1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 1 Of 56
Standard Operating Procedure
Gravimetric Calibration of Volumetric Apparatus and Preventative
Maintenance Practices
THIS DOCUMENT MAY NOT BE REPRODUCED WHOLLY OR IN PART WITHOUT THE EXPRESSED WRITTEN
PERMISSION OF
INTEGRATED SERVICE SOLUTIONS, INC. A TRESCAL COMPANY
AN ISO 9001:2015 REGISTERED COMPANY
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 2 Of 56
Table of Contents
1.0 Purpose ................................................................................................................................. 3
2.0 Scope .................................................................................................................................... 3
3.0 Records ................................................................................................................................. 3
4.0 Responsibilities ..................................................................................................................... 4
5.0 Definitions ............................................................................................................................. 4
6.0 References ............................................................................................................................ 6
7.0 Environmental Requirements ............................................................................................... 7
8.0 Calibration Frequency, Limits and Test Points ..................................................................... 8
9.0 General Safety Issues .......................................................................................................... 15
10.0 Materials and Equipment ................................................................................................... 16
11.0 General Instructions: .......................................................................................................... 17
12.0 ‘As Found’ Condition Determination: ................................................................................. 47
13.0 Calibration Adjustment:...................................................................................................... 47
14.0 ‘As Left’ Condition / Submittal: .......................................................................................... 47
15.0 End of procedure ................................................................................................................ 47
16.0 Balance Suitability Testing (Optional):................................................................................ 48
17.0 Addendum: Reference Water Density Conversion Table ................................................... 49
18.0 Addendum: Reference Z factors: ........................................................................................ 50
19.0 Addendum: Example of Accredited Certificates: ................................................................ 51
20.0 Addendum: Examples of Calibration Labels: ...................................................................... 52
21.0 Revision History .................................................................................................................. 53
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 3 Of 56
Gravimetric Calibration of Volumetric Apparatus and Preventative
Maintenance Practices
1.0 Purpose
1.1 The following are the purposes of this Standard Operating Procedure:
1.1.1 To standardize Integrated Service Solutions, Inc. A Trescal Company processes
used by technicians to calibrate instruments and devices included in the scope
of this procedure. The sole exception is whenever a Client specifically requests
an exemption to this policy.
1.1.2 To secure sufficient documentation for compliance with applicable regulating
agencies and Client requirements including, but not limited to: International
Organization for Standardization (ISO); Current Good Manufacturing Practices
(cGMP); Pharmacopeia requirements (i.e. – USP); current industry standards.
2.0 Scope
2.1 The scope of this procedure includes, but is not limited to, the gravimetric calibration
and preventative maintenance of:
2.1.1 Piston Operated Volumetric Apparatus (i.e. – Pipettes single channel, Pipettes
multi-channel, adjustable or fixed, Burettes, etc.)
2.1.2 Syringes
2.1.3 Dispensers are included, but have separate default tolerances and test points.
Figure 2-1, Typical Single Channel Pipette or Multi-channel Pipette
2.2 The scope of this procedure excludes the calibration of:
2.2.1 Auto-samplers
2.2.2 Dilutors
2.2.3 Non-gravimetric methods of calibration, including photometric and titrimetric.
3.0 Records
3.1 Records of services will be generated and be managed in accordance with the
Company Quality Assurance Manual, ISO-QAM-1001, current revision.
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 4 Of 56
4.0 Responsibilities
4.1 Integrated Service Solutions, Inc. A Trescal Company is responsible for:
4.1.1 Providing qualified service personnel to perform all tasks defined in this
procedure. Personnel qualifications will be based upon formal and/or on-the-
job training.
4.1.2 Providing all necessary documentation to the client in a timely manner and
complying with the user requirements.
4.1.3 Providing all necessary standards and equipment to complete the service as
defined in the project service proposal/agreement.
4.2 The Client is responsible for:
4.2.1 Designating a site contact for company personnel. The site contact is
responsible for all communications (verbal and written) between Integrated
Service Solutions, Inc. A Trescal Company and the Client. This includes, but is
not limited to scheduling of all required work, resolution of conflicts, and
completion/review of all necessary paperwork.
4.2.2 Ensuring that all Client site safety and other required contractor procedures are
disclosed to Company Personnel and that all Company Service Personnel
assigned to the site have received formal training on those procedures.
4.2.3 Ensuring a safe physical operating environment for all Company Service
personnel.
4.2.4 When applicable, to provide operator assistance for equipment or devices that
require calibration.
4.2.5 Providing additional materials and support equipment as defined in the project
service proposal/agreement.
4.2.6 Providing any necessary documentation (i.e. – manuals, SOPs, etc) to complete
all proposed services.
4.2.7 To retain all original completed documentation by Integrated Service Solutions,
Inc. A Trescal Company via internal storage procedures.
5.0 Definitions
5.1 Accuracy: The degree of agreement between the measured value of a quantity and
the accepted value for that quantity.
5.2 Calibration: The comparison of measuring and test equipment of unknown accuracy
(UUT) to a measurement standard of known accuracy in order to detect, correlate,
report, or eliminate by adjustment any variation in the accuracy of the instrument
being compared.
5.3 Measuring and Test Equipment (M&TE): All devices used to measure, gage, test,
inspect, or otherwise determine compliance with prescribed technical requirements.
5.4 Measurement Standard: Those devices used to calibrate measuring and test
equipment or other measurement standards and provide traceability. Typically, the
required TUR of the measurement standard to the measuring and test equipment is ≥
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 5 Of 56
4:1, but may not be necessary in all cases. The minimum allowable TUR for a
measurement is 1:1.
5.5 Precision: The degree of consistency, repeatability, and resolution of independently
measured values of a quantity or parameter under specified conditions.
5.6 Quality: Meaning the totality of features and characteristics that bear on the ability
of a device to satisfy fitness-for-use, including safety and performance.
5.7 Range of Interest (ROI): Terminology used to express a bracketed area within the
dynamic measurement range of an instrument, where the lowest and highest
process measurement observations possible are encompassed.
5.8 Test Accuracy Ratio (TAR): The ratio of measurement accuracy required by the unit
to the measurement accuracy provided by the test instrumentation.
5.9 Test Uncertainty Ratio (TUR): The ratio of the tolerance of the instrument being
calibrated to the uncertainty of the standard.
5.10 Tolerance: The maximum permissible variation or limits allowed a quantity /
parameter from a specified value.
5.11 Traceability: The ability to relate individual measurement results through an
unbroken chain of calibrations to one or more of the following: standards maintained
by the NIST, fundamental or natural physical constants with values assigned or
accepted by the NIST, national standards of other countries that are correlated with
NIST standards.
5.12 Uncertainty: The range of values within which the true value is estimated to lie. It is a
best estimate of possible inaccuracy due to both random and systemic errors.
5.13 UUT: Abbreviation for “Unit-Under-Test.” It is the instrument or device undergoing
the calibration.
All other terms and definitions that are utilized in this standardizing document have been
deemed as “common knowledge” and as such are not defined in this section.
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 6 Of 56
6.0 References
The following reference material was utilized in the authoring of this procedure:
6.1 ANSI/ISO/ASQ Q9001: current revision: American National Standard Quality
Management Systems: Requirements.
6.2 ANSI/ISO/IEC 17025:2017: International Standards, General requirements for the
competence of testing and calibration laboratories, May 2005.
6.3 FDA Guideline: 21 CFR Part 11 - Electronic Records; Electronic Signatures, Code of
Federal Regulations, Title 21 - Food and Drugs, Chapter I - Food and Drug
administration, Office of the Federal Register, Maryland, USA.
6.4 FDA & ICH Guideline (1994): Q2A Validation of Analytical Procedures: Text, Guidance
for Industry. ICH Harmonized Tripartite Guideline adopted by US Food and Drug
Administration, Maryland, USA, March 1995.
6.5 FDA & ICH Guideline (1995): Q2B Validation of Analytical Procedures: Methodology,
Guidance for Industry. ICH Harmonized Tripartite Guideline adopted by US Food and
Drug Administration, Maryland, USA, November 1996.
6.6 FDA & ICH Guideline (2000): Good Manufacturing Practice Guide for Active
Pharmaceutical Ingredients, Q7A. ICH Harmonized Tripartite Guideline adopted by US
Food and Drug Administration, Maryland, USA, August 2001.
6.7 FDA & ICH Guideline (2009): Q8 (R2) Pharmaceutical Development, Guidance for
Industry. ICH Harmonized Tripartite Guideline adopted by US Food and Drug
Administration, Maryland, USA, November 2009.
6.8 FDA& ICH Guideline (2006): Q9 Quality Risk Management, Guidance for Industry. ICH
Harmonized Tripartite Guideline adopted by US Food and Drug Administration,
Maryland, USA, June 2006.
6.9 FDA & ICH Guideline (2009): Q10 Pharmaceutical Quality Systems, Guidance for
Industry. ICH Harmonized Tripartite Guideline adopted by US Food and Drug
Administration, Maryland, USA, April 2009.
6.10 ISO / IEC Guide 98-3:2008: Uncertainty of Measurement: Guide to the Expression of
Uncertainty in Measurement.
6.11 ISO 8655-1:2002(E): International Standard for Piston-operated volumetric apparatus
– part 1: Terminology, general requirements and user recommendations, first edition
September 2002.
6.12 ISO 8655-2:2002(E): International Standard for Piston-operated volumetric apparatus
– part 2: Piston Pipettes, first edition September 2002.
6.13 ISO 8655-3:2002(E): International Standard for Piston-operated volumetric apparatus
– part 3: Piston Burettes, first edition September 2002.
6.14 ISO 8655-4:2002(E): International Standard for Piston-operated volumetric apparatus
– part 4: Dilutors, first edition September 2002.
6.15 ISO 8655-5:2002(E): International Standard for Piston-operated volumetric apparatus
– part 5: Dispensers, first edition September 2002.
6.16 ISO 8655-6:2002(E): International Standard for Piston-operated volumetric apparatus
– part 6: Gravimetric methods for the determination of measurement error, first
edition September 2002.
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 7 Of 56
6.17 United States Pharmacopoeia (current revision): Monograph <1251> - Weighing on
an Analytical Balance.
6.18 Speedcal Mobile Operating Instructions: Testing System for Multi-channel Piston-
operated Pipettes, 1000030415.
7.0 Environmental Requirements
7.1 The temperature of the test environment, analytical equipment, test water, and UUT
should be identical, and stabilized for at least 2 hours prior to and throughout the
calibration process.
7.2 The ambient relative humidity (RH) should be maintained within 45% to 75% RH in
order to reduce the evaporation bias error. If the RH is <45%, appropriate
precautions must be taken, including the use of an evaporation trap and bias
correction. In order promote stabile readings and reduce evaporation bias error,
technicians will use the evaporation trap at all ambient conditions as permitted by
the volume tested. Note ambient conditions on calibration certificate.
7.3 The analytical equipment location should be free of vibration and air currents.
7.4 The lighting should be of necessary intensity and glare free. Direct sunlight should be
avoided.
7.5 The average barometric pressure in the test laboratory should be known to within ±
25 mBar, when making density conversions manually with Section 17.0. The
barometric pressure will be assumed to be set nominally at 1013 mBar for
calibrations below 100 µLiter full scale volume.
7.6 The local barometric pressure is used to select a conversion factor. The Pipette
Calibration program references a standard barometric pressure of 1013.0 mBar.
Changes in local barometric pressure conditions will result in an error of less than ±
0.1% from 800 mBar to 1067 mBar, which is included in the calculations of
uncertainty.
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 8 Of 56
8.0 Calibration Frequency, Limits and Test Points
Listed below are the default calibration specifications. Actual calibration test points, limits,
replicates, frequency, and levels of service are to be defined by the Client. They are conveyed to
technicians through company work orders and instructions.
8.1 This procedure is recommended to be performed minimally every 3 to 6 months, or
whenever changes or repairs have been made that may affect the accuracy of the
measurement system.
8.2 The default test points are 1 0%, 50%, and 100% of t he nominal volume for an
1
adjustable GLP a pp a r a t us with 5 replicates at each test point. The default test
point for a fixed volume GLP apparatus is at the set volume with 5 replicates. A GLP
multichannel apparatus will have this testing performed on each channel.
Note: Prior to 01 Jan 2021, the default setpoints were 20%, 50%, and 100% of the
nominal volume for an adjustable GLP apparatus. Customers obtained prior to that
date will default to these setpoints if they have not requested specific setpoints.
8.3 The default test point for a Non GLP apparatus is 100% of the nominal volume for an
adjustable Non GLP apparatus with 5 replicates at the set test point. The default
test point for a fixed volume Non GLP apparatus is at the set volume with 5
replicates. A non GLP multichannel ap p ar at u s will have this testing
performed on only 3 of the channels.
8.4 Clients may also select the level of service they require. As with the GLP and Non
GLP pipettes, if 1 test point is selected it will be at 100% of the nominal volume and 3
test points will be at 10%(or20% for clients obtained prior to 01 Jan 2021), 50%, and
100% of the nominal volume. The default levels are as follows:
Services / Description LEVEL 1 LEVEL 2 LEVEL 3 LEVEL 3A LEVEL 4
Single channel: Single channel: Single channel: Single channel: Single channel:
1 test point/5 3 test points/5 1 test point/5 3 test points/5 3 test points/5
replicates. replicates. replicates. replicates. replicates.
Multi channel: Multi channel: Multi channel: Multi channel: Multi channel:
1 test point/ 5 3 test points/5 1 test points/5 3 test points/5 3 test points/5
replicates with 3 replicates with all replicates with 3 replicates with all replicates with all
channels checked channels checked channels checked channels checked channels checked
ISO 17025:2017 Accredited
Calibration Certificate X X X X X
As Found Data reported X X X
As Left Data reported X X X X X
Preventive Maintenance: X X
Failed Calibrations Only
Preventive Maintenance:
100% of Pipettes X X X
Note: See Addendum 19.0 for more information on the difference between accredited and non-accredited
certificates. Levels 3 and 3A are offered for new pipettes or pipettes that are being upgraded, where
the As Found Data would not impact use prior to adjustment.
1 GLP and Non GLP apparatus refers to a level of service provided by the company.
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 9 Of 56
8.5 When limits of error are not specified by the client, the technician will default to
those given in the ISO 8655 series of documents, excluding Customers that have been
serviced by the Company prior to 01 Jan 2021. See the ISO 8655 limits below. The
limits for Customers that have been serviced by the Company prior to 01 Jan 2021
are in section 8.6.
8.5.1 ISO 8655 Limits for Single Channel Fixed-volume pipettes:
8.5.1.1 For fixed-volume air displacement piston pipettes, the maximum
permissible errors in the following table apply. The maximum
permissible errors for piston pipettes with intermediate nominal
volumes (between those given in this table) are equal to the permissible
errors in µL of the next greater nominal volume.
Maximum Possible Error for Air Displacement Pipettes
Nominal volume Maximum permissible inaccuracy Maximum permissible imprecision
µl (systematic error) (random error)
a
a
b
+/- % +/- µl +/- % +/- µl c
1.000 5.0 0.05 5.0 0.05
2.000 4.0 0.08 2.0 0.04
5.000 2.5 0.125 1.5 0.075
10.00 1.2 0.12 0.8 0.08
20.00 1.0 0.2 0.5 0.1
50.00 1.0 0.5 0.4 0.2
100.0 0.8 0.8 0.3 0.3
200.0 0.8 1.6 0.3 0.6
500.0 0.8 4.0 0.3 1.5
1000 0.8 8.0 0.3 3.0
2000 0.8 16.0 0.3 6.0
5000 0.8 40.0 0.3 15.0
10000 0.6 60.0 0.3 30.0
a Expressed as the deviation of the mean of five measurements from the nominal volume or from the selected volume (k=2).
b Expressed as the coefficient of variation of five measurements (k=2).
c Expressed as the standard deviation of five measurements (k=2).
8.5.2 ISO 8655 Limits for Single Channel Variable-volume pipettes:
For variable-volume pipettes, the maximum permissible Inaccuracy and
Imprecision errors are those for the nominal full scale volume (in µL) as given in
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 10 Of 56
the table above, applied to every selectable volume throughout the useful range
of the pipette.
8.5.3 ISO 8655 Limits for Multi-Channel pipettes:
The maximum permissible systematic and random errors of multi-channel
piston pipettes shall be equal to twice the values specified for single-channel
piston pipettes.
8.5.4 ISO 8655 Limits for Single Stroke dispensers:
8.5.4.1 For single stroke dispensers, the maximum permissible errors in the
following table apply. The maximum permissible errors for dispensers
with intermediate nominal volumes (between those given in this table)
are equal to the permissible errors of the next greater nominal volume.
Nominal volume Maximum permissible inaccuracy Maximum permissible imprecision
ml (systematic error) (random error)
b
a
a
+/- % +/- µl +/- % +/- µl c
0.01 2.0 0.2 1.0 0.1
0.02 2.0 0.4 0.5 0.1
0.05 1.5 0.75 0.4 0.2
0.1 1.5 1.5 0.3 0.3
0.2 1.0 2.0 0.3 0.6
0.5 1.0 5.0 0.2 1.0
1 0.6 6.0 0.2 2.0
2 0.6 12.0 0.2 4.0
5 0.6 30.0 0.2 10.0
10 0.6 60.0 0.2 20.0
25 0.6 150.0 0.2 50.0
50 0.6 300.0 0.2 100
100 0.6 600.0 0.2 200
200 0.6 1200 0.2 400
a Expressed as the deviation of the mean of five measurements from the nominal volume or from the selected volume (k=2).
b
Expressed as the coefficient of variation of five measurements (k=2).
c
Expressed as the repeatability standard deviation of five measurements (k=2).
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 11 Of 56
8.5.5 ISO 8655 Limits for Multiple Delivery dispensers:
8.5.5.1 For multiple delivery dispensers, the maximum permissible errors in the
following table apply. The maximum permissible errors for dispensers
with intermediate nominal volumes (between those given in this table)
are equal to the permissible errors of the next greater nominal volume.
Nominal volume Maximum permissible systematic error Maximum permissible random error
b
a
a
ml +/- % +/- µl +/- % +/- µl c
0.001 5.0 0.05 5.0 0.05
0.002 5.0 0.1 5.0 0.1
0.003 2.5 0.075 3.5 0.11
0.01 2.0 0.2 2.5 0.25
0.02 1.5 0.3 2.0 0.4
0.05 1.0 0.5 1.5 0.75
0.1 1.0 1.0 1.0 1.0
0.2 1.0 2.0 1.0 2.0
0.5 1.0 5.0 0.6 3.0
1 1.0 10 0.4 4.0
2 0.8 16 0.4 8.0
5 0.6 30 0.3 15
10 0.5 50 0.3 30
25 0.5 125 0.3 75
50 0.5 250 0.25 125
100 0.5 500 0.25 250
200 0.5 1000 0.25 500
a Expressed as the deviation of the mean of five measurements from the nominal volume or from the selected volume (k=2) .
b Expressed as the coefficient of variation of five measurements (k=2).
c Expressed as the repeatability standard deviation of five measurements (k=2).
8.6 Customers that have been serviced by the Company prior to 01 Jan 2021 will use the
following default limits of error for precision and accuracy:
8.6.1 Fixed-volume pipettes:
8.6.1.1 For fixed-volume air displacement piston pipettes, the maximum
permissible errors in the following table apply. The maximum
permissible errors for piston pipettes with intermediate nominal
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 12 Of 56
volumes (between those given in this table) are equal to the permissible
errors of the next greater nominal volume.
Maximum Possible Error for Air Displacement Pipettes
Nominal volume Maximum permissible inaccuracy Maximum permissible imprecision
µl (systematic error) (random error)
b
a
a
+/- % +/- µl +/- % +/- µl c
1.000 10.0 0.10 10.0 0.10
2.000 8.0 0.16 4.0 0.08
5.000 5.0 0.25 3.0 0.15
10.00 2.4 0.24 1.6 0.16
20.00 2.0 0.40 1.0 0.20
50.00 2.0 1.0 0.8 0.40
100.0 1.6 1.6 0.6 0.60
200.0 1.6 3.2 0.6 1.20
500.0 1.6 8.0 0.6 3.00
1000 1.6 16.0 0.6 6.00
2000 1.6 32.0 0.6 12.0
5000 1.6 80.0 0.6 30.0
10000 1.2 120.0 0.6 60.0
a Expressed as the deviation of the mean of five measurements from the nominal volume or from the selected volume (k=2).
b Expressed as the coefficient of variation of five measurements (k=2).
c Expressed as the standard deviation of five measurements (k=2).
8.6.2 Variable-volume pipettes:
For variable-volume pipettes, the maximum permissible Inaccuracy and
Imprecision errors (± µL) are those for the nominal full scale volume as given in
the table above, applied to every selectable volume throughout the useful range
of the pipette.
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 13 Of 56
8.6.3 Single Stroke dispensers:
8.6.3.1 For single stroke dispensers, the maximum permissible errors in the
following table apply. The maximum permissible errors for dispensers
with intermediate nominal volumes (between those given in this table)
are equal to the permissible errors of the next greater nominal volume.
Nominal volume Maximum permissible inaccuracy Maximum permissible imprecision
ml (systematic error) (random error)
a
a
b
+/- % +/- µl +/- % +/- µl c
0.01 4.0 0.4 2.0 0.2
0.02 4.0 0.8 1.0 0.2
0.05 3.0 1.5 0.8 0.4
0.1 3.0 3.0 0.6 0.6
0.2 2.0 4.0 0.6 1.2
0.5 2.0 10.0 0.4 2.0
1 1.2 12.0 0.4 4.0
2 1.2 24.0 0.4 8.0
5 1.2 60.0 0.4 20.0
10 1.2 120.0 0.4 40.0
25 1.2 300.0 0.4 100
50 1.2 600.0 0.4 200
100 1.2 1200 0.4 400
200 1.2 2400 0.4 800
a Expressed as the deviation of the mean of five measurements from the nominal volume or from the selected volume (k=2).
b Expressed as the coefficient of variation of five measurements (k=2).
c Expressed as the repeatability standard deviation of five measurements (k=2).
© COPYRIGHT 2021-2024, CONFIDENTIAL & PROPRIETARY
Integrated Service Solutions, Inc., A Trescal Company
1565 Bustard Road
Lansdale, PA 19446
Phone: 610-287-3433 Fax: 610-287-0233
Web: www.integratedservicesolutions.com
Document Type: Standard Operating Procedure Effective Date: 06 Jun 2021
Title: Gravimetric Calibration of Volumetric Apparatus and PM Practices
ID: ISO-SOP-3023 Revision: 26.00 Page: 14 Of 56
8.6.4 Multiple Delivery dispensers:
8.6.4.1 For multiple delivery dispensers, the maximum permissible errors in the
following table apply. The maximum permissible errors for dispensers
with intermediate nominal volumes (between those given in this table)
are equal to the permissible errors of the next greater nominal volume.
Nominal volume Maximum permissible systematic error Maximum permissible random error
a
b
a
ml +/- % +/- µl +/- % +/- µl c
0.001 10.0 0.1 10 0.1
0.002 10.0 0.2 10 0.2
0.003 5.0 0.15 7.0 0.22
0.01 4.0 0.4 5.0 0.5
0.02 3.0 0.6 4.0 0.8
0.05 2.0 1.0 3.0 1.5
0.1 2.0 2.0 2.0 2.0
0.2 2.0 4.0 2.0 4.0
0.5 2.0 10 1.2 6.0
1 2.0 20 0.8 8.0
2 1.6 32 0.8 16
5 1.2 60 0.6 30
10 1.0 100 0.6 60
25 1.0 250 0.6 150
50 1.0 500 0.5 250
100 1.0 1000 0.5 500
200 1.0 2000 0.5 1000
a Expressed as the deviation of the mean of five measurements from the nominal volume or from the selected volume (k=2) .
b Expressed as the coefficient of variation of five measurements (k=2).
c Expressed as the repeatability standard deviation of five measurements (k=2).
8.7 The most current uncertainty of measurement capabilities can be found on
Integrated Service Solutions, Inc. A Trescal Company scope of accreditation. The
scope reports the best uncertainty measurement within the company’s capabilities.
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9.0 General Safety Issues
9.1 The following are general safety issues. Not all may apply to this procedure directly.
9.2 Wear the proper safety attire. This may include, but is not limited to: safety glasses,
safety shoes, hard hats, full-face shields, lab coats/aprons, and gloves. The pipette
software will remind the technician of this requirement.
Note: PPE index B Always applies at a minimum when handling pipettes.
9.3 Inspect area for potential hazardous conditions (i.e. – wet floors, exposed electrical
wires, loosely hanging overhead equipment, other personnel working in the area,
etc.).
9.4 Ensure that pipettes used with bio-hazardous materials have been decontaminated
properly in accordance with local protocols set by the client, before attempting
service. The customer will be required to submit documentation attesting to the
state of decontamination. Do not proceed unless this documentation has been
received.
9.5 To prevent accidental cross-contamination in clean room environments insure that
instrumentation used is cleaned with a 70% Isopropyl Alcohol (IPA) or equivalent,
prior to use.
9.6 Maintain Client pipettes in bagged batches as delivered.
9.7 Review ISO-QSP-2117, General Safety Practices for additional instructions, as
applicable.
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10.0 Materials and Equipment
The following materials and equipment may be necessary for the completion of this procedure:
Test Equipment Type Required Accuracy
Micro-Balance ± 0.01 mg sensitivity
1 to 19 µLiter Full Scale Volume
System TUR/TAR ≥ 4:1 Typical ± 0.01 mg Imprecision
Analytical Balance
± 0.1 mg sensitivity
20 µLiter Full Scale Volume and above ± 0.1 mg Imprecision
System TUR/TAR ≥ 4:1 Typical
Multichannel Pipette Calibrator
± 0.1 mg sensitivity
20 µLiter Full Scale Volume and above ± 0.1 mg Imprecision
System TUR/TAR ≥ 4:1 Typical
Speedcal –M12 ± 0.01 mg sensitivity
10µL to 1.2 mL Full Scale Volume < 0.02 mg Imprecision
System TUR/TAR ≥ 4:1 Typical
Resolution to ± 0.1 °C,
RTD / Thermistors Thermometry System
Accuracy to ± 0.1 °C
(Ambient Air & Water Temperature Monitor) 0° to 40 ° C minimum range of measurement
Hygrometer Less than or equal to 10% uncertainty
Mass Set, 100 g to 1 mg ASTM Class 1 tolerance, OIML weight Class E2 2
As specified for the type and volume of the
Pipette tips
pipette.
Weighing vessel 3:1 height to diameter ratio and/or utilizes a lid
Evaporation trap N/A
Distilled or Deionized Water at room temperature N/A
70% Isopropyl Alcohol (IPA) N/A
Computer with access to the Pipette Calibration
program. N/A
(Speedcal mobile and Pipette Wedge Software
are required for use with the mobile Speedcal.)
10.1 All test equipment is to be traceable to NIST standards and currently in calibration, as
applicable.
2 Use of lower classmass set is allowed, however the certified value from the calibration report must be used.
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10.2 Additional materials that may be expended during the course of routine calibrations
include, but are not limited to:
10.2.1 Pipette specific o-rings, gaskets, filters, and other parts as applicable.
10.2.2 Greases and lubricants as applicable.
10.2.3 Pipette maintenance kit.
10.2.4 Acetone, alcohol, metal polishes and other solvents as applicable for cleaning
and decontaminating instruments.
11.0 General Instructions:
11.1 Pipette techniques
11.1.1 Pipette Operation:
11.1.1.1 Attach the appropriate tip onto the nose cone of the pipette. Use the
tips recommended by the manufacturer for the type and size of the
pipette. Whenever possible use tips that are supplied by the customer.
11.1.1.2 Adjustable pipettes: set the first volume which is to be tested. Work
from the largest to smallest volumes.
11.1.1.3 The each new tip must be pre-wet prior to measuring. Aspirate and
then dispense the set volume five times to reach humidity equilibrium
in the dead air volume.
11.1.2 Pipette Aspiration:
11.1.2.1 Hold the pipette vertically.
11.1.2.2 Immerse the tip approximately 2 to 3 mm into the test liquid.
11.1.2.3 Aspirate the test volume with a slow and uniform motion.
11.1.2.4 Observe the waiting period of 1 to 3 sec., (Take note: the waiting time
depends on the size of the pipette tip; see OEM instruction manual).
11.1.2.5 Pull the pipette tip straight up from the test liquid slowly and uniformly.
11.1.2.6 Examine the tip and remove any remaining liquid by placing the pipette
tip against the inside of the vessel.
11.1.3 Pipette Dispensing:
11.1.3.1 Touch the filled tip against the inside of the weighing vessel at an angle
of approximately 30° to 45°.
11.1.3.2 Dispense the test volume slowly and uniformly down to the first stop
where applicable (measuring stroke).
11.1.3.3 Press the control button to the second stop (blow-out) and dispense any
liquid remaining in the tip.
11.1.3.4 Hold down the control button and pull the tip up along the inside of the
weighing vessel.
11.1.3.5 Slowly and evenly let the control button slide up again.
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11.1.3.6 Determine the weight of the dispensed volume on an analytical balance.
The time required to complete the weighing of a dispensed volume shall
be kept to a minimum, ideally less than 60 seconds.
11.1.4 The Pipette Calibration program software is used to record volumetric
calibrations. The program gathers the mass readings from the analytical
balance, calculates the volume values by making temperature and water density
corrections, and calculates the acceptance limits.
11.2 Pipette Preventive Maintenance:
11.2.1 Preventive maintenance is performed after the As Found data is taken and prior
to taking the As Left data, as required.
11.2.2 Perform preventative maintenance as required by the client or the condition of
the unit. Document any preventive maintenance performed in the appropriate
data entry box in the software. Where applicable, the software will prompt the
service of PM based on the level selected, the date of the last PM performed
and PM interval assigned to the unit.
11.2.3 The default preventive maintenance:
11.2.3.1 Visually inspect the condition of the unit for any physical damage that
may affect the integrity of the unit.
11.2.3.2 Wipe the exterior with a suitable cleaning agent. If not otherwise stated
in the instruction manual, all parts of the pipette can be cleaned with a
soap solution or 70 % Isopropyl Alcohol (IPA). Acetone may also be
used, if needed and not excluded by the instruction manual. Be certain
that all cleaning agents or solvents are completely removed after use
and the instrument is allowed to dry thoroughly.
11.2.3.3 Perform additional maintenance as required.
11.2.4 If Preventive Maintenance is a requirement of a service levels described in
section 8.4, the following must be also performed:
11.2.4.1 Disassemble the pipette and clean with a suitable cleaning agent. Again,
if not otherwise stated in the instruction manual, all parts of the pipette
can be cleaned with a soap solution, 70 % Isopropyl Alcohol (IPA), or
acetone. The parts must then be rinsed with distilled water. Do not
reassemble the parts until they have dried completely.
11.2.4.2 An exception is electronic pipettes and dispensers, which cannot be
opened except by the manufacturer. Examples include: Matrix multi
pipettes, Co-Star multi pipettes, Eppendorf Repeater pipettes, and
Gilson MicroMan pipettes.
11.2.4.3 Lubrication: After cleaning, manual pipettes should be lubricated lightly
using OEM silicon lubricant.
11.2.4.4 Replace seals and/or o-rings, as needed, based on their condition.
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11.2.5 Sterilization: Refer to the OEM instruction manual of the UUT pipette contains
information on cleaning with solvents or autoclaving (121 °C, for 20 minutes), if
sterilization is required. Cleaning with solvents is the preferred method.
11.3 Pipette Leak Test
11.3.1 The leak test is an optional, add-on service that is quoted separately. It is not
part of the standard calibration procedure and therefore is subject to contract
negotiations.
11.3.2 Manual Test Method:
11.3.2.1 To check for leaks, hold the pipette vertically for approximately 15
seconds with a filled tip. Do not touch the pipette tip.
11.3.2.2 Observe the meniscus of the liquid in the pipette tip.
11.3.2.3 If there is a leak, a droplet is visible on the pipette tip.
11.3.2.4 The leak test can also be conducted with transparent PVC tubing or a
leak-test bottle. Recommended tubing sizes;
• 10 to 100 µl 0.5 to 1 mm inner diameter
• 100 to 500 µl 1.5 to 2 mm inner diameter
• 500 to 2,500 µl 5.0 mm inner diameter
11.3.2.5 For this purpose, a 20 cm-long tube is attached to the tip of the pipette.
11.3.2.6 Hold the pipette vertically, aspirate liquid (colored liquid may be used if
desired) and mark the meniscus level on the tube.
11.3.2.7 The meniscus must not sink in the tubing which hangs freely, even after
liquid has been aspirated and dispensed several times (approximately
15 seconds).
11.3.3 Automated Test Method:
11.3.3.1 To perform leak test automatically, use the AND model AD1690 Pipette
Leak Testing Tool, and associated accessories.
11.3.3.2 The Leak Tester determines the presence of a leak by a pressure
change, after the initial pressure is set inside the instrument, to a
maximum of -20kPa ± 4kPa.
11.3.3.3 The amount, -20kPa, attained by evacuating the air with the Leak
Tester, is approximately 0.2 atmospheres (based on atmospheric
pressure at sea level of 100kPa, approximately 1 atmosphere).
11.3.3.4 This Leak Tester is a tool for determining leakage, and is not used to
measure pressure values quantitatively. The Leak Tester displays -20kPa
as a reference pressure and measures leakage as a pressure change (∆P)
from this value.
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11.3.3.5 The Direct Mode of Operation of the AD1690 is in accordance with the
OEM instruction manual.
11.3.3.6 The Indirect Mode of Operation the AD1690 is in accordance with the
Leak Tester Module and instructional Video.
11.3.3.7 Performance of the automated leak test is strictly on a contracted
optional basis, as part of a comprehensive preventative maintenance
program, and will normally be performed in the Indirect Mode.
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Figure 11-1, Indirect Pipette Leak Test
Figure 11-2, A&D AD1690 Pipette Leak Tester
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11.4 Pipette and Volumetric Calibration Methods:
11.4.1 Select a suitable analytical balance as described in the Materials and Equipment
section.
11.4.2 Company field analytical balances (with 5 Digit Resolution) have been verified as
suitable for use for 0.1 µliter to 200.0 milliliter pipettes, excluding the mobile
speedcal which is suitable for 10 µliter to 1.2 milliliters.
11.4.3 If in doubt of the suitability of the balance for the range of interest, perform a
balance suitability test as described in Section 16.0.
11.4.4 Open the Field Pipette software on the computer. If the Speedcal or mobile
speedcal will be used, open the software for that equipment and the Pipette
Wedge software. Refer to Sections 11.10 – 11.11 for further instruction on the
use of that software.
11.4.5 The balance should be set to perform an internal calibration. Consult the
appropriate balance manual to change the settings.
Note: All balances should be set to record to 5 decimal places.
11.4.6 Set-up:
11.4.6.1 Set up a work area with a suitable analytical balance, either a Company
owned asset or as provided by the Customer. The balance must have a
current, valid calibration.
11.4.6.2 At the beginning of the day or after the balance is moved, perform the
following:
11.4.6.3 Ensure the balance is leveled and has been allowed to come into
equilibrium with the environment. Verify the weighing area is clean and
free of debris.
11.4.6.4 Allow the balance to perform an internal calibration or press the
Adjust.int button.
11.4.6.5 Zero the Balance.
11.4.6.6 Perform a balance verification and capture the results on the Balance
Verification Form in the Pipette software. Note: The program will not
allow the technician to record calibrations until this step is completed.
11.4.6.6.1 Select the Verify Balance button for a single weighing
balance or Verify MultiChnl Balance for the mobile
speedcal.
11.4.6.6.2 For a single pan balance, weigh the following nominal
weights on the analytical balance: 1mg, 10mg, 100mg,
1g, 10g, 20g, 50g, 100g, and 110g, unless other weights
are required by the customer. Weigh each once.
11.4.6.6.3 For the mobile speedcal, weigh 10g once on each
channel of the balance.
11.4.6.7 Compare the measured value with the calibrated value of the weight.
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11.4.6.8 If the measured value is within +/-5 counts (single pan balance), or .01g
(mobile speedcal) of the calibrated value of the weight at the balance’s
lowest resolution, it passes the verification test.
11.4.6.9 If the measured value does not meet the above specifications, it fails
the verification test. Remove the weight and repeat the internal
calibration. Repeat the balance verification. If the verification test
continues to fail, return the balance to the Metrology Laboratory for
calibration and repair. No calibrations shall be performed using a
balance that has failed its daily verification.
11.4.7 Obtain a container of distilled or deionized water for use in the calibration
procedure. Allow the water to stabilize to room temperature.
11.4.8 Obtain the appropriate pipette tips, as required, for dispensing and allow the
tips to stabilize to room temperature.
11.4.9 Visually inspect the UUT for any defects, broken or missing parts and note on
the Calibration Data Sheet as necessary.
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11.4.10 For Multi-Channel Pipettes, pick up tips in each channel and draw the maximum
volume. Visually inspect to insure all channels draw and check for visual
uniformity. Note pass or fail in the comments section of the calibration report.
11.5 “As Found” Pipette Condition Determination for 20 µLiter to 1,000 µLiter Pipette
Calibration:
11.5.1 On the Conditions screen of the Field Pipette Software, record the water
temperature and ambient humidity and temperature readings in Celsius using a
calibrated instrument. A multichannel calibrator, such as a MCP or mobile
SpeedCal may be used to take multiple readings at once. Select the MCP box if
using this equipment. If the wedge software is being used, select ISS Wedge as
the Com Type.
11.5.2 On the Standards screen Select the standards being used to perform the
calibration and verify they are not past their calibration due date.
11.5.3 Select the UUT for calibration and record the appropriate data on the
Instrument screen of the Pipette Calibration program. Do not make any repairs
or adjustments prior to taking the “As Found” calibration data (refer to the
service level).
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11.5.4 Select the customer from the dropdown box. Select the instrument
identification from the drop down box or scan the barcode from its calibration
sticker.
11.5.5 Select the appropriate test plan and click on the Add Cal Date button.
11.5.6 The software will display a pop-up box that asks for confirmation that a
decontamination sheet was received for this equipment and that the required
PPE is currently being used.
11.5.6.1 Make sure you are wearing the appropriate PPE as required by the
customer and section 9.0 of this procedure.
11.5.6.2 If you do not have a copy of a decontamination form, obtain one from
the customer and submit to your dispatcher. Review the
decontamination form for any instructions from the customer.
11.5.6.3 Once the decontamination form has been received and the appropriate
PPE is in place, click Yes and proceed with calibration.
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11.5.7 Select the MCP box if the MCP or mobile speedcal is being used and the number
of channels being tested.
11.5.8 Go to the Readings screen and select Import Template.
11.5.9 Place a collection vessel in the balance. Place the evaporation trap over the
vessel to reduce the effects of evaporation on the sampling process. Empty the
vessel as required during the calibration process.
Note: When dispensing larger volumes (e.g. 10 ml) a larger collection vessel is
necessary and must be used without the evaporation trap.
11.5.10 Determine the volumes of the pipette to be calibrated and set the pipette to the
highest volume first.
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11.5.11 Tare the balance, aspirate the appropriate volume of test water, and dispense
into the collection vessel.
11.5.12 Allow the balance to stabilize; the weight may be transferred to the calibration
software via RS-232 connection or the Pipette Wedge Software. The software
will complete the necessary density corrected value in µl.
11.5.12.1 The Pipette Calibration program will multiply the mass reading by 1µl /
density of water (as in Section 17.0) and store the corrected reading.
11.5.13 Repeat 11.5.10 and 11.5.11 for the required number of replicates.
11.5.14 Reset the pipette to the next required setting and repeat 11.5.10 through
11.5.11.
11.5.15 Repeat for any additional settings.
11.5.16 The following are the Accuracy and Precision Calculations performed within the
Pipette Calibration program:
11.5.16.1 The program calculates the accuracy for each pipette setting by taking
the mean volume (average) of the five calculated “As Found” readings
minus the set volume and divide by the set volume.
11.5.16.2 The Percent Accuracy = ((mean volume-set volume)/set volume) * 100
11.5.16.3 The program calculates the precision for each pipette setting using the
following formula:
11.5.16.4 The Percent Precision = (Standard Deviation / MV) x 100
11.5.16.5 Where: MV= mean volume.
11.5.17 Proceed to section 12.0 to complete testing.
11.6 “As Found” Pipette Condition Determination for 19 µLiter and Below Pipette
Calibration:
11.6.1 When ambient RH cannot be controlled or maintained at acceptable levels
(<45% RH), the affect of evaporation may need to be determined for volumes of
19 µL and below. When performing calibrations in the ranges above 19 µLiter,
the evaporation rate of the distilled water becomes a negligible variable (0.010
to 0.025 mg per weighing cycle) and doesn’t need to be calculated. When the
RH can be maintained, follow Section 11.5 for 1 µLiter to 19 µLiter volumetric As
Found calibrations.
11.6.2 Perform the Set-up and As Found instructions for 20 µLiter to 1,000 µLiter
pipettes with the additional steps below:
11.6.3 Draw a sample of purified water, tare the balance, then dispense the volume
into the collection vessel.
11.6.4 Allow the balance to stabilize, and then record the density corrected reading.
11.6.5 Estimate the amount of time required to perform a dispense cycle (From actual
pipette dispense through stabilization, to recording a reading), by observing a
few typical pipette dispense cycles.
11.6.6 Tare the balance, wait the time estimated above and record the reading from
0.00 µliter to -0.10 µliter in absolute terms; this value is the Nominal
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Evaporation Rate and should be added (as needed) to each sample reading
taken.
11.6.7 Perform the remaining steps in 11.5.
11.6.8 Proceed to section 12.0 to complete the testing.
11.7 Changes to collected data:
11.7.1 When obtaining As Found Data, results may be discounted and retested only
with an acceptable reason. Examples of acceptable reasons include: a loose tip,
excess liquid transfer from the exterior of the pipette, or another issue that
affects the validity of the test.
11.7.2 When a data point is deleted, the pipette software will require a reason be
entered prior to continuing testing. Enter the reason in the Pipette Audit form
and correct any issues before proceeding.
11.7.3 The software will retain a record of these changes and the documented reason
for the change.
11.8 Precision Syringes follow the same procedures as stated in pipette calibration
section.
11.9 Burette Calibration Instructions:
11.9.1 The procedure used for Burette testing is taken verbatim from ISO 8655-6, as
amended for OEM configurations.
11.9.2 An apparatus that is routinely dismantled and reassembled within the scope of
its intended use (e.g. for cleaning purposes) shall be dismantled and
reassembled at least once prior to the test in accordance with the supplier's
operation manual.
11.9.3 The apparatus shall be operated as specified in the supplier's operation manual.
11.9.4 Metrohm Addendum: the tips used, and configuration setup will be as specified
by Metrohm to reduce variance in testing methods due to setup. See figure 11-
3.
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Figure 11-3; note the tip location in relationship to the burette liquid
volume.
11.9.5 Test volume: In the case of a fixed-volume apparatus, the test volume is the
nominal volume. In the case of a variable-volume apparatus, at least three
volumes shall be tested:
11.9.5.1 The nominal volume, approximately 50% of the nominal volume, the
lower limit of the useful volume range or 10% of the nominal volume
(whichever is the greater).
11.9.6 Measurement of further volumes is optional. The setting devices of the
apparatus (e.g. dials, scales) shall be sufficient for the selection of the test
volume. Testing tolerances are per OEM designated test limits.
11.9.7 Test room: The test shall be carried out in a draught-free room with a stable
environment. The test room shall have a relative humidity above 50% and a
constant temperature between 15 °C and 30 °C.
11.9.8 Preparation: Carry out the testing by delivery into the weighing vessel. Carefully
clean the weighing vessel and add a small quantity of test liquid to it. Place the
weighing vessel and its test liquid in the balance case. Then place the burette
under test, with its reservoir already filled with test liquid, as close to the
balance as possible. Allow both to come to equilibrium for at least 2 hours.
11.9.9 See Section 18.0 for corrections to be made when the balance readings are
converted to volumes.
11.9.10 Evaporation: For small volumes below 50 µLiter errors due to evaporation of the
test liquid during weighing shall be taken into consideration. The error due to
evaporation during the measuring series can be determined experimentally and
compensated mathematically.
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11.9.11 Test cycle time: The test cycle time (time required to complete the weighing of
one dispensed volume) shall be kept to a minimum. It should ideally not exceed
60 seconds. It is important that it is regular, both within each cycle and as far as
possible from cycle to cycle, so that a reliable mathematical compensation of
the error due to evaporation during the measuring series can be applied.
11.9.12 Test procedure: Measure the mass of the weighing vessel and its test liquid and
consider this value as the tare mass prior to the first measurement. Load the
piston burette bubble free, with test liquid from the reservoir, in accordance
with the supplier's instructions. Deliver the test liquid from the burette into the
weighing vessel, until the selected volume is reached. If the burette is
automatically controlled, deliver test liquid until the volume preset is reached
and no further delivery occurs. Weigh the weighing vessel again and calculate
the mass of liquid delivered.
11.9.13 When testing partial volumes of the nominal volume of the piston burette, the
piston need not be reset to the initial position (zero) prior to the next
measurement. Ensure that the upper volume limit of the piston and thus the
nominal volume of the piston burette is not exceeded when dispensing a partial
volume.
11.9.14 When testing piston burettes — especially in the case of automated tests —
wiping of the delivery jet on the vessel wall to remove droplets can be
impossible due to the individual test setup. In such cases, ascertain that the
weighing is carried out only after a complete drop has been delivered from the
delivery jet into the weighing vessel. The test liquid can, for example, be
expelled through an extended tip in such a way that the stream breaks and no
drops form.
11.9.15 At the start and at the end of the weighing procedure, the temperature of the
test liquid in its container shall be recorded to within the nearest 0.2 °C.
11.9.16 Proceed to section 12.0 to complete the unit under test.
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11.10 Speed•Cal™ MPC V92 General Operation:
11.10.1 Speed•Cal™ is a stationary multichannel pipette calibration system that can
calibrate up to 12 channels at one time.
11.10.2 Activate the Pipette Calibration and Speed•Cal™ MPC V92 Software.
Note: When selecting options within the Speed•Cal™ MPC V92, word(s)
bracketed in this manner, <Example> are found as click ‘buttons’ or tabs in
the applicable Speed•Cal™ MPC V92 Software menu screen.
Keyboard entries are identified as *Example*
11.10.3 Speed•Cal™ MPC V92 Software; <Start> Tab:
11.10.4 Select <Username> from the drop-down menu. Type in *password* and press
*Enter*.
11.10.5 Click <Connect> and <Communications Test> Buttons. All 12 red LED indicators
on the Speed•Cal™ MPC should activate.
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11.10.6 Speed•Cal™ MPC V92 Software; “Environment” Tab:
11.10.6.1 Click <Confirm>.
Note: Actual temperature, humidity, and atmospheric data are to be
entered into the Pipette Calibration program.
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11.10.7 Speed•Cal™ MPC Preventative Maintenance Check; <Machine> Tab:
11.10.7.1 Aspirate the Speed•Cal™ MPC measurement vessels using the water
removal tool and vacuum pump assembly.
11.10.7.2 Click <Empty>. The blue water level indicator should clear and
characters should populate the Answer and Value columns.
11.10.7.3 Click <Tare> to zero out Speed•Cal™ MPC.
11.10.8 Speed•Cal™ MPC measurement vessels should be checked / drained nightly and
at workday startup.
11.10.9 Once stable, click <Intern. Just> radio button.
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11.10.10 Single Channel Pipette on Speed•Cal™ MPC V92:
11.10.10.1 Initial Set-up: <Configuration-Tested Item> Tab
11.10.10.2 Refer to Section 8.0 or the customer specifications to determine the
appropriate test plan.
11.10.10.3 Click on <Read Config V90> (1); then navigate to the applicable test
plan: Program files/Speed•Cal/SPCAL/Templates.
(1)
11.10.10.4 Speed•Cal™ MPC V92; <Single Channel> Tab: Select the appropriate
Radio Button for the desired test volume (4), and set the pipette
accordingly.
11.10.10.5 Click <Start> (3). The first channel on the Speed•Cal™ will illuminate.
11.10.10.6 Dispense a sample volume into the lit channel.
11.10.10.7 Press the <Spacebar> or click <Continue>. Repeat these steps until the
range is complete. Go to the next page.
11.10.10.8 Select next test volume (4) and set pipette volume accordingly. Repeat
until complete.
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(4)
(3)
11.10.10.9 The level indicator will slowly climb as the water level increases inside
the flask.
11.10.10.10 Empty the unit when the water level indicates approximately ¾ full by
going back to the <Machine> tab, aspirating the water, and then clicking
<Empty>.
11.10.10.11 This process cannot be performed while a test is in progress, but can be
completed between test volumes.
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11.10.10.12 Speed•Cal™ MPC V92 Software; <Excel> Tab (calibration completion):
11.10.10.13 Select <Measurement Result Single Channel> (5).
11.10.10.14 Click <Transfer to Excel> (6): Clear any error dialogs that may appear
within Excel.
11.10.10.15 Wait until <Transfer Status and Progress> Status Indicator (7) indicates
‘Finished’.
11.10.10.16 Open the Field Pipette Calibration program.
(6)
(5)
(7)
Note: this screen appears
after each volume of
pipette test plan.
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11.10.10.17 Pipette Calibration Program Import:
11.10.10.18 Select <Open Pipette Form>
11.10.10.19 Select the <Conditions> tab and enter in the relevant information
(temperature, humidity, atmospheric data and job number)
11.10.10.20 Click the <Instruments> tab and enter in the equipment information.
11.10.10.21 Click the <Readings> tab and select <Import AF Speed•Cal™>.
11.10.10.22 If no adjustments are to be made, click <Copy AF to AL>.
11.10.11 Multichannel Pipette Calibration on Speed•Cal™ MPC:
11.10.11.1 All steps identical to Section 11.10.10, except for the following:
11.10.11.2 Speed•Cal™ MPC V92 Software; <Tested Item> Tab (13):
11.10.11.3 Click on <Read Config V90> Radio Button (14).
(13)
(14)
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11.10.11.4 Select a Multichannel Pipette Test Plan, from Configuration file folders;
Select Pipette Test Plan
11.10.11.5 Under the Speed•Cal™ MPC V92 Software; <Multi-Channel> Tab;
11.10.11.6 Select the appropriate <Test Volume µl> Radio Button for the desired
test volume, and set the pipette accordingly.
11.10.11.7 Click <New Measurement Start>. Channel LEDs will illuminate when
ready for testing. Dispense the sample volume into the lit channel.
11.10.11.8 Press the Spacebar or click <Continue> radio button. LEDs will
extinguish while measurement is taking place.
11.10.11.9 DO not touch the channel vessels until the LEDs re-illuminate.
11.10.11.10 Repeat until the range is complete.
11.10.11.11 Select the next sample volume and set the pipette accordingly. Repeat
until the measurement test plan is completed. Repeat prior steps until
all sample volumes have been dispensed and measured.
11.10.11.12 The level indicator will slowly climb as water level increases inside the
flask. Empty the unit when the water level indicates approximately ¾
full by going back to the <Machine> tab, aspirating the water and then
clicking the <Empty>. This process cannot be performed while a test is
in progress, but can be completed between test volumes.
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11.10.11.13 Speed•Cal™ MPC V92 (Normal Status Windows during Testing);
Screen appears between each
multichannel pipette.
To check overview, click here.
11.10.11.14 The screen below appears after each volume of Pipette Test Plan.
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11.10.11.15 Speed•Cal™ MPC V92 Software; <Excel> Tab:
11.10.11.16 Select <Measurement Result Multichannel>.
11.10.11.17 Press <Transfer to Excel> Radio Button. Clear any error dialogs that may
appear within Excel.
11.10.11.18 When the <Transfer Status and Progress> status window indicates
‘Finished’, switch to Pipette Dispatch Database Switchboard.
11.10.11.19 Speed•Cal™ MPC V92 (Normal Status Windows after Testing);
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11.10.11.20 Status Dialog that appears during transfer to excel:
11.10.11.21 Refer to Section 11.10.10.17 to import data to Pipette Calibration
program.
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11.10.12 Documenting Measurements After Adjustment (Single or Multichannel):
11.10.12.1 Perform all tasks in an identical manner to 11.10.11.10 and 11.10.11.11,
but Do not “Copy As-Found Data to As-Left”:
11.10.12.2 Under Speed•Cal™ /<Single Channel> or <Multi Channel> tab, record
adjustments in accordance with the OEM or Client work instructions.
Several ranges can be measured in succession until the unit is within
tolerance.
11.10.12.3 When adjustment is complete and the As Left data has been collected in
the Speed•Cal™ MPC V92, open the <Excel> tab, select the proper radio
button, and transfer the data to Excel.
11.10.12.4 In the Pipette Calibration program press “Import l As-Left Data”.
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11.11 Mobile Speedcal M12 Operation:
11.11.1 Speedcal Mobile M12 is a multichannel pipette calibration system that can
calibrate up to 12 channels at one time.
11.11.2 Assemble the unit according the Speedcal Mobile Operating Instructions. The
unit should not be moved unless the cover is in place, restricting the movement
of the load cells. Make sure that your laptop is connected to the balance with
an Ethernet cord.
11.11.3 Follow the instructions in Section 11.4 for selecting a suitable location for the
unit and performance of the balance verification. The unit must be leveled
using the leveling feet and indicator on the unit.
11.11.4 Open the Pipette Software, the Pipette Wedge, and the Speedcal Mobile
software on the laptop.
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11.11.5 On the Pipette Wedge Screen, select SpeedCal Mobile as the Balance. If the IP
Address is required, use the IP address given on the Sartorius SpeedCal Mobile
home page.
11.11.6 Click on the Set Com Parameters button.
11.11.7 The Pipette Wedge will shorten to the screen below that can be used to tare
the balance and shows the fill level of the load cells.
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11.11.8 The Speedcal Mobile Screen shows the current reading for each channel of the
mobile speedcal. It can also be used to tare the balance and shows the fill level
of the load cells.
11.11.9 Calibrate the pipettes as describe in Sections 11.5 and 11.6, pressing F3 to
transfer the readings from the mobile speedcal into the Pipette Software.
11.11.10 Empty the measurement channels using a suction device and instructions
provided with the mobile speedcal.
11.11.11 Switch off the device and disassemble according to the Speedcal Mobile
operating instructions prior to transporting.
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12.0 ‘As Found’ Condition Determination:
12.1 Compare the noted deviations from the ‘As Found’ test data taken to the UUT tolerance
specifications.
12.2 Depending on the As-found condition, the UUT may need to be repaired, optimized or
adjusted before collecting the ‘as-left data’.
12.3 Refer to ISO-QSP-2010 General Field Service and Calibration Practices for additional
specific procedural instructions.
13.0 Calibration Adjustment:
13.1 All as found readings must be taken prior to beginning adjustment. Where a pipette or
measurement channel is inoperative, the comments should indicate that no as found
measurements could be taken, as applicable.
13.2 All calibration adjustments are to be completed as per manufacturer’s
instructions/documentation.
13.3 Document in the comments section of the ‘Calibration Data Report’ any adjustments
that were made to the UUT.
14.0 ‘As Left’ Condition / Submittal:
14.1 Confirm all imported data from Speed•Cal™ MPC V92 software before data submittal.
14.2 Enter all appropriate data in the Pipette Calibration software and review all data to
verify the report is correct.
14.3 Certify the pdf document is complete and true by affixing your e-signature.
14.4 Remove any old calibration labels and replace with the appropriate new label.
14.5 Complete all documentation and review prior to submittal to customer.
15.0 End of procedure
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16.0 Balance Suitability Testing (Optional):
16.1 The USP requires that all balances required to accurately weigh be tested to verify
the balance is suitable for its intended use. In a GXP environment, this requirement
includes any balances used for pipette calibrations. Company owned balances have
had system suitability tests performed, with the results on file with Quality
Assurance.
16.2 USP suitability testing is accomplished by determining the minimum mass the UUT
can measure with a measurement uncertainty of ± 0.01% of the reading. The
balance is then suitable for use within its determined operational range.
16.3 Refer to Balance and Load Indicator Calibration Protocol: ISO-SOP-3007, for testing
methodology.
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17.0 Addendum: Reference Water Density Conversion Table
3
The Values listed below are calculated from the reference values of Annex A, ISO8655-6 (2009)
and ISO/TR 20461 (2000) for determination of Volume from Balance mass readings. The Table in
Annex A (see §23.0) is presented as micro liters per milligram, this table is presented as a
correction factor [mass (mg) ∗ CF = Volume (µL)]
Additional values may be obtained by referencing Annex A (For Temperatures to 30°C, or using
the formula (3) in ISO/TR20461, valid from 5 °C to 40 °C.
Water Water Water
Temperature Density Temperature Density Temperature Density
15.0 0.999129 18.0 0.998625 21.0 0.998022
15.1 0.999113 18.1 0.998606 21.1 0.998000
15.2 0.999098 18.2 0.998588 21.2 0.997979
15.3 0.999083 18.3 0.998569 21.3 0.997957
15.4 0.999067 18.4 0.998550 21.4 0.997935
15.5 0.999052 18.5 0.998531 21.5 0.997913
15.6 0.999036 18.6 0.998512 21.6 0.997890
15.7 0.999020 18.7 0.998493 21.7 0.997868
15.8 0.999004 18.8 0.998474 21.8 0.997845
15.9 0.998988 18.9 0.998454 21.9 0.997823
16.0 0.998972 19.0 0.998435 22.0 0.997800
16.1 0.998956 19.1 0.998415 22.1 0.997778
16.2 0.998939 19.2 0.998395 22.2 0.997755
16.3 0.998923 19.3 0.998375 22.3 0.997732
16.4 0.998906 19.4 0.998356 22.4 0.997709
16.5 0.998889 19.5 0.998335 22.5 0.997686
16.6 0.998873 19.6 0.998315 22.6 0.997662
16.7 0.998856 19.7 0.998295 22.7 0.997639
16.8 0.998839 19.8 0.998275 22.8 0.997616
16.9 0.998821 19.9 0.998254 22.9 0.997592
17.0 0.998804 20.0 0.998234 23.0 0.997568
17.1 0.998787 20.1 0.998213 23.1 0.997545
17.2 0.998769 20.2 0.998192 23.2 0.997521
17.3 0.998751 20.3 0.998171 23.3 0.997497
17.4 0.998734 20.4 0.998150 23.4 0.997473
17.5 0.998716 20.5 0.998129 23.5 0.997449
17.6 0.998698 20.6 0.998108 23.6 0.997425
17.7 0.998680 20.7 0.998087 23.7 0.997400
17.8 0.998662 20.8 0.998065 23.8 0.997376
17.9 0.998643 20.9 0.998044 23.9 0.997351
3 Validated Reference: Handbook of Hydrology, Chapter 11.3 Water Quality (S.C. McCutcheon, J.L. Martin, & T.O. Barnwell) with Water Density
formula referenced to ISO/TR 20461:2000.
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18.0 Addendum: Reference Z factors:
(Calculation of Volume from Balance gram readings)
Values for correction factors are given below extracted from Annex A - ISO8655-6 (2009), table
A.1. Correction factors may also be calculated from equation (3) in ISO/TR 20461:2000
Z values in micro liters per gram
Temperature Air Pressure (kPa)
(°C) 80 85 90 100 101.3 105
15.0 1001,7 1001,8 1001,9 1002,0 1002,0 1002,0
15.5 1001,8 1001,9 1001,9 1002,0 1002,0 1002,1
16.0 1001,9 1002,0 1002,0 1002,1 1002,1 1002,2
16.5 1002,0 1002,0 1002,1 1002,2 1002,2 1002,2
17.0 1002,1 1002,1 1002,2 1002,3 1002,3 1002,3
17.5 1002,2 1002,2 1002,3 1002,4 1002,4 1002,4
18.0 1002,2 1002,3 1002,3 1002,4 1002,5 1002,5
18.5 1002,3 1002,4 1002,4 1002,5 1002,6 1002,6
19.0 1002,4 1002,5 1002,5 1002,6 1002,7 1002,7
19.5 1002,5 1002,6 1002,6 1002,7 1002,8 1002,8
20.0 1002,6 1002,7 1002,7 1002,8 1002,8 1002,9
20.5 1002,7 1002,8 1002,8 1002,9 1002,9 1003,0
21.0 1002,8 1002,9 1002,9 1003,1 1003,1 1003,1
21.5 1003,0 1003,0 1003,1 1003,1 1003,2 1003,2
22.0 1003,1 1003,1 1003,2 1003,3 1003,3 1003,3
22.5 1003,2 1003,2 1003,3 1003,4 1003,4 1003,4
23.0 1003,3 1003,3 1003,4 1003,5 1003,5 1003,6
23.5 1003,4 1003,5 1003,5 1003,6 1003,6 1003,7
24.0 1003,5 1003,6 1003,6 1003,7 1003,8 1003,8
24.5 1003,7 1003,7 1003,8 1003,9 1003,9 1003,9
25.0 1003,8 1003,8 1003,9 1004,0 1004,0 1004,0
25.5 1003,9 1004,0 1004,0 1004,1 1004,1 1004,2
26.0 1004,0 1004,1 1004,1 1004,2 1004,3 1004,3
26.5 1004,2 1004,2 1004,3 1004,4 1004,4 1004,4
27.0 1004,3 1004,4 1004,4 1004,5 1004,5 1004,6
27.5 1004,5 1004,5 1004,6 1004,7 1004,7 1004,7
28.0 1004,6 1004,6 1004,7 1004,8 1004,8 1004,8
28.5 1004,7 1004,8 1004,8 1004,9 1005,0 1005,0
29.0 1004,9 1004,9 1005,0 1005,1 1005,1 1005,1
29.5 1005,0 1005,1 1005,1 1005,2 1005,2 1005,3
30.0 1005,2 1005,2 1005,3 1005,4 1005,4 1005,4
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