ASTM D4298-22

Standard Guide for Intercomparing Permeation Tubes to Establish Traceability

SIGNIFICANCE AND USE
5.1 The accuracy of air pollution measurements is directly dependent upon accurate calibrations.  
5.2 Such measurements gain accuracy and can be intercompared when the measurement procedures are traceable to national measurement standards.  
5.3 This guide describes procedures for enhancing the accuracy of air pollution measurements which may be specified by those organizations requiring traceability to national standards.
SCOPE
1.1 This guide covers two procedures for establishing the permeation rate of a permeation tube and defining the uncertainty of the rate by comparison to National Institute of Standards and Technology's Standard Reference Materials (SRM).  
1.2 Procedure A consists of a direct comparison of the permeation rate of the device undergoing calibration with that of an SRM.  
1.3 Procedure B consists of a gravimetric calibration process in which a certified permeation tube is used as a quality control for the measurements.  
1.4 Both procedures are limited to the case where a suitable certified permeation device is available.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. (See 8.2 on Safety Precautions.)  
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Aug-2022
• ICS: 17.020 - Metrology and measurement in general
• Technical Committee: D22 - Air Quality
• Drafting Committee: D22.01 - Quality Control

Relations

• Refers: ASTM E617-23 - Standard Specification for Laboratory Weights and Precision Mass Standards
• Effective Date: 15-Aug-2023
• Refers: ASTM D1356-20a - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-Sep-2020
• Refers: ASTM D1356-20 - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 15-Mar-2020
• Refers: ASTM D3249-95(2019) - Standard Practice for General Ambient Air Analyzer Procedures
• Effective Date: 01-Oct-2019
• Refers: ASTM E617-18 - Standard Specification for Laboratory Weights and Precision Mass Standards
• Effective Date: 01-Oct-2018
• Refers: ASTM D3631-99(2017) - Standard Test Methods for Measuring Surface Atmospheric Pressure
• Effective Date: 01-Mar-2017
• Refers: ASTM D1356-15a - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 15-Oct-2015
• Refers: ASTM D1356-15 - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-Jul-2015
• Refers: ASTM D1356-14b - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-Dec-2014
• Refers: ASTM D1356-14a - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-May-2014
• Refers: ASTM D1356-14 - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 15-Jan-2014
• Refers: ASTM E1-13 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-May-2013
• Refers: ASTM D3631-99(2011) - Standard Test Methods for Measuring Surface Atmospheric Pressure
• Effective Date: 01-Oct-2011
• Refers: ASTM D3249-95(2011) - Standard Practice for General Ambient Air Analyzer Procedures
• Effective Date: 01-Oct-2011
• Refers: ASTM E2251-11 - Standard Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids
• Effective Date: 01-May-2011

Overview

ASTM D4298-22: Standard Guide for Intercomparing Permeation Tubes to Establish Traceability is a key ASTM International standard focused on ensuring the accuracy and traceability of air pollution measurements through proper calibration of permeation tubes. This guide details two accepted procedures for establishing the permeation rate of a permeation tube and defining its uncertainty, using comparison with National Institute of Standards and Technology (NIST) Standard Reference Materials (SRM) or certified reference materials (CRM). Traceable calibration and intercomparison are essential for organizations that must comply with regulatory requirements and demand reliable environmental data.

Key Topics

• Traceability and Calibration: Describes the importance of ensuring measurement results are traceable to recognized national standards, which supports data comparability and regulatory compliance.
• Procedures for Intercomparison:
  • Procedure A (Direct Comparison): Involves direct comparison of the device under calibration with a certified SRM under controlled conditions.
  • Procedure B (Gravimetric Process): Utilizes gravimetric calibration where mass loss over time is measured, and a certified permeation tube is used as quality control.
• Measurement Uncertainty: The guide provides methods to define and express measurement uncertainty, essential for demonstrating the reliability of results.
• Use of Certified Reference Materials: Emphasizes availability and use of CRMs or SRMs as benchmarks to improve calibration confidence.
• Environmental and Safety Guidelines: Highlights the need to establish appropriate safety, health, and environmental practices during the calibration and measurement process.
• SI Units Compliance: All measurements and reported values are specified in SI units, ensuring consistency in international applications.

Applications

ASTM D4298-22 is particularly relevant to:

• Air Quality Laboratories: For calibration and standardization of equipment used to measure air pollution concentrations.
• Regulatory Agencies and Environmental Compliance: Ensures that measurement data are accurate and traceable, meeting legal and policy requirements for air monitoring.
• Calibration Service Providers: Provides a framework for intercomparing permeation tubes using recognized procedures, supporting reliable reference standards.
• Instrument Manufacturers: Assists in quality control and certification processes for permeation tube-based gas generators or analyzers.
• Research Institutions: Offers guidance for studies that require high-confidence measurement of trace gases or pollutants.

The procedures outlined in this standard support the establishment of a robust quality assurance program for air monitoring, critical in validating environmental measurement systems and providing defensible data for public health protection.

Related Standards

For enhanced calibration and traceability in environmental monitoring, the following ASTM standards are commonly referenced with ASTM D4298-22:

• ASTM D1356 - Terminology Relating to Sampling and Analysis of Atmospheres
• ASTM D3249 - Practice for General Ambient Air Analyzer Procedures
• ASTM D3609 - Practice for Calibration Techniques Using Permeation Tubes
• ASTM D3631 - Test Methods for Measuring Surface Atmospheric Pressure
• ASTM E1/E2251 - Specifications for Liquid-in-Glass Thermometers
• ASTM E617 - Specification for Laboratory Weights and Precision Mass Standards

By following these standards together, organizations can build a comprehensive, traceable calibration program for consistent and reliable air pollution measurement.

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Keywords: permeation tube calibration, traceability, air pollution measurement, intercomparing permeation tubes, ASTM standards, certified reference material, NIST SRM, measurement uncertainty, environmental monitoring, calibration procedures.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4298 − 22
Standard Guide for
Intercomparing Permeation Tubes to Establish Traceability
This standard is issued under the fixed designation D4298; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D3249Practice for General Ambient Air Analyzer Proce-
dures
1.1 This guide covers two procedures for establishing the
D3609Practice for Calibration Techniques Using Perme-
permeation rate of a permeation tube and defining the uncer-
ation Tubes
tainty of the rate by comparison to National Institute of
D3631Test Methods for Measuring Surface Atmospheric
Standards and Technology’s Standard Reference Materials
Pressure
(SRM).
E1Specification for ASTM Liquid-in-Glass Thermometers
1.2 Procedure A consists of a direct comparison of the
E319Practice for the Evaluation of Single-Pan Mechanical
permeation rate of the device undergoing calibration with that 3
Balances (Withdrawn 2021)
of an SRM.
E617Specification for Laboratory Weights and Precision
1.3 Procedure B consists of a gravimetric calibration pro- Mass Standards
E2251Specification for Liquid-in-Glass ASTM Thermom-
cess in which a certified permeation tube is used as a quality
control for the measurements. eters with Low-Hazard Precision Liquids
1.4 Both procedures are limited to the case where a suitable
3. Terminology
certified permeation device is available.
3.1 Definitions:
1.5 The values stated in SI units are to be regarded as
3.1.1 For definitions of terms used in this guide, refer to
standard. No other units of measurement are included in this
Terminology D1356.
standard.
3.2 Definitions of Terms Specific to This Standard:
1.6 This standard does not purport to address all of the 3.2.1 working standard—a standard used in the laboratory
or field for periodic standardization of a measuring instrument.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Guide
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 4.1 Procedure A—A certified SRM permeation source, ob-
(See 8.2 on Safety Precautions.) tainedfromtheNationalInstituteofStandardsandTechnology
1.7 This international standard was developed in accor- is used to calibrate a continuous analyzer. The analyzer is then
dance with internationally recognized principles on standard- used to measure the concentration of a gaseous mixture
ization established in the Decision on Principles for the generated from the permeation tube under calibration. Equa-
Development of International Standards, Guides and Recom- tionsareprovidedthatpermitcalibrationofthepermeationrate
mendations issued by the World Trade Organization Technical of the latter from the test data.
Barriers to Trade (TBT) Committee.
4.2 Procedure B—The permeation source is calibrated,
gravimetrically, using temperature and mass standards trace-
2. Referenced Documents
able to the United States National Institute of Standards and
2.1 ASTM Standards:
Technology (NIST), or other national or international standard
D1356Terminology Relating to Sampling and Analysis of
reference. The validity of the calibration is confirmed by
Atmospheres
concurrently measuring the permeation rate of a certified
reference material (CRM).
This guide is under the jurisdiction of ASTM Committee D22 on Air Quality
and is the direct responsibility of Subcommittee D22.01 on Quality Control.
5. Significance and Use
Current edition approved Sept. 1, 2022. Published September 2022. Originally
ɛ1
5.1 The accuracy of air pollution measurements is directly
approved in 1983. Last previous edition approved in 2014 as D4298–04 (2014) .
DOI: 10.1520/D4298-22.
dependent upon accurate calibrations.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4298 − 22
5.2 Such measurements gain accuracy and can be intercom- 8.1.1 The procedural precautions described in Practice
pared when the measurement procedures are traceable to D3609 are applicable to this guide.
national measurement standards.
8.1.2 When possible, the permeation device should be
compared to the CRM using the same system with identical
5.3 This guide describes procedures for enhancing the
flow and temperature conditions. Unpredictable errors may be
accuracyofairpollutionmeasurementswhichmaybespecified
introduced if permeation devices are compared at widely
by those organizations requiring traceability to national stan-
differenttemperaturesandflowrates(pertainstoProcedureA).
dards.
Intercomparisons are valid only at temperatures for which the
CRM tube is calibrated.
6. Apparatus
8.1.3 Equilibration of the permeation device, the calibration
6.1 For apparatus used in the calibration of permeation
equipment, and the analytical system must be quality assured,
devices, refer to Practice D3609.
prior to use. During storage, avoid exposing tubes to high
6.1.1 The thermometers used shall conform to Specification
humidity or wide variations in temperature that may perma-
E1 or Specification E2251 and shall have calibration certifi-
nently alter the permeation rate.
cates traceable to the NIST. Measurement uncertainty should
be 0.1°C or less. 8.2 Safety Precautions:
6.1.2 Barometer—An aneroid or other barometer capable of
8.2.1 For precautions concerning the use of analytical in-
measuring atmospheric pressure to within 6300Pa (25mm struments and of cylinders containing pressurized gases, see
Hg) shall be used. Calibrate the barometer as described inTest
Practice D3249.
Methods D3631.
9. Calibration and Standardization
6.2 Apparatus for Procedure A:
6.2.1 Analytical Instruments—An analytical instrument re-
9.1 Procedure A:
sponsive to the permeant with the following minimum perfor-
9.1.1 Set up a gas generation system using a certified
mance specifications:
reference material (CRM) permeation tube and apparatus and
Noise 1 % of full-scale procedure such as described in Practice D3609. Equilibrate at
Zero drift ±4 % of full-scale per day
the desired temperature of calibration.
Span drift ±3 % of full-scale per day
9.1.2 Optimize the performance of the analytical instrument
Range 0 ppm to 0.5 ppm (or appropriate for source strength)
according to the manufacturer’s instructions.
6.2.2 Continuous strip chart recorder with the following
9.1.3 Using dry air or nitrogen, set the zero point of the
minimum performance specifications:
instrument.
Uncertainty 0.33 × (0.25 % full-scale
9.1.4 Use the gas generation system to provide gas concen-
component deflection)
Chart width no less than 6 in.
trations corresponding to 20%, 40%, 60%, and 80% of
Time for full-scale travel 1 s
full-scale readings. Record the concentration and respective
NOTE 1—ISO JCGM 100:2008 points out that with approximately
readings. Repeat the measurements in random order.
normal plotted points, the above maximum 3 × standard deviations is
9.1.5 Plot concentration versus instrument readings and
equivalent to >99% of plotted points lying within 6 (0.25% full-scale
draw the line of best fit, or alternatively fit by linear least
deflection) of true values.
squares regression. Calculate the slope (ppm(v)/scale reading)
6.3 Apparatus for Procedure B:
and standard deviation estimate s , expressed as µg/min.
cal
6.3.1 Analytical balance, meeting the requirements of Prac-
9.1.5.1 If any point de
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D4298 − 04 (Reapproved 2014) D4298 − 22
Standard Guide for
Intercomparing Permeation Tubes to Establish Traceability
This standard is issued under the fixed designation D4298; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorial corrections were made throughout in December 2014.
1. Scope
1.1 This guide covers two procedures for establishing the permeation rate of a permeation tube and defining the uncertainty of the
rate by comparison to National Institute of Standards and Technology’s Standard Reference Materials (SRM).
1.2 Procedure A consists of a direct comparison of the permeation rate of the device undergoing calibration with that of an SRM.
1.3 Procedure B consists of a gravimetric calibration process in which a certified permeation tube is used as a quality control for
the measurements.
1.4 Both procedures are limited to the case where a suitable certified permeation device is available.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. (See 8.2 on Safety Precautions.)
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
D3249 Practice for General Ambient Air Analyzer Procedures
D3609 Practice for Calibration Techniques Using Permeation Tubes
D3631 Test Methods for Measuring Surface Atmospheric Pressure
E1 Specification for ASTM Liquid-in-Glass Thermometers
E319 Practice for the Evaluation of Single-Pan Mechanical Balances (Withdrawn 2021)
E617 Specification for Laboratory Weights and Precision Mass Standards
This guide is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.01 on Quality Control.
Current edition approved Dec. 1, 2014Sept. 1, 2022. Published January 2015September 2022. Originally approved in 1983. Last previous edition approved in 20102014
ɛ1
as D4298 – 04 (2010).(2014) . DOI: 10.1520/D4298-04R14E01.10.1520/D4298-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4298 − 22
E2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this guide, refer to Terminology D1356.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 working standard—a standard used in the laboratory or field for periodic standardization of a measuring instrument.
4. Summary of Guide
4.1 Procedure A—A certified SRM permeation source, obtained from the National Institute of Standards and Technology is used
to calibrate a continuous analyzer. The analyzer is then used to measure the concentration of a gaseous mixture generated from
the permeation tube under calibration. Equations are provided that permit calibration of the permeation rate of the latter from the
test data.
4.2 Procedure B—The permeation source is calibrated, gravimetrically, using temperature and mass standards traceable to NIST
standards. the United States National Institute of Standards and Technology (NIST), or other national or international standard
reference. The validity of the calibration is confirmed by concurrently measuring the permeation rate of a Certified Reference
Materialcertified reference material (CRM).
5. Significance and Use
5.1 The accuracy of air pollution measurements is directly dependent upon accurate calibrations.
5.2 Such measurements gain accuracy and can be intercompared when the measurement procedures are traceable to national
measurement standards.
5.3 This guide describes procedures for enhancing the accuracy of air pollution measurements which may be specified by those
organizations requiring traceability to national standards.
6. Apparatus
6.1 For apparatus used in the calibration of permeation devices, refer to Practice D3609.
6.1.1 The thermometers used shall conform to Specification E1 or Specification E2251 and shall have calibration certificates
traceable to the NIST. Measurement uncertainty should be 0.1°C0.1 °C or less.
6.1.2 Barometer—The mercury barometer shall conform to An aneroid or other barometer capable of measuring atmospheric
pressure to within 6300 Pa (25 mm Hg) shall be used. Calibrate the barometer as described in Test Methods D3631.
6.2 Apparatus for Procedure A:
6.2.1 Analytical Instruments—An analytical instrument responsive to the permeant with the following minimum performance
specifications:
Noise 1 % of full-scale
Zero drift ±4 % of full-scale per day
Span drift ±3 % of full-scale per day
Range 0 to 0.5 ppm (or appropriate for source strength)
Range 0 ppm to 0.5 ppm (or appropriate for source strength)
6.2.2 Continuous strip chart recorder with the following minimum performance specifications:
D4298 − 22
Uncertainty 0.33 × (0.25 % full-scale
component deflection)
Chart width no less than 6 in.
Time for full-scale travel 1 s
NOTE 1—ISO GUMJCGM 100:2008 points out that with approximately normal plotted points, the above maximum 3 × standard deviations is equivalent
to >99 % of plotted points lying within 6 (0.25 % full-scale deflection) of true values.
6.3 Apparatus for Procedure B:
6.3.1 Analytical balance, meeting the requirements of Practices E319 and D3609.
6.3.2 Analytical weights meeting the requirements of Specification E617 and having a calibration certificate traceable to the
NIST.NIST or other national or international standard reference weights.
7. Materials
7.1 Refer to Practice D3609.
7.2 CRM Permeation Device.
8. Precautions
8.1 Procedural Precautions:
8.1.1 The procedural precautions described in Practice D3609 are applicable to the present this guide.
8.1.2 When possible, the permeation device should be compared to the CRM using the same system with identical flow and
temperature conditions. Unpredictable errors may be introduced if permeation devices are compared at widely different
temperatures and flow rates (pertains to Procedure A). Intercomparisons are valid only at temperatures for which the CRM tube
is calibrated.
8.1.3 Equilibration of the permeation device, the calibration equipment, and the analytical system must be quality assured, prior
to use. During storage, avoid exposing tubes to high humiditieshumidity or wide variations in temperature,temperature that may
permanently alter the permeation rate.
8.2 Safety Precautions:
8.2.1 For precautions concerning the use of analytical instruments and of cylinders containing pressurized gases, see Practice
D3249.
9. Calibration and Standardization
9.1 Procedure A:
9.1.1 Set up a gas generation system using a Certified Reference Materialcertified reference material (CRM) permeation tube and
apparatus and procedure such as described in Practice D3609. Equilibrate at the desired temperature of calibration.
9.1.2 Optimize the performance of the analytical instrument according to the manufacturer’s instructions.
9.1.3 Using dry air or nitrogen, set the zero point of the instrument.
ISO GUM,JCGM 100:2008, Guide to the Expression of Uncertainty in Measurement,GUM 1995 with minor corrections,
...