ASTM E2269-21

Standard Test Method for Determining Argon Concentration in Sealed Insulating Glass Units using Gas Chromatography

SIGNIFICANCE AND USE
4.1 This test method is intended to provide a means for determining the concentration of fill gases, typically argon, oxygen, and nitrogen gases in individual sealed insulating glass units, which were intended to be filled with a specific concentration of fill gases at the time of manufacture.  
4.2 The fill gases, oxygen and nitrogen, are physically separated by gas chromatography and compared to corresponding components separated under similar conditions from a reference standard mixture or mixtures of known composition. If the carrier gas is the same as the fill gas, then just the oxygen and nitrogen (air contaminate) are separated.  
4.3 The composition of the sample is calculated from the chromatogram by comparing the area under the curve of each component with the area under the curve of the corresponding component on the reference standard chromatogram.  
4.4 It is essential that the person or persons performing this test are very knowledgeable about the principles and techniques of gas chromatography, operation and calibration of gas chromatographs. More information can be found in Practice E355.  
4.5 It takes time for the fill gas to equilibrate in any insulating glass unit. This is particularly important in insulating glass units using a tubular spacer and in units containing interior components such as tubular muntin bars. Performing this test before a unit has equilibrated could result in fill gas concentrations that are measurably different than the actual fill gas concentration.  
4.6 This method may be used to determine the initial fill gas concentration achieved by the filling method, or the fill gas concentration in units that have been in service or that have been subjected to durability tests such as those described in Test Method E2188.  
4.7 This is a destructive test method in that the edge seal of the insulating glass unit is breached in order to obtain a gas sample for analysis by gas chromatography.
SCOPE
1.1 This test method covers procedures for using gas chromatographs to determine the concentration of argon gas in the space between the panes of sealed insulating glass.  
1.2 This test method is not applicable to insulating glass units containing open capillary/breather tubes.  
1.3 The values stated in inch-pound units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.  
1.5 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-Mar-2021
• ICS: 71.040.50 - Physicochemical methods of analysis
• ICS: 81.040.01 - Glass in general
• Technical Committee: E06 - Performance of Buildings
• Drafting Committee: E06.22 - Durability Performance of Building Constructions

Relations

• Refers: ASTM C162-23 - Standard Terminology of Glass and Glass Products
• Effective Date: 01-Oct-2023
• Refers: ASTM E2188-19 - Standard Test Method for Insulating Glass Unit Performance
• Effective Date: 01-Apr-2019
• Refers: ASTM C717-19 - Standard Terminology of Building Seals and Sealants
• Effective Date: 01-Mar-2019
• Refers: ASTM C717-18 - Standard Terminology of Building Seals and Sealants
• Effective Date: 01-Mar-2018
• Refers: ASTM C717-17a - Standard Terminology of Building Seals and Sealants
• Effective Date: 01-Nov-2017
• Refers: ASTM C717-17 - Standard Terminology of Building Seals and Sealants
• Effective Date: 01-Jan-2017
• Refers: ASTM C717-16a - Standard Terminology of Building Seals and Sealants
• Effective Date: 15-Nov-2016
• Refers: ASTM C717-16 - Standard Terminology of Building Seals and Sealants
• Effective Date: 01-Sep-2016
• Refers: ASTM C162-05(2015) - Standard Terminology of<brk type="line"/> Glass and Glass Products
• Effective Date: 01-Nov-2015
• Refers: ASTM E631-15 - Standard Terminology of Building Constructions
• Effective Date: 01-Mar-2015
• Refers: ASTM E631-14 - Standard Terminology of Building Constructions
• Effective Date: 01-Nov-2014
• Refers: ASTM C717-14a - Standard Terminology of Building Seals and Sealants
• Effective Date: 01-May-2014
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM C717-14 - Standard Terminology of Building Seals and Sealants
• Effective Date: 01-Feb-2014
• Refers: ASTM C717-13 - Standard Terminology of Building Seals and Sealants
• Effective Date: 01-Nov-2013

Overview

ASTM E2269-21 is the internationally recognized standard test method for determining the concentration of argon gas within sealed insulating glass (IG) units using gas chromatography. Developed by ASTM International, this standard provides a clear procedure for extracting and analyzing fill gas samples from IG units to quantify argon concentration, which is critical for assessing energy performance in buildings. The method separates argon, oxygen, and nitrogen gases for accurate measurement, supporting manufacturers, laboratories, and quality assurance processes in ensuring product performance.

Key Topics

• Gas Chromatography for IG Units: The method specifies procedures for using gas chromatographs to analyze the airspace between panes of sealed insulating glass units, focusing primarily on argon but applicable for oxygen and nitrogen separation as well.
• Sampling and Analysis: The process involves breaching the edge seal of the IG unit to extract a gas sample. Gas chromatography is then used to separate and quantify each gas component, comparing the sample chromatogram to reference standards of known composition.
• Destructive Testing: This is a destructive procedure since the seal must be breached to obtain a representative gas sample.
• Requirements for Skill: The standard stresses the importance of operator expertise in gas chromatography, including instrument calibration and result calculation.
• Equilibration: Fill gas distribution must be equilibrated within the IG unit before testing, as premature testing can lead to inaccurate results. This consideration is especially critical for units with tubular spacers or interior muntin bars.
• Fill Gas Importance: The measured argon concentration provides essential data for estimating the thermal and energy performance of insulating glass units.

Applications

• Quality Control in Manufacturing: AST E2269-21 is used by IG unit manufacturers to verify that specified argon concentrations are achieved during production, a key step in delivering high-performance glazing products for windows, doors, and facades.
• Durability and Performance Assessment: The method enables testing of IG units that have undergone durability evaluations, such as those exposed to weathering or subjected to accelerated aging tests, to assess the retention of argon over time.
• Research and Development: Laboratories utilize this test method in product development and for comparative studies of fill gas retention, unit design, and sealant efficacy.
• Building Energy Efficiency Verification: Accurate assessment of fill gas concentration supports compliance with energy codes and building certifications by confirming the insulating value of installed IG units.

Related Standards

• ASTM C162: Terminology of Glass and Glass Products - provides definitions used within this standard.
• ASTM C717: Terminology of Building Seals and Sealants - for understanding components of IG units.
• ASTM E177: Practice for Use of the Terms Precision and Bias in ASTM Test Methods.
• ASTM E355: Practice for Gas Chromatography Terms and Relationships - essential for proper instrument use and result calculation.
• ASTM E631: Terminology of Building Constructions.
• ASTM E691: Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method.
• ASTM E2188: Test Method for Insulating Glass Unit Performance - referenced for units subjected to durability tests.

Practical Value

Adhering to ASTM E2269-21 ensures that manufacturers, laboratories, and specifiers have a reliable and standardized approach to measure argon concentration in IG units. Accurate fill gas measurement supports compliance with building codes, helps predict long-term thermal performance, and enables quality control during manufacturing and after in-service use. Utilizing this method contributes significantly to the energy efficiency and durability of glazing products used in residential and commercial buildings.

Keywords: ASTM E2269-21, argon concentration, gas chromatography, sealed insulating glass units, IGU, insulating glass, fill gas, quality control, energy efficiency, thermal performance, gas sampling, building envelope standards.

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: E2269 − 21
Standard Test Method for
Determining Argon Concentration in Sealed Insulating Glass
Units using Gas Chromatography
This standard is issued under the fixed designation E2269; 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.
1. Scope E2188 Test Method for Insulating Glass Unit Performance
1.1 This test method covers procedures for using gas chro-
3. Terminology
matographs to determine the concentration of argon gas in the
3.1 Definitions—For definitions of terms found in this
space between the panes of sealed insulating glass.
standard, refer to Terminologies C162, C717, and E631.
1.2 This test method is not applicable to insulating glass
3.2 Definitions of Terms Specific to This Standard:
units containing open capillary/breather tubes.
3.2.1 fill gas—any gas or mixture of gases intended to
1.3 The values stated in inch-pound units are to be regarded
replace atmospheric air in the space between the panes of a
as standard. No other units of measurement are included in this
sealed insulating glass unit.Afill gas is typically inert; and the
standard.
most commonly used fill gases include argon, krypton, and
1.4 This standard does not purport to address all of the sulfur hexafluoride (SF ).
safety concerns, if any, associated with its use. It is the
3.2.2 sealed insulating glass unit—a pre-assembled unit,
responsibility of the user of this standard to establish appro-
comprising sealed panes of glass separated by dehydrated
priate safety, health, and environmental practices and deter-
space (s), intended for clear vision areas of buildings. the unit
mine the applicability of regulatory limitations prior to use.
isnormallyusedforwindows,windowwalls,picturewindows,
1.5 This international standard was developed in accor-
sliding doors, patio doors, or other types of windows or doors.
dance with internationally recognized principles on standard-
4. Significance and Use
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
4.1 This test method is intended to provide a means for
mendations issued by the World Trade Organization Technical
determining the concentration of fill gases, typically argon,
Barriers to Trade (TBT) Committee.
oxygen,andnitrogengasesinindividualsealedinsulatingglass
units, which were intended to be filled with a specific concen-
2. Referenced Documents
tration of fill gases at the time of manufacture.
2.1 ASTM Standards:
4.2 The fill gases, oxygen and nitrogen, are physically
C162 Terminology of Glass and Glass Products
separatedbygaschromatographyandcomparedtocorrespond-
C717 Terminology of Building Seals and Sealants
ing components separated under similar conditions from a
E177 Practice for Use of the Terms Precision and Bias in
reference standard mixture or mixtures of known composition.
ASTM Test Methods
If the carrier gas is the same as the fill gas, then just the oxygen
E355 Practice for Gas Chromatography Terms and Relation-
and nitrogen (air contaminate) are separated.
ships
4.3 The composition of the sample is calculated from the
E631 Terminology of Building Constructions
chromatogram by comparing the area under the curve of each
E691 Practice for Conducting an Interlaboratory Study to
component with the area under the curve of the corresponding
Determine the Precision of a Test Method
component on the reference standard chromatogram.
4.4 It is essential that the person or persons performing this
This test method is under the jurisdiction of ASTM Committee E06 on
test are very knowledgeable about the principles and tech-
Performance of Buildings and is the direct responsibility of Subcommittee E06.22
on Durability Performance of Building Constructions.
niques of gas chromatography, operation and calibration of gas
Current edition approved April 1, 2021. Published April 2021. Originally
chromatographs. More information can be found in Practice
approved in 2003. Last previous edition approved in 2014 as E2269 – 14. DOI:
E355.
10.1520/E2269-21.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.5 It takes time for the fill gas to equilibrate in any
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
insulatingglassunit.Thisisparticularlyimportantininsulating
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. glass units using a tubular spacer and in units containing
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2269 − 21
interior components such as tubular muntin bars. Performing a weight to the center of glass, or by clamping the center of the
this test before a unit has equilibrated could result in fill gas unit, or by using a gas extraction pump. If the gas sampling
concentrations that are measurably different than the actual fill occurs with the unit under negative pressure, contamination of
gas concentration. the gas sample can occur.
4.6 This method may be used to determine the initial fill gas 7.2 Drill or punch a hole through the edge sealant and the
concentration achieved by the filling method, or the fill gas spacer. Drilling a hole is not necessary in spacers that allow the
concentration in units that have been in service or that have needle to pass through the spacer without damage or obstruc-
been subjected to durability tests such as those described in tion to the needle.
Test Method E2188.
8. Calibration and Standardization
4.7 This is a destructive test method in that the edge seal of
the insulating glass unit is breached in order to obtain a gas 8.1 Apparatus Preparation:
sample for analysis by gas chromatography. 8.1.1 Prepare gas chromatograph as directed by the manu-
facturer.
5. Apparatus
8.2 Reference Standard Introduction and Separation:
5.1 Gas Chromatograph—There are many configurations of
8.2.1 Purging Syringe:
gas chromatographs. Check with your suppliers to assemble a
8.2.2 Fill the gas-tight syringe from the cylinder containing
suitable instrument. If your gas chromatograph is using a
the reference standard. Filling and evacuating of the syringe
helium carrier gas, it must be capable of separating argon from
must be done at a controlled rate to ensure proper sample
oxygen and nitrogen as indicated by the return of the recorded
collection.
peak to the baseline between each successive peak. If your gas
8.2.3 Remove the syringe from the cylinder outlet and
chromatograph is using the fill gas as the carrier gas, it must be
evacuate the syringe to purge any contaminants that it may
capable of separating oxygen and nitrogen as indicated by the
have contained.
return of the recorded peak to the baseline between each
8.2.4 Repeat 8.2.2 and 8.2.3 at least two more times.
successive peak.
8.2.5 Refill the syringe with the reference standard gas.
8.2.6 Introducethereferencestandardsample(s)intothegas
5.2 Chromatograms must be reproducible so that successive
chromatograph sampling port.
runs of a reference standard agree on each component peak
8.2.7 The reference standard introduction and separation
area within 60.1 %.
shall be repeated before and after the Procedure in Section 9.
6. Reagents and Materials
For a group of samples, additional recalibrations shall be
conductedperiodically(forexample,afterevery10samples)to
6.1 Gas Cylinders:
confirm uniformity.
6.1.1 Carrier Gas:
8.2.8 As a minimum, the reference standard mixtures shall
6.1.1.1 Helium carrier gas cylinder, analytical grade with
be run twice within an 8 h period when no changes to the
purity 99.9 %, ultra high purity (UHP), or
chromatograph conditions or configurations have occurred.
6.1.1.2 F
...

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.
Designation: E2269 − 14 E2269 − 21
Standard Test Method for
Determining Argon Concentration in Sealed Insulating Glass
Units using Gas Chromatography
This standard is issued under the fixed designation E2269; 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.
1. Scope
1.1 This test method covers procedures for using gas chromatographs to determine the concentration of argon gas in the space
between the panes of sealed insulating glass.
1.2 This test method is not applicable to insulating glass units containing open capillary/breather tubes.
1.3 The values stated in SIinch-pound units are to be regarded as standard. No other units of measurement are included in this
standard.
1.4 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.
1.5 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:
C162 Terminology of Glass and Glass Products
C717 Terminology of Building Seals and Sealants
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E355 Practice for Gas Chromatography Terms and Relationships
E631 Terminology of Building Constructions
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E773 Test Method for Accelerated Weathering of Sealed Insulating Glass Units (Withdrawn 2010)
E2188 Test Method for Insulating Glass Unit Performance
3. Terminology
3.1 Definitions—For definitions of terms found in this standard, refer to Terminologies C162, C717, and E631.
This test method is under the jurisdiction of ASTM Committee E06 on Performance of Buildings and is the direct responsibility of Subcommittee E06.22 on Durability
Performance of Building Constructions.
Current edition approved April 1, 2014April 1, 2021. Published May 2014April 2021. Originally approved in 2003. Last previous edition approved in 20052014 as
E2269 – 05.E2269 – 14. DOI: 10.1520/E2269-14.10.1520/E2269-21.
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’sstandard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2269 − 21
3.2 Definitions of Terms Specific to This Standard:
3.2.1 fill gas—any gas or mixture of gases intended to replace atmospheric air in the space between the panes of a sealed insulating
glass unit. A fill gas is typically inert; and the most commonly used fill gases include argon, krypton, and sulfur hexafluoride (SF ).
3.2.2 sealed insulating glass unit—a pre-assembled unit, comprising sealed panes of glass separated by dehydrated space (s),
intended for clear vision areas of buildings. the unit is normally used for windows, window walls, picture windows, sliding doors,
patio doors, or other types of windows or doors.
4. Significance and Use
4.1 This test method is intended to provide a means for determining the concentration of fill gases, typically argon, oxygen, and
nitrogen gases in individual sealed insulating glass units, which were intended to be filled with a specific concentration of argon
fill gases at the time of manufacture.
4.2 The argon, oxygen, and nitrogenfill gases, oxygen and nitrogen, are physically separated by gas chromatography and compared
to corresponding components separated under similar conditions from a reference standard mixture or mixtures of known
composition. If the carrier gas is the same as the fill gas, then just the oxygen and nitrogen (air contaminate) are separated.
4.3 The composition of the sample is calculated from the chromatogram by comparing the area under the curve of each component
with the area under the curve of the corresponding component on the reference standard chromatogram.
4.4 It is essential that the person or persons performing this test are very knowledgeable about the principles and techniques of
gas chromatography, operation and calibration of gas chromatographs. More information can be found in Practice E355.
4.5 It takes time for the fill gas to equilibrate in any insulating glass unit. This is particularly important in insulating glass units
using a tubular spacer and in units containing interior components such as tubular muntin bars. Performing this test before a unit
has equilibrated could result in fill gas concentrations that are measurably different than the actual fill gas concentration.
4.6 This method may be used to determine the initial argonfill gas concentration achieved by the filling method, or the argonfill
gas concentration in units whichthat have been in service or whichthat have been subjected to durability tests such as those
described in Test MethodsMethod E773 and E2188.
4.7 This method is not applicable to units filled with mixtures of argon and gases other than air.
4.7 This is a destructive test method in that the edge seal of the insulating glass unit is breached in order to obtain a gas sample
for analysis by gas chromatography.
4.9 The argon concentration in the gas fill is part of the information necessary to estimate the thermal performance of the sealed
insulating glass unit.
NOTE 1—Other data necessary include gap width, glass thickness, coating type, film coefficients, and so forth, but are beyond the scope of this standard.
5. Apparatus
5.1 Gas Chromatograph, Chromatograph—There are many configurations of gas chromatographs. Check with your suppliers to
assemble a suitable instrument. If your gas chromatograph is using a helium carrier gas, it must be capable of separating argon
from oxygen and nitrogen as indicated by the return of the recorded peak to the baseline between each successive peak and
including the following components:peak. If your gas chromatograph is using the fill gas as the carrier gas, it must be capable of
separating oxygen and nitrogen as indicated by the return of the recorded peak to the baseline between each successive peak.
5.1.1 Gas Sampling Valve, with a capacity of 100 to 250 μL.
5.1.2 Adsorption Column, capable of separating argon from other gases.
NOTE 2—Examples of columns which may be used include: Haysep and Restek, 5Å Plot.
E2269 − 21
5.2 Detector, such as a thermal conductivity detector (TCD).
5.3 Integrator.
5.2 Chromatograms must be reproducible so that successive runs of a reference standard agree on each component peak area
within 60.1 %.
6. Reagents and Materials
6.1 Gas Cylinders:
6.1.1 Helium carrier gas cylinder, analytical grade with purity 99.9 %.Carrier Gas:
6.1.1.1 Helium carrier gas cylinder, analytical grade with purity 99.9 %, ultra high purity (UHP), or
6.1.1.2 Fill gas carrier gas cylinder, analytical grade with purity 99.9 %, ultra high purity (UHP).
6.1.2 Compressed air cylinder (for valve actuation).
6.1.3 Liquid CO or N cylinder with dip tube, or refrigeration system for cooling column oven if using a column that requires
2 2
sub-ambient temperatures for operation.
6.2 10 mL gas-tight syringe(s) with closure valve and side port needle.Gas-tight syringe(s).
6.3 Reference Standard Mixtures:
6.3.1 At least two reference standard mixtures that contain known percentages of argon, oxygen, and nitrogen. These are required
for calibration.
6.3.2 Reference standard mixture with argon concentration greater than 98 %.
6.3.3 Reference standard mixture with argon concentration equal to 5050 % 6 5 %.
6.3.4 If the argon concentration to be determined is less than 50 %, an additional reference standard mixture is necessary that
would bracket the expected argon fill level.
NOTE 1—Suitable standard mixtures can be obtained with a certificate of analysis of the makeup of the mixture from commercial gas suppliers. The
accuracy of the results of this method depends on the availability of accurate calibration standards.
7. Sampling
7.1 Condition the insulating glass unit so that at the time of sampling a positive pressure exists inside the unit. This is may be
achieved by heating the unit above the sealing temperature or by placing the unit horizontally on a flat surface and applying a
weight to the center of glass. glass, or by clamping the center of the unit, or by using a gas extraction pump. If the gas sampling
occurs with the unit under negative pressure, contamination of the gas sample can occur.
7.2 Wrap the shank of the sampling needle with PIB (poly isobutylene) sealant or other sealing mastic.
7.2 Drill or punch a 1.6 mm hole through the edge sealant and the spacer. The hole is drilled into one of the long sides of the unit
approximately 76 mm from a corner. Drilling a hole is not necessary in spacers that allow the needle to pass through the spacer
without damage or obstruction to the needle.
7.4 Remove the drill or punch and immediately plug the hole with a finger.
E2269 − 21
7.5 Slide the finger off the hole and immediately insert the PIB wrapped sampling needle, with the syringe evacuated (plunger
forward).
7.6 Seal the needle into the hole with the PIB sealant.
8. Calibration and Standardization
8.1 Apparatus Preparation:
8.1.1 Prepare gas chromatograph as directed by the manufacturer.
NOTE 4—The following is an example of operating conditions that have been found to be satisfactory using the Haysep column for this test method:
Carrier Gas Helium, 30mL/min
Column Haysep DB, 100 to 120 mesh
Column Size 9.1 m by 3 mm stainless steel
Column (Oven) Temperature −30°C
Sampling Loop Temperature 100°C
...