1、Designation: E2269 05E2269 14Standard Test Method forDetermining Argon Concentration in Sealed Insulating GlassUnits using Gas Chromatography1This standard is issued under the fixed designation E2269; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers procedures for using gas chromatographs to determine the concent
3、ration of argon gas in the spacebetween 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 SI units are to be regarded as the standard. The values given in parentheses are for informa
4、tion only.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 responsibilityof the user of this standard to establish appropriate safety and health practices and det
5、ermine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C162 Terminology of Glass and Glass ProductsC717 Terminology of Building Seals and SealantsE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE355 Practice for Gas Chromat
6、ography Terms and RelationshipsE631 Terminology of Building ConstructionsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE773 Test Method for Accelerated Weathering of Sealed Insulating Glass Units (Withdrawn 2010)3E2188 Test Method for Insulating Gla
7、ss Unit Performance3. Terminology3.1 DefinitionsFor definitions of terms found in this standard, refer to Terminologies C162, C717, and E631.3.2 Definitions of Terms Specific to This Standard:3.2.1 fill gasany gas or mixture of gases intended to replace atmospheric air in the space between the panes
8、 of a sealedinsulating glass unit. A fill gas is typically inert; and the most commonly used fill gases include argon, krypton, and sulfurhexafluoride (SF6).3.2.2 sealed insulating glass unita pre-assembled unit, comprising sealed panes of glass separated by dehydrated space (s),intended for clear v
9、ision 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 Use4.1 This test method is intended to provide a means for determining the concentration of argon, oxygen, and nitrogen ga
10、ses inindividual sealed insulating glass units, which were intended to be filled with a specific concentration of argon at the time ofmanufacture.1 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
11、DurabilityPerformance of Building Constructions.Current edition approved May 1, 2005April 1, 2014. Published May 2005May 2014. Originally approved in 2003. Last previous edition approved in 20032005 asE2269 03.E2269 05. DOI: 10.1520/E2269-05.10.1520/E2269-14.2 For referencedASTM standards, visit the
12、ASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.This document is
13、 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. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropr
14、iate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.2 The argon, oxygen, and nitrogen are physically separated by
15、gas chromatography and compared to correspondingcomponents separated under similar conditions from a reference standard mixture or mixtures of known composition.4.3 The composition of the sample is calculated from the chromatogram by comparing the area under the curve of eachcomponent with the area
16、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 ofgas chromatography, operation and calibration of gas chromatographs. More information
17、 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 unitsusing a tubular spacer and in units containing interior components such as tubular muntin bars. Performing this test before a unithas
18、 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 argon gas concentration achieved by the filling method, or the argon gasconcentration in units which have been in service or
19、 which have been subjected to durability tests such as those described in TestMethods E773 and E2188.4.7 This method is not applicable to units filled with mixtures of argon and gases other than air.4.8 This is a destructive test method in that the edge seal of the insulating glass unit is breached
20、in order to obtain a gas samplefor 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 sealedinsulating glass unit.NOTE 1Other data necessary include gap width, glass thickness, coating type, film
21、coefficients, and so forth, but are beyond the scope of this standard.5. Apparatus5.1 Gas Chromatograph, capable of separating argon from oxygen and nitrogen as indicated by the return of the recorded peakto the baseline between each successive peak and including the following components:5.1.1 Gas S
22、ampling Valve, with a capacity of 100 to 250 L.5.1.2 Adsorption Column, capable of separating argon from other gases.NOTE 2Examples of columns which may be used include: Haysep4 and Restek, 5 Plot.5.2 Detector, such as a thermal conductivity detector (TCD).5.3 Integrator.5.4 Chromatograms must be re
23、producible so that successive runs of a reference standard agree on each component peak areawithin 6 0.1 %.60.1 %.6. Reagents and Materials6.1 Gas Cylinders:6.1.1 Helium carrier gas cylinder, analytical grade with purity 99.9 %.6.1.2 Compressed air cylinder (for valve actuation).6.1.3 Liquid CO2 or
24、N2 cylinder with dip tube, or refrigeration system for cooling column oven if using a column that requiressub-ambient temperatures for operation.6.2 10 mL gas-tight syringe(s) with closure valve and side port needle.6.3 Reference Standard Mixtures:6.3.1 At least 2two reference standard mixtures that
25、 contain known percentages of argon, oxygen, and nitrogen. These arerequired 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 50 6 5 %.6.3.4 If the argon concentration to be determined is le
26、ss than 50 %, an additional reference standard mixture is necessary thatwould bracket the expected argon fill level.NOTE 3Suitable standard mixtures can be obtained with a certificate of analysis of the makeup of the mixture from commercial gas suppliers. Theaccuracy of the results of this method de
27、pends on the availability of accurate calibration standards.7. Sampling7.1 Condition the insulating glass unit so that at the time of sampling a positive pressure exists inside the unit. This is achievedby heating the unit above the sealing temperature or by placing the unit horizontally on a flat s
28、urface and applying a weight to thecenter of glass. If the gas sampling occurs with the unit under negative pressure, contamination of the gas sample can occur.4 The term “Haysep” and the Haysep logo are trademarks of Valco Instruments Co. Inc., P.O. Box 1674, Bandera, TX 78003.E2269 1427.2 Wrap the
29、 shank of the sampling needle with PIB (poly isobutylene) sealant or other sealing mastic.7.3 Drill or punch a 1.6 mm (116 in.) hole through the edge sealant and the spacer. The hole is drilled into one of the long sidesof the unit approximately 76 mm (3 in.) from a corner. Drilling a hole is not ne
30、cessary in spacers that allow the needle to passthrough the spacer without damage or obstruction to the needle.7.4 Remove the drill or punch and immediately plug the hole with a finger.7.5 Slide the finger off the hole and immediately insert the PIB wrapped sampling needle, with the syringe evacuate
31、d (plungerforward).7.6 Seal the needle into the hole with the PIB sealant.8. Calibration and Standardization8.1 Apparatus Preparation:8.1.1 Prepare gas chromatograph as directed by the manufacturer.NOTE 4The following is an example of operating conditions that have been found to be satisfactory usin
32、g the Haysep column for this test method:Carrier Gas Helium, 30mL/minColumn Haysep DB, 100 to 120 meshColumn Size 9.1 m by 3 mm (30 ft by 18 in.)stainless steelColumn Size 9.1 m by 3 mm stainless steelColumn (Oven) Temperature 30CSampling Loop Temperature 100CSample Volume 250 L8.2 Reference Standar
33、d Introduction and Separation:8.2.1 Purging Syringe:8.2.2 Fill the 10 mL gas-tight syringe from the cylinder containing the reference standard. Filling and evacuating of the syringemust be done at a controlled rate to ensure proper sample collection.8.2.3 Remove the syringe from the cylinder outlet
34、and evacuate the syringe to purge any contaminants that it may havecontained.8.2.4 Repeat 8.2.2 and 8.2.3 at least 2two more times.8.2.5 Refill the syringe with the reference standard gas.8.2.6 Close the syringe valve and remove it from the cylinder.8.2.7 Introduce the reference standard sample(s) i
35、nto the gas chromatograph sampling port.8.2.8 The reference standard introduction and separation shall be repeated before and after the Procedure in Section 99 Fora group of samples, additional re-calibrations shall be conducted periodically (for example, after every 10 samples) to confirmuniformity
36、.8.2.9 As a minimum the reference standard mixtures shall be run twice within an 8-hour8-h period when no changes to thechromatograph conditions or configurations have occurred.8.2.10 Record the chromatogram and the integrated percentages of oxygen, nitrogen and argon (O2, N2, and Ar).9. Procedure9.
37、1 With the syringe evacuated (plunger forward), insert the syringe needle into the insulating glass unit as described in Section7.9.2 Fill the syringe with the airspace gas then evacuate its contents back into the airspace to purge any contaminants that it mayhave contained. Filling and evacuating o
38、f the syringe must be done at a controlled rate to ensure proper sample collection.9.3 Repeat 9.2 at least two more times.9.4 Fill the syringe with the gas sample.9.5 Close the syringe valve.9.6 Carefully grip the needle at its base and pull it out of the gas space.9.7 Insert the needle into the gas
39、 sampling inlet and open the syringe valve.9.8 Inject the contents of the syringe into the column via the septum connected at the inlet of the gas sampling valve.9.9 Record the chromatogram with the integrated percentages of Ar, O2, and N2.10. Calculation or Interpretation of Results10.1 Refer to Pr
40、actice E355.E2269 14311. Report11.1 Complete Description of Specimen Tested:11.1.1 Dimensions of the test specimen (width by height) and overall thickness.11.1.2 Type and thickness of glass.11.1.3 Glass coatings and surface locations if applicable.11.1.4 Airspace thickness(es).11.1.5 Describe the sp
41、acer composition(s) and configuration(s).11.1.6 Describe the corner construction including the type and number of corner keys.11.1.7 Desiccant type and quantity, if provided.11.1.8 Presence and composition (if known) of muntin bars.11.2 Report composition of reference standard gases used.11.3 Report
42、 type of adsorption column used, column size, column temperature, sampling loop temperature, and sample volume.11.4 Report argon concentration measured for each reference standard gas before and after measurement of the sample.11.5 Report measured argon concentration for each sample.12. Precision an
43、d Bias512.1 PrecisionThe precision of this test method is based on an interlaboratory study of E06 - ASTM E2269, Standard TestMethod for Determining Argon Concentration in Sealed Insulating Glass Units using Gas Chromatography, conducted in 2013. Asingle laboratory participated in this study submitt
44、ing a total of ten test results forArgon concentration. Because of the destructivenature of the testing, every “test result” reported represents an individual determination. Except for the use of only one laboratory,Practice E691 was followed for the design and analysis of the data; the details are
45、given in ASTM Research Report No. RR:E06-1004.12.1.1 Repeatability (r)The difference between repetitive results obtained by the same operator in a given laboratory applyingthe same test method with the same apparatus under constant operating conditions on identical test material within short interva
46、lsof time would, in the long run, in the normal and correct operation of the test method, exceed the following values only in onecase in 20.12.1.1.1 Repeatability can be interpreted as the maximum difference between two results, obtained under repeatabilityconditions, that is accepted as plausible d
47、ue to random causes under normal and correct operation of the test method.12.1.1.2 The single-lab repeatability estimate is listed in Table 1.12.1.2 Reproducibility (R)The difference between two single and independent results obtained by different operators applyingthe same test method in different
48、laboratories using different apparatus on identical test material would, in the long run, in thenormal and correct operation of the test method, exceed the following values only in one case in 20.12.1.2.1 Reproducibility can be interpreted as the maximum difference between two results, obtained unde
49、r reproducibilityconditions, that is accepted as plausible due to random causes under normal and correct operation of the test method.12.1.2.2 Reproducibility limits cannot be determined from single-lab data.12.1.3 The above terms (repeatability limit and reproducibility limit) are used as specified in Practice E177.12.1.4 Any judgment in accordance with statements 12.1.1 and 12.1.2 will have an approximate 95 % probability of beingcorrect. The precision statistics obtained in this ILS must not be treated as exact mathematical quantities which are applicable
