply, i.e., they simply consist of a
capillary leak attached to the system
under test. In the tracer probe method of
leak testing, tracer gas is simply sprayed
over the capillary. Alternatively, a physical
reference capillary leak can be made with
a self-contained gas supply that can be
permanently attached to the leak. Figure 3
shows a physical capillary orifice leak
with its own tracer gas reservoir and a
leak factor gage. The gage pressure may be
                                                                                                                              Calibrated Reference Leaks 77
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diagram of its system is shown in Fig. 4b.                   room temperature would be much too
This leak contains a reservoir of liquid                     slow). The leak is designed to yield a
Refrigerant-134a halogenated                                 point source of helium to simulate a pin
hydrocarbon tracer to be valved into a                       hole leak. The point source of leakage
ballast tank in gaseous form. Also                           may be used to calibrate the detector
connected to the ballast tank is a glass                     probe of a helium mass spectrometer leak
capillary tube and pressure gage. The rate                   detector. The helium detector probe
of gas leakage through the calibrated leak                   calibrator may also be used as a training
depends on the pressure in the ballast                       tool to train operators on the distance and
tank. Laminar gas flow occurs through the                    speed a probe must be from a certain size
leak. This permits the pressure gage to be                   leak to detect the leak. The major
marked in leakage units, where leakage is                    disadvantage of the helium detector probe
proportional to the ratio of the difference                  calibrator is that it requires an external
between the squares of the absolute                          tank of helium for refilling, unlike
pressures. The halogen leak standard is                      refrigerant calibrators that can store extra
commonly used with heated anode                              refrigerant in an on-board liquid tank
halogen leak detectors. It is an excellent                   (Fig. 4).
leak standard to use with probe
instruments because the probe may be                             Other types of variable value reference
passed directly across the leak exit. The                    leaks are controlled by elegant needle
calibration then approximates detector                       valve or crushed tubing whose
probe operating conditions.                                  conductance is changed by flexing.
                                                             Although the conductance of these leaks
Variable Leak Rate Helium                                    can be made quite repeatable, they should
Reference Leaks                                              not be considered calibrated leaks because
                                                             of a complete lack of standardization of
Variable reference leaks have been                           leakage rates in these artificial orifice
designed to leak helium for use with                         types of physical leaks.
helium mass spectrometer leak detectors
equipped with a detector probe. The leak                     Sources of Inaccuracy of
arrangement is shown in Figs. 3 and 5.                       Leakage Measurements
The leak standard in Fig. 5 uses either a                    with Standard Leaks
capillary or fluorocarbon resin permeation
membrane as the gas flow restriction (the                    The inaccuracy of leak detector
time response for a glass membrane at                        measurements made with physical
                                                             standard leaks can be caused by factors
FIGURE 5. Variable rate helium leak standard                 such as: (1) inaccuracy in calibrating the
(capillary style sniffer).                                   leak, (2) nonlinearity of the leak detection
                                                             instrument, (3) variation in pressure
                                  Fill and flush             differential applied across the leak,
                                  valve                      (4) impurity of gas applied to the leak and
                                                             (5) variation in the amount of gas
                                           6 mm (0.25 in.)   reaching the detector.
                                           male pipe thread
                                                             Accuracies of Calibrations of
                           Gas reservoir                     Commercially Available Physical
                                                             Reference Leaks
                           Capillary pinpont
                           helium source                     Beginning in 1987, the National Institute
                                                             of Standards and Technology established a
                     6 mm                                    leak calibration program that calibrated
                     (0.25 in.)                              leaks over the range of 10–11 to
                                                             10–3 Pa·m3·s–1 (10–10 to 10–2 std cm3·s–1).
                                                                 In a 1980 study, tests of standard leaks
                                                             from various manufacturers have shown
                                                             that their accuracies could differ by more
                                                             than ±50 percent of a mean value.1 This is
                                                             shown by the experimental plot of Fig. 6,
                                                             which shows the calibrated leakage
                                                             reading compared to the response of a
                                                             linear mass spectrometer. The straight line
                                                             drawn in the graph is the least mean
                                                             square value of leakage as a function of
                                                             spectrometer response. This line does not
                                                             imply the correct value, but the general
                                                             pattern around which the values of the
                                                             leaks congregate.
78 Leak Testing
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Even the leaks made by any single            A typical leak detector response error
                     manufacturer vary by about 10 percent.       curve is shown in Fig. 7. The instrument
                     This is usually the guarantee that is        response is not linear with leakage. This
                     presented on purchase of the permeation      error is added to the error that occurs
                     calibrated leak. Leaks of a variable type,   because of the difference in leak
                     such as that shown in Fig. 4, are claimed    calibration. Because of this lack of
                     to be accurate only to ±20 percent.          linearity, the farther apart the two leaks
                                                                  are in nominal value, the greater the error
                         Beginning in 1987, many                  in the calibration. Because such deviations
                     manufacturers of leaks began deriving        exist it is recommended that, when the
                     their measurements directly from leaks       leakage measurement is done to a
                     calibrated by the National Institute of      specified high tolerance, a calibrated leak
                     Standards and Technology. The existence      to the exact specified value be used as a
                     of national standards in leak                standard.
                     measurement should improve the relative
                     agreement between the manufacturers of       Effect of Barometric
                     leaks and may also reduce the                Pressure on Leakage
                     uncertainties that manufacturers provide     Measurements
                     for calibrated leaks.
                                                                  Leakage depends on the pressure
                 Errors in Response of Commercial                 differential acting across the leak. When
                 Electronic Leak Detectors                        leak detection is done by a tracer probe,
                                                                  the pressure differential is usually 100 kPa
                     Most commercial leak detectors display       (1 atm). The gas is sprayed over the
                     the response to a detected leak as a         suspected area without aid of additional
                     current reading on a sensitive               pressure. Should leak detection be
                     microammeter. It is usually assumed by       performed at high altitudes, the
                     the operator that current reading twice      atmospheric pressure is less than 100 kPa
                     the magnitude of a previously observable     (1 std atm). The magnitude of this
                     one represents a leak of twice the size.     reduction is as much as 20 percent in
                     This assumption of linearity in response is  places such as Boulder, Colorado. If the
                     not necessarily correct; nonlinearity may    leaks that are being located are of a
                     result from the structure of the pumping     laminar nature, the laminar flow through
                     system, the background usually associated
                     with the leak testing practice, the          FIGURE 7. Typical range of error possible in actual leakage
                     electronic circuitry associated with the     measurements with a leak detector. Variations with
                     detection system and the mode of gas         magnitude of leakage increase the difficulties of correlating
                     flow through the leak.                       measured leakage rates with standard reference leaks.
FIGURE 6. Comparison of leakage values for leaks supplied by
various vendors, measured by linear mass spectrometer.
Resulting ion current depends on mass spectrometer
configuration.
        10–2 (10–1)
Stated leakage, Pa·m3·s–1 (std cm3·s–1)10–3 (10–2)                                                                                                                                Possible variation
                                                                                                    Actual leakage (relative units)10–4 (10–3)                                    in measurement
10–5 (10–4)
10–6 (10–5)
10–7 (10–6)
10–8 (10–7)
10–9 (10–8)                                                                                                                          Measured                         Calibrated
                                                                                                                                            leak                      leak
                                                                                                                                                  Measured leakage
10–10 (10–9)                                                                                                                                        (relative units)
                  10–14 10–13 10–12 10–11 10–10 10–9
                                                      10–8  10–7  Legend
             Ion current (A)                                                                                                         = range of deviation due to nonlinearity of instrument response
                                                                                                                                     = error due to comparison and instrument linearity
                                                                                                                              Calibrated Reference Leaks 79
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the leak is proportional to the square of         Effect of Position of Calibrated
the pressure differential. The values             Leak on Test System
obtained for leakage readings at the
altitude of Boulder, Colorado, are                Tracer gas may be absorbed on test system
40 percent less than those obtained with a        surfaces as it travels to the detector. This
100 kPa (1 std atm) pressure during use.          would decrease the response of the leak
Therefore, a leakage rate measured to             detector. Therefore, calibrated leaks
atmosphere in Boulder, Colorado will be           should be positioned on the system as
only 60 percent as large as with the same         near as possible to suspected leak sites to
leak measured at Cape Kennedy on the              improve accuracy. Alternatively, they may
seashore of Florida.                              be positioned as far away from the
                                                  detector as possible to show minimum
    Certain calibrated leaks contain their        sensitivity. Both of these positions are
own gas supply, whereas others have the           conservative choices that ensure that
tracer gas sprayed onto the entry orifice of      leakage from test object discontinuities
the leak at 100 kPa (1 atm) pressure              will not be underrated.
during use. Calibrated leaks with a self
contained gas supply always deliver to the        Specifying Maximum Allowable
detector a fixed amount of gas that can be        Leakage Rate
used to measure the sensitivity of the leak
detector. On the other hand, leaks where          Because of the variations discussed here,
gas is added during use produce the               the accuracy of any leakage measurement
calibrated amount of leakage only when a          probably varies from half to twice the
100 kPa (1 atm) pressure differential is          actual value. This implies that, if a leak is
supplied. These nonreservoir physical             measured as 1 × 10–6 Pa·m3·s–1
reference leaks therefore deliver less than       (1 × 10–5 std cm3·s–1), the actual value of
the calibrated amount of leakage when             this leak is between 2 × 10–6 and
used at high altitudes where the                  0.5 × 10–6 Pa·m3·s–1 (2 × 10–5 and
atmospheric pressure is lower. However, at        0.5 × 10–5 std cm3·s–1). Therefore, if the
these altitudes, the pressure of the tracer       maximum allowable leakage rate of a
gas across the leak is lower. In such cases,      particular system is 2 × 10–6 Pa·m3·s–1
a physical reference leak without its own         (2 × 10–5 std cm3·s–1), the specification
gas supply describes more accurately the          may be written with a leakage tolerance of
sensitivity of the leakage test. It is this test  1 × 10–6 Pa·m3·s–1 (1 × 10–5 std cm3·s–1),
sensitivity that is important in practical        knowing that the accuracy of the leakage
leak testing.                                     measurement is a factor of two. There is
                                                  reasonable assurance that if the measured
Effect of Tracer Gas Purity                       leakage is not higher than that stated on
on Accuracy of Leakage                            the specification, 1 × 10–6 Pa·m3·s–1
Measurements                                      (1 × 10–5 std cm3·s–1), the actual system
                                                  leakage will be no greater than the
Another source of inaccuracy is the               allowable rate, 2 × 10–6 Pa·m3·s–1
impurity of the tracer gas used for leakage       (2 × 10–5 std cm3·s–1). This technique of
measurement. If a tracer probe technique          specifying leakage is much more sensible
of leak location is used, the gas is sprayed      than specifying a slightly higher leakage
over the suspected area in the                    value, such as 2 × 10–6 Pa·m3·s–1
environmental atmosphere. In such a               (2 × 10–5 std cm3·s–1), and thereby
case, it is quite possible that the tracer gas    requiring an unreasonably high accuracy
is diluted with air as it approaches the          (such as ±10 percent) during leak testing.
leak. Therefore, the response of the leak
detector operating on the internal
vacuum of the test system will be reduced
by the amount air impurity entering the
detector with the tracer gas. In this case, a
calibrated leak with a self-contained gas
supply is undesirable because it would not
reproduce the leakage measurement
technique. In other words, the gas should
be sprayed onto the calibrated leak in the
same manner as onto the tested leak. The
gas in a self-contained calibrated leak
would be purer than the gas encountered
by simple spraying from a tracer probe.
80 Leak Testing
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PART 2. Operation of Standard (Calibrated)
Halogen Leaks
Functions of Known                                            Halogen Leak Calibrator
Leakage Standards                                             without Reservoir
The halogen gas leak detector (known also                     Figure 8 shows a leak calibrator that has
as the alkali ion diode halogen leak                          no reservoir for halogen tracer gas. It
detector) is a transfer agent or compactor.                   contains a single orifice in heat resistant
Leak testing with halogen tracer gas                          glass. When a reservoir of refrigerant-134a
requires use of a known reference halogen                     is attached, the pressure of the
leak to calibrate the leak testing operation                  refrigerant-134a gas is 165 kPa gage
properly. The halogen leak detector is                        (24 lbf·in.–2 gage) and that gas will leak
adjusted to produce an alarm or meter                         through its orifice at a fixed rate.
indication of the panel indicator when
exposed to a known leakage rate. The                          Calibrated Halogen Leak
detector is then used to compare                              with Gas Reservoir
unknown leakage rates to the specific
known leakage rate of a calibrated                            The calibrated halogen leak of Fig. 3 has
reference leak.                                               its own refrigerant-134a reservoir plus a
                                                              leak factor gage. The gage reads in
    The maximum acceptable leakage rate,                      multiplying factors, used when the
however, must first be determined, either                     pressure is changed to vary the leakage
by the user or from specifications that the                   rate. The gage is set at a factor of 1 at the
user must meet. The type and range of                         factory (165 kPa or 24 lbf·in.–2 gage).
leak standard then may be selected, but                       These leak capsules, used when a precise
only after this has been accomplished.                        leakage rate is required, are frequently
Three types of halogen leak standards are                     mounted in the halogen leak detector
(1) the calibrated standard leak (no gas),                    control unit.
(2) the leak capsule (single gas reservoir)
and (3) the halogen leak standard (reserve
gas supply).
FIGURE 8. Calibrator for halogen leak standards with small    Adjustable Halogen Leak
bore capillary tube orifices for leaks from 3 × 10–5 to       Standards with Ballast
3 × 10–8 Pa·m3·s–1 (3 × 10–4 to 3 × 10–7 std cm3·s–1) or      Tank
with larger bore capillary tube orifices for leaks from
3 × 10–4 to 3 × 10–7 Pa·m3·s–1 (3 × 10–3 to                   The halogen leak standard shown in
3 × 10–6 std cm3·s–1). Movement of a colored liquid within    Fig. 4a contains a reservoir of liquid
the calibrated capillary tube over a specific period of time  refrigerant-134a, which is valved in
                                                              gaseous form into a ballast tank.
permits calculation of the rate of leakage from the standard  Connected to the ballast tank is a glass
                                                              capillary tube and pressure gage. The
leak, when the calibrator is attached to the standard         amount of leakage is dependent on the
                                                              amount of refrigerant-134a tracer gas
through a vent valve.                                         pressure in the ballast tank. Pressure is
                                                              indicated by a Bourdon gage and
                                                              controlled by two valves (Fig. 4b).
                                                              Applications of Calibrated
                                                              Halogen Leaks and
                                                              Capsules
                                                              Predetermined standard halogen leaks are
                                                              of great advantage to quality control
                                                              engineers in refrigeration, air
                                                              conditioning and space vehicle
                                                                                                                              Calibrated Reference Leaks 81
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manufacturing, where critical checks of      second (std cm3·s–1) and also in ounce per
lines, valves and hydraulic systems are of   year (oz·yr–1) by the manufacturer of these
the utmost importance. They afford great     standard leaks. The SI units are mole per
accuracy wherever halogen leak detectors     second (mol·s–1) and pascal cubic meter
are used and where a leak of one specific    per second (Pa·m3·s–1).
value is required.
                                             Components of Adjustable
    The adjustable halogen leak standard     Halogen Leak Standard
in Fig. 4 provides the same advantages as
the calibrated leaks and capsule but has     The adjustable halogen leak standard is a
the additional advantage of being            compact instrument consisting of the
adjustable to the full scale rating. Thus,   following seven functional components
they can be used more easily for             (see Fig. 4):
quantitative measurements of actual leaks
and of background contamination. Leak         1. direct reading leakage rate indicator
standards also enable the establishment of        (calibrated in ounces of
leakage rate specifications and provide           refrigerant-134a per year);
uniform standards for calibrating leak
detectors at each location of product         2. probe fitting in the center of which is
inspection.                                       a glass leak capillary (a different
                                                  capillary for each leakage rate);
Halogen Leak Standards to
Prolong Life of Alkali Ion Diode              3. leakage increase valve and control
Sensing Element                                   knob;
All three leak standards can be used to       4. leakage decrease valve and control
extend the useful life of the alkali ion          knob;
diode sensing elements in heated anode
halogen leak detectors. Users frequently      5. vent (with protective cap) for
replace the detector’s sensitive element          exhausting refrigerant-134a gas;
long before the end of its useful life. A
sensing element can be used until it no       6. tank for holding liquid
longer responds to the desired setting of         refrigerant-134a (the tank contains
the leak standard. Additionally, any leak         some refrigerant-134a when shipped
standard permits use of the lowest                from the factory); and
possible anode heater current to provide
adequate leak detector sensitivity. This      7. a reservoir for holding refrigerant-134a
practice increases element life and results       gas at a pressure corresponding to the
in reduced maintenance and lower                  desired leakage rate.
replacement costs.
                                             Principles of Operation of
Accuracy of Adjustable                       Adjustable Halogen Leak
Halogen Leak Standards                       Standard
Typical accuracy of the adjustable halogen   The adjustable halogen leak standard
leak standard of Fig. 4 is about ±20         (Fig. 5) operates as discussed below. The
percent of scale setting on the upper two    filler tank provides a supply of
thirds of the scale and ±30 percent of       refrigerant-134a liquid under its own
scale setting on the lower one third of the  partial pressure. The increase valve
scale.                                       controls the amount of refrigerant gas fed
                                             from the filler tank to the ballast tank, the
Description of Adjustable                    leakage rate meter and the leak capillary.
Halogen Leak Standard                        The pressure in the system is maintained
                                             by the ballast tank. With the increase and
The leak standard of Fig. 4 is a simple,     decrease valves closed, the system is
accurate instrument that expels a halogen    practically in a static state, except for the
compound gas, refrigerant-134a through a     minute amount of refrigerant gas that
glass capillary marked probe to the          escapes through the leak capillary. The
atmosphere at a known rate. This known       decrease valve provides a means of
rate is adjustable when using certain        decreasing the pressure built up in the
halogen leak standards. The leak standard    system. With the decrease valve opened,
is intended primarily for use with halogen   refrigerant gas is allowed to escape
sensitive leak detectors. The leakage rate   through the vent opening on the front of
for each unit is marked on the scale plate.  the leak standard. The rate of refrigerant
Leakage rates are customarily labeled in     gas escaping through the leak capillary is
units of standard cubic centimeter per       a function of the pressure in the system
                                             and is indicated on the leakage rate meter.
82 Leak Testing
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Preparation for Operation                         1. To check the operation and sensitivity
of Adjustable Halogen                                 of the halogen leak detector. The
Leak Standard                                         probe of the detector to be checked is
                                                      moved past the probe fitting of the
The following procedure is used with                  leak standard, which is set at the
adjustable halogen leak standards.                    maximum leakage rate allowable for
                                                      any single leak on the item being leak
 1. Remove the protective caps from the               tested. If an adequate signal is
     leak capillary in the probe fitting and          obtained, the leak detector has
     from the vent.                                   sufficient sensitivity (or more) to
                                                      detect this rate of leakage.
 2. To increase the leakage rate, turn
     increase valve knob counterclockwise         2. To determine size of leaks. If the leak
     slowly until the instrument pointer              standard is set so that the leak detector
     starts to move upscale. As the pointer           gives the same signal for the leak
     approaches the desired leakage rate,             standard as for the leak, the leak
     gradually close the increase valve so            standard then indicates the size of the
     the pointer will stop at the desired             leak, only if 100 percent pure
     leakage rate. If the instrument pointer          refrigerant-134a is in the test system.
     continues to go upscale, this indicates
     that the increase valve is not firmly        3. To extend the useful life of the sensing
     closed. Always make sure the increase            element of the halogen leak detector.
     valve is closed firmly. (Avoid running           Users frequently replace the detector’s
     the instrument pointer off scale. This           sensing element long before the end
     can subject the instrument to as much            of its useful life. A sensing element
     as 500 percent over pressure. Although           can be used until it no longer
     the unit can withstand the overload,             responds to the desired standard leak
     repeated abuse may damage it.)                   setting. Additionally, the leak standard
                                                      permits use of the lowest possible
 3. To decrease the leakage rate, turn the            heater current to provide adequate
     decrease valve knob counterclockwise             leak detector sensitivity. These
     slowly until the instrument pointer              practices increase element life and
     starts to move downscale. As the                 result in reduced maintenance and
     pointer approaches the desired leakage           lower replacement costs.
     rate, gradually close the decrease valve
     so that the pointer will stop at the         4. To simplify establishment of leakage
     desired leakage rate. If the instrument          rate specifications. The leak standard
     pointer continues to go downscale,               makes feasible the establishment of
     indication is that the decrease valve is         leakage rate specifications and
     not firmly closed. Make sure the                 provides a uniform standard for
     decrease valve is closed firmly.                 calibrating leak detectors at each
                                                      location of product inspection.
 4. After increasing or decreasing the
     leakage rate, be sure both valves are        5. To improve product quality. By
     closed by turning knobs clockwise.               calibrating leak detectors with the leak
                                                      standard, it becomes possible to locate
 5. After increasing or decreasing the                and repair all significant leaks. This
     leakage rate and noting that the valves          ensures that products are
     are firmly closed, wait about 60 s for           manufactured in accordance with
     the leakage rate to stabilize before             leakage specifications.
     calibrating the leak detector. When the
     leakage rate is being decreased,            Precautions for Adjustable
     refrigerant-134a gas is allowed to          Halogen Leak Standard
     escape through the vent to
     atmosphere. During this operation it is     The following precautions should be
     best to remove the leak standard from       applied when using the adjustable
     the test area to avoid building up a        halogen leak of Fig. 4. Never allow any
     background of halogen vapor at the          grease or liquid to enter the leak capillary,
     test site. If this is not possible, attach  as it may plug the leak or alter its leakage
     the vent tubing to the vent and             rate. When the leak standard is not in use,
     discharge the gas from the test area        it is recommended that the instrument
     through a window or other vent.             pointer be set up scale and that the
                                                 protective caps be placed over the vent
 6. The leak standard is now ready for use.      and leak capillary. This must be done to
                                                 prevent plugging of the capillary.
Applications of Adjustable
Halogen Leak Standard
The adjustable halogen leak standard of
Fig. 4 may be used in several ways.
                                                                                                                              Calibrated Reference Leaks 83
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Operational Procedure                                                   100 percent tracer gas probe intake
When Pressurized System                                                 and the signal obtained during normal
Contains 100 Percent                                                    probing procedure.
Refrigerant
                                                                   Interpretation of Unknown
With the leak standard prepared for use,                           Leakage Rate from
proceed as follows.                                                Comparable Standard Leak
 1. Turn on the leak detector and let it                           A leak that gives the same leak signal as
     warm up for the time prescribed in the                        the standard is the same size as that
     applicable leak detector instruction                          indicated by the leak standard. A larger or
     book. Set the leak detector in the same                       smaller signal indicates a larger or smaller
     mode of operation as that to be used                          leak, respectively. If it is desired to
     during leakage testing.                                       determine the size of any leak that is
                                                                   located, adjust the leak standard in small
 2. Place the probe squarely against the                           leakage rate increments (waiting about
     probe fitting on the leak standard (see                       60 s after each change) until the signal
     Fig. 4) and observe the indicator                             caused by the leak standard is the same as
     reading. Remove the leak detector                             that caused by the leak. The leak standard
     probe tip from the leak standard probe                        then indicates the size of the leak in
     fitting. When the leak detector reading                       question, in terms of its leakage rate.
     has settled to a stationary indication,
     pass the tip of the leak detector probe                       Operational Procedure
     past the probe fitting on the leak                            When Pressurized System
     standard at a rate of about 25 mm·s–1                         Contains Less than 100
     (1 in.·s–1). The tip of the probe should                      Percent Refrigerant
     just graze the front circular edge of the
     probe fitting and pass across the                             Halogen leak standards can also be used
     center of the probe fitting as shown in                       to calibrate a leak detector when the
     Figs. 4 and 9.                                                system being checked contains less than
                                                                   100 percent refrigerant-134a. For
 3. Repeat the procedure of step 2 above,                          applications using mixed gases in
     reducing or increasing the sensitivity                        pressurized components, the leak standard
     setting of the leak detector each time,                       may be used to calibrate a leak detector.
     until the leak detector signal is                             However, a leak from the vessel (such as a
     adequate for the specified leakage rate.                      tank, pipe or steam condenser) that
     The results of this test will indicate the                    produces the same leak signal as does the
     allowed probing speed and the safety                          leak standard will have a total leakage rate
     factor required and provide the                               that is approximately inversely
     operator with a feeling for the                               proportional to the percentage of
     difference in indications between a                           refrigerant-134a tracer gas in the
                                                                   enclosure. For example, suppose that,
FIGURE 9. Technique for checking leak                              with 10 percent refrigerant-134a in the
testing sensitivity with sniffer probe tip                         vessel, the leak standard indication is 30 g
moving past the orifice of an adjustable leak                      per annum (1 oz·yr–1). The total leakage
standard.                                                          rate is then 100/10 × 30 = 300 g·yr–1
                                                                   (10 oz·yr–1).
                               Tip of sniffer probe leak detector
                                                                       Halogen leak standards are also used to
                                                                   calibrate a leak detector when test systems
                                                                   contain a halogen tracer gas other than
                                                                   refrigerant-134a, such as refrigerant-22,
                                                                   refrigerant-114 or refrigerant-11. The
                                                                   leakage rates for these other tracer gases
                                                                   may be read directly in standard cubic
                                                                   centimeter per second. Leakage rates in
                                                                   ounce per year can be obtained by
                                                                   multiplying the readings in standard
                                                                   cubic centimeter per second by 5.5 × 104.
                                                                   Readings in pascal cubic meter per second
                                                                   can be obtained by dividing the reading
                                                                   in standard cubic centimeter per second
                                                                   by a factor of 10.
84 Leak Testing
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Measuring Atmospheric                            Use of Calibrator for
Contamination with                               Halogen Leak Standard
Adjustable Halogen Leak
Standard                                         The calibrator is an accessory designed to
                                                 check the accuracy of calibrated leaks,
To measure the amount of atmospheric             leak capsules and halogen leak standards.
contamination with a heated anode                Three models of the calibrator differ in
halogen vapor leak detector, the                 the bore size of the calibrated glass
equipment required includes an                   capillary tube, which is the major
adjustable halogen leak standard, a              component of the calibrator. A small bore
halogen leak detector and a pure air             capillary tube is used for leaks from
supply. The procedure recommended by             3 × 10–5 to 3 × 10–8 Pa·m3·s–1 (3 × 10–4 to
the leak detector manufacturer is as             3 × 10–7 std cm3·s–1). A larger bore
follows.                                         capillary tube is used for leaks from
                                                 3 × 10–4 to 3 × 10–7 Pa·m3·s–1 (3 × 10–3 to
 1. In contaminated test areas, with the         3 × 10–6 std cm3·s–1). Another model is
     leak detector operating at an air flow      supplied with both capillary tubes.
     of 4 cm3·s–1 (0.5 ft3·h–1), allow the leak
     detector to breathe pure air for about          The major component of the calibrator
     1 min, then allow the leak detector to      is a calibrated glass capillary tube.
     breathe air from the contaminated           Accessories are provided allowing the
     area. If the leak detector gives a signal,  capillary tube to be connected to and
     the area is contaminated. Note the          supported by the halogen standard leak
     magnitude of the leak detector signal.      under test. To perform a calibration, the
     Do not adjust the sensitivity setting of    calibrator is attached to the standard leak
     the leak detector between this              through a vent valve. A colored indicating
     measurement and that which follows.         liquid is inserted into the open end of the
                                                 capillary tube and the vent valve is
 2. Move the leak detector and leak              opened. The indicating liquid is drawn
     standard to an area where there is no       into the capillary tube by applying a
     atmospheric contamination. Adjust           slight suction to the plastic suction tube
     the leak standard so that when the          connected to the vent valve. The vent
     leak detector sniffs the reference leak,    valve is then closed, retaining all the
     the leak signal is the same as when the     escaping halogen vapor in the capillary
     leak detector sniffed air in the            tube of the calibrator. By noting the
     contaminated area. Note the leakage         amount of movement of the indicating
     rate shown on the dial of the leak          liquid in the capillary tube for a specific
     standard. This is a measure of the level    period of time, the magnitude of the leak
     of atmospheric contamination with           from the standard can be calculated and
     halogen vapors in the original              compared with the reading of the leakage
     contaminated area measured in step 1.       rate gage on the standard.
 3. If it is desired to determine
     (approximately) the degree of
     contamination of the contaminated
     area in parts per million (µL·L–1) of
     halogen gas, the reading of the leak
     standard from Step 2 in ounces per
     year can be multiplied by 16. For
     example, if the indication on the
     reference leak is 1.5 oz·yr–1 the
     contamination level is 1.5 × 16 =
     24 µL·L–1. (For a leakage in grams per
     year, divide the number by 1.8 to
     arrive at the number of parts per
     million.)
 4. When using a leak detector that has its
     own integral pure air supply, an
     indication of the degree of
     atmospheric contamination with
     halogens can be obtained by holding a
     finger over the probe tip for 30 s and
     then switching the leak detector to
     manual zero with the other hand. If
     the leak detector reading is then
     greater than the indication received
     with leakage of the rejection level, the
     halogen contamination of the air in
     the test area is excessive.
                                                                                                                              Calibrated Reference Leaks 85
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PART 3. Operation of Standard (Calibrated)
Helium Leaks
Functions of Calibrated                        tracer gas or gas mixture flowing through
Helium Reference                               the leak and (3) the pressure differential
Standard Leaks                                 acting across the leak.
Calibrated helium standard leaks are               In the viscous flow range, the mass
essential when helium is used as the tracer    flow rate is inversely proportional to the
gas in leak testing for quantitative leakage   gas viscosity and directly proportional to
rate measurements. Calibration serves to       the difference in the squares of the
determine the user’s ability to detect         upstream and downstream pressures. In
leakage and to perform quantitative            the molecular flow range, the mass flow
measurement of leakage rates. It is            rate is inversely proportional to the square
imperative that the entire leak testing        root of the mass of the gas molecule and
system be calibrated. It is not sufficient     directly proportional to the difference in
merely to calibrate the leak testing           partial pressure. Leakage at rates of
instrument. In the case of a detector probe    1 × 10–5 Pa·m3·s–1 (10–4 std cm3·s–1) or
test, for example, the detector probe must     greater will be most likely to be viscous
be included in the leak testing system         flow. Leakage at rates between 10–5 and
during the calibration operations and used     10–8 Pa·m3·s–1 (between 10–4 and
in the normal manner as during testing.        10–7 std cm3·s–1) will usually be
                                               transitional in nature, exhibiting
    The difficulty of repeating exact          characteristics of both molecular and
detector probe techniques virtually            viscous flow. Leakage at rates in the range
precludes the detector probe method as a       of 10–8 Pa·m3·s–1 (10–7 std cm3·s–1) or
way of measuring leakage rates                 smaller will probably be molecular.
quantitatively, although detector probe
tests are good qualitative tools. In vacuum    Membrane or Diffusion
pumped systems, the system leak and the        Calibrated Reference
artificial reference leak must be located      Helium Leaks
very close to each other for the
quantitative measurement to be valid.              Two types of helium standard leaks or
                                               calibrators are in general use, namely the
Rating of Calibrated Helium Leaks              membrane type and the capillary type.
                                               The design of a membrane or diffusion
Calibrated helium leaks are usually            type standard leak is shown in Fig. 2. This
measured in units of pascal cubic meter        standard leak has a reservoir filled with
per second (Pa·m3·s–1) or standard cubic       helium surrounding a sealed glass tube
centimeter per second (std cm3·s–1). It is     through which helium diffuses at a very
expected that standards in the future will     low rate, usually from 10–8 to
be calibrated in mass flow units of mole       10–10 Pa·m3·s–1 (10–7 to 10–9 std cm3·s–1).
per second. However, when discussing the       The standard calibrated helium leak
flow of a compressible fluid, it is necessary  shown in Fig. 2 is fitted with a shutoff
to state not only the volumetric flow rate     valve that uses a metallic seal rather than
(V/t) but also pressure P and temperature      an elastomeric seal. This avoids spurious
T. Note that the units of leakage are          changes in leakage rate due to helium
identical to the units of throughput (the      hangup. The reservoir is filled with
product PS of pressure P and pumping           100 percent helium at 100 kPa (1 atm or
speed S). Both leakage and throughput          14.7 lbf·in.–2 absolute) of pressure. During
describe the mass flow rate or, actually,      calibration of this leak, the pressure
the number of gas molecules escaping per       differential feeding helium tracer gas into
unit time if the temperature is given.         an evacuated test system is therefore from
                                               100 kPa to 0 kPa (14.7 to 0 lbf·in.–2).
Characteristics of Gaseous Flow                Because the partial pressure of helium in
Involved in Leakage Calibrations               air is only about 0.5 Pa (4 mtorr), the glass
                                               membrane calibrator of Fig. 2 continues
At least three additional variables must be    to leak helium even when it is not under
considered when using standard                 vacuum.
calibrated leaks: (1) the nature of flow
(viscous, transitional or molecular) of gas
passing through the leak, (2) the specific
86 Leak Testing
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Capillary Standard                             (1) Q2 =           M1  Q1
Calibrated Helium Leaks                                           M2
The capillary helium leak consists merely      where Q1 is flow rate for gas 1 (any units
of flattened tubing or glass capillary         of leakage rate), Q 2 is flow rate for gas 2
enclosed in a protective metallic sheath.      (same units of leakage rate) and M1 is
They are generally calibrated with one         molecular mass for gas 1 (relative atomic
end at vacuum and the other end at
atmospheric pressure. Capillary leak           mass).
standards are available with fixed leakage
rates varying from 10–3 to 10–6 Pa·m3·s–1      Computation of Viscous
(10–2 to 10–5 std cm3·s–1). These capillary    Flow Leakage Rates for
leaks may have self-contained helium           Other Gases from Helium
reservoirs. They are more susceptible to       Leakage Rates
drastic changes in leakage rate caused by
clogging or by foreign agents such as dust     If the flow rate has been identified as
or condensation than are membrane leaks.       corresponding to viscous flow for one gas,
                                               the viscous flow rate for any other gas can
Computation of Molecular                       be determined by use of Eq. 2:
Flow Leakage Rates for
Other Gases from Helium                        (2)  Q2 =          n1  Q1
Leakage Rates                                                     n2
Although helium is commonly used as the        where Q1 is flow rate for gas 1 (any units
tracer gas for mass spectrometer leak          of leakage rate), Q 2 is flow rate for gas 2
testing, it is usually necessary to determine  (same units of leakage rate), n1 is viscosity
the rate at which air would leak through a     of gas 1 (pascal second) and n2 is viscosity
similar discontinuity. In the molecular        of gas 2 (pascal second).
flow range (and only in the molecular
flow range), the air leakage rate will be          Table 1 lists the viscosities and
about 35 percent of the helium leakage
rate through the same pressure differential.   molecular masses of helium, argon and
When molecular flow occurs, the flow rate
for one gas can be compared to the flow        neon inert tracer gases, air, nitrogen,
rate of any other gas by use of Eq. 1:
                                               ammonia and other gases and vapors
                                               commonly encountered in leak testing.
                                               The values of the viscosities and
                                               molecular masses from this table can be
                                               used in Eqs. 1 and 2 to compute leakage
TABLE 1. Physical properties of certain gases and vapors.
                                   Relative         Gas
                         Chemical  Molecular        Constant          _V_i_s_c_o_s_it_y__a_t_1_5__°_C__(_5_9_°_F_)_
                                                                         µPa·s (millipoise)
Gas                      Symbols   Mass (Mr)        (J·kg–1·K–1)
                                                                         174 (1.74)
Air                      NH3        29.00            287                   97 (0.97)
Ammonia                  Ar         17.03            488.22
Argon                               40               207.86              220 (2.20)
Carbon dioxide           CO2        44.01            188.89              145 (1.45)
Dichlorodifluoromethane  CCl2F2    120.93                                127 (1.27)
Dichloromethane          CH2Cl2     84.83              68.75
Helium                   He                            98                192 (1.92)
Hydrochloric acid                     4.00          2078.60              140 (1.40)
Hydrogen                 HCI        36.50            227.79
Krypton                                             4116.04                86 (0.86)
Methane                  H2           2.02             99.22             246 (2.46)
Neon                     Kr         83.80            518.35              107 (1.08)
Nitrogen                            16.04            412.01              309 (3.09)
Nitrous oxide            CH4        20.18            296.84              173 (1.73)
Oxygen                   Ne         28.01            188.96              143 (1.43)
Refrigerant R-134a                  44.00            259.91              199 (1.99)
Sulfur dioxide           N2         31.99              81
Sulfur hexafluoride      N2O       102.03            129.91              123 (1.23)
Water vapor              O2         64.00              57                152 (1.52)
                         C2H2F4    146               461.40
                         SO2        18.02                                  93 (0.93)
                         SF6
                         H2O
                                                                                                                              Calibrated Reference Leaks 87
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