1、Designation: E 2269 05Standard Test Method forDetermining Argon Concentration in Sealed Insulating GlassUnits using Gas Chromatography1This standard is issued under the fixed designation E 2269; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers procedures for using gas chro-matographs to determine the concentrati
3、on of argon gas in thespace between the panes of sealed insulating glass.1.2 This test method is not applicable to insulating glassunits containing open capillary/breather tubes.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationon
4、ly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Reference
5、d Documents2.1 ASTM Standards:2C 162 Terminology of Glass and Glass ProductsC 717 Terminology of Building Seals and SealantsE 355 Practice for Gas Chromatography Terms and Rela-tionshipsE 631 Terminology of Building ConstructionsE 773 Test Method for Accelerated Weathering of SealedInsulating Glass
6、UnitsE 2188 Test Method for Insulating Glass Unit Performance3. Terminology3.1 DefinitionsFor definitions of terms found in thisstandard, refer to Terminologies C 162, C 717, and E 631.3.2 Definitions of Terms Specific to This Standard:3.2.1 fill gasany gas or mixture of gases intended toreplace atm
7、ospheric air in the space between the panes of asealed insulating glass unit. A fill gas is typically inert; and themost commonly used fill gases include argon, krypton, andsulfur hexafluoride (SF6).3.2.2 sealed insulating glass unita pre-assembled unit,comprising sealed panes of glass separated by
8、dehydratedspace (s), intended for clear vision areas of buildings. the unitis 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 fordetermining the concentr
9、ation of argon, oxygen, and nitrogengases in individual sealed insulating glass units, which wereintended to be filled with a specific concentration of argon atthe time of manufacture.4.2 The argon, oxygen, and nitrogen are physically sepa-rated by gas chromatography and compared to correspondingcom
10、ponents separated under similar conditions from a refer-ence standard mixture or mixtures of known composition.4.3 The composition of the sample is calculated from thechromatogram by comparing the area under the curve of eachcomponent with the area under the curve of the correspondingcomponent on th
11、e reference standard chromatogram.4.4 It is essential that the person or persons performing thistest are very knowledgeable about the principles and tech-niques of gas chromatography, operation and calibration of gaschromatographs. More information can be found in PracticeE 355.4.5 It takes time for
12、 the fill gas to equilibrate in anyinsulating glass unit. This is particularly important in insulatingglass units using a tubular spacer and in units containinginterior components such as tubular muntin bars. Performingthis test before a unit has equilibrated could result in fill gasconcentrations t
13、hat are measurably different than the actual fillgas concentration.4.6 This method may be used to determine the initial argongas concentration achieved by the filling method, or the argongas concentration in units which have been in service or which1This test method is under the jurisdiction of ASTM
14、 Committee E06 onPerformance of Buildings and is the direct responsibility of Subcommittee E06.22on Durability Performance of Building Constructions.Current edition approved May 1, 2005. Published May 2005. Originallyapproved in 2003. Last edition approved in 2003 as E 2269 03.2For referenced ASTM s
15、tandards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke
16、n, PA 19428-2959, United States.have been subjected to durability tests such as those describedin Test Methods E 773 and E 2188.4.7 This method is not applicable to units filled withmixtures of argon and gases other than air.4.8 This is a destructive test method in that the edge seal ofthe insulatin
17、g glass unit is breached in order to obtain a gassample for analysis by gas chromatography.4.9 The argon concentration in the gas fill is part of theinformation necessary to estimate the thermal performance ofthe sealed insulating glass unit.NOTE 1Other data necessary include gap width, glass thickn
18、ess,coating type, film coefficients, and so forth, but are beyond the scope ofthis standard.5. Apparatus5.1 Gas Chromatograph, capable of separating argon fromoxygen and nitrogen as indicated by the return of the recordedpeak to the baseline between each successive peak andincluding the following co
19、mponents:5.1.1 Gas Sampling Valve, with a capacity of 100 to 250 L.5.1.2 Adsorption Column, capable of separating argon fromother gases.NOTE 2Examples of columns which may be used include: Haysep3and Restek, 5 Plot.5.2 Detector, such as a thermal conductivity detector(TCD).5.3 Integrator.5.4 Chromat
20、ograms must be reproducible so that successiveruns of a reference standard agree on each component peakarea within 6 0.1 %.6. Reagents and Materials6.1 Gas Cylinders:6.1.1 Helium carrier gas cylinder, analytical grade withpurity 99.9 %.6.1.2 Compressed air cylinder (for valve actuation).6.1.3 Liquid
21、 CO2or N2cylinder with dip tube, or refrigera-tion system for cooling column oven if using a column thatrequires sub-ambient temperatures for operation.6.2 10 mL gas-tight syringe(s) with closure valve and sideport needle.6.3 Reference Standard Mixtures:6.3.1 At least 2 reference standard mixtures t
22、hat containknown percentages of argon, oxygen, and nitrogen. These arerequired for calibration.6.3.2 Reference standard mixture with argon concentrationgreater than 98 %.6.3.3 Reference standard mixture with argon concentrationequal to 50 6 5%.6.3.4 If the argon concentration to be determined is les
23、s than50 %, an additional reference standard mixture is necessarythat would bracket the expected argon fill level.NOTE 3Suitable standard mixtures can be obtained with a certificateof analysis of the makeup of the mixture from commercial gas suppliers.The accuracy of the results of this method depen
24、ds on the availability ofaccurate calibration standards.7. Sampling7.1 Condition the insulating glass unit so that at the time ofsampling a positive pressure exists inside the unit. This isachieved by heating the unit above the sealing temperature orby placing the unit horizontally on a flat surface
25、 and applyinga weight to the center of glass. If the gas sampling occurs withthe unit under negative pressure, contamination of the gassample can occur.7.2 Wrap the shank of the sampling needle with PIB (polyisobutylene) sealant or other sealing mastic.7.3 Drill or punch a 1.6 mm (116 in.) hole thro
26、ugh the edgesealant and the spacer. The hole is drilled into one of the longsides of the unit approximately 76 mm (3 in.) from a corner.Drilling a hole is not necessary in spacers that allow the needleto pass through the spacer without damage or obstruction to theneedle.7.4 Remove the drill or punch
27、 and immediately plug thehole with a finger.7.5 Slide the finger off the hole and immediately insert thePIB wrapped sampling needle, with the syringe evacuated(plunger forward).7.6 Seal the needle into the hole with the PIB sealant.8. Calibration and Standardization8.1 Apparatus Preparation:8.1.1 Pr
28、epare gas chromatograph as directed by the manu-facturer.NOTE 4The following is an example of operating conditions that havebeen found to be satisfactory using the Haysep column for this testmethod:Carrier Gas Helium, 30mL/minColumn Haysep DB, 100 to 120 meshColumn Size 9.1 m by 3 mm (30 ft by18 in.
29、) stainless steelColumn (Oven) Temperature 30CSampling Loop Temperature 100CSample Volume 250 L8.2 Reference Standard Introduction and Separation:8.2.1 Purging Syringe:8.2.2 Fill the 10 mL gas-tight syringe from the cylindercontaining the reference standard. Filling and evacuating of thesyringe must
30、 be done at a controlled rate to ensure propersample collection.8.2.3 Remove the syringe from the cylinder outlet andevacuate the syringe to purge any contaminants that it mayhave contained.8.2.4 Repeat 8.2.2 and 8.2.3 at least 2 more times.8.2.5 Refill the syringe with the reference standard gas.8.
31、2.6 Close the syringe valve and remove it from thecylinder.8.2.7 Introduce the reference standard sample(s) into the gaschromatograph sampling port.8.2.8 The reference standard introduction and separationshall be repeated before and after the Procedure in Section 9.For a group of samples, additional
32、 re-calibrations shall beconducted periodically (for example, after every 10 samples) toconfirm uniformity.3The term “Haysep” and the Haysep logo are trademarks of Valco InstrumentsCo. Inc., P.O. Box 1674, Bandera, TX 78003.E22690528.2.9 As a minimum the reference standard mixtures shallbe run twice
33、 within an 8-hour period when no changes to thechromatograph conditions or configurations have occurred.8.2.10 Record the chromatogram and the integrated percent-ages of oxygen, nitrogen and argon (O2,N2, and Ar).9. Procedure9.1 With the syringe evacuated (plunger forward), insert thesyringe needle
34、into the insulating glass unit as described inSection 7.9.2 Fill the syringe with the airspace gas then evacuate itscontents back into the airspace to purge any contaminants thatit may have contained. Filling and evacuating of the syringemust be done at a controlled rate to ensure proper samplecolle
35、ction.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 thegas space.9.7 Insert the needle into the gas sampling inlet and open thesyringe valve.9.8 Inject the contents of the syrin
36、ge into the column via theseptum connected at the inlet of the gas sampling valve.9.9 Record the chromatogram with the integrated percent-ages of Ar, O2, and N2.10. Calculation or Interpretation of Results10.1 Refer to Practice E 355.11. Report11.1 Complete Description of Specimen Tested:11.1.1 Dime
37、nsions 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 spacer composition(s) and configura-tion(s).11.1.6 Describe the corner construction includ
38、ing the typeand 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 type of adsorption column used, column size,column temperature, sampling loop temperatu
39、re, and samplevolume.11.4 Report argon concentration measured for each refer-ence standard gas before and after measurement of the sample.11.5 Report measured argon concentration for each sample.12. Precision and Bias12.1 Precision and bias for this test method are beingdetermined.13. Keywords13.1 f
40、ill gas; gas chromatography; gas concentration; sealedinsulating glass unitAPPENDIX(Nonmandatory Information)X1. GAS FILL CORRECTION FOR HOLLOW TUBE SPACERS PRIOR TO EQUILIBRIUMFIG. X1.1 IG Unit DimensionsE2269053X1.1 Initial Gas Fill Correction Only for Hollow TubeSpacersX1.1.1 This correction is i
41、ntended for use prior to gasequilibrium.X1.1.2 This correction is intended for use in insulating glassunits made with hollow tube spacers.X1.1.3 The correction given below may be suitable for usewhen gas-filling insulating glass units are made with hollowtube spacers. Air can remain in the hollow tu
42、bes after gascompletely fills the airspace. When this air and the fill gassubsequently mix together, the actual percentage of fill gas inthe insulating glass unit can be of lesser concentration thanexpected.Corrected Initial Gas Fill % 5Volume Fill Gas InitialTotal Gas Space Volume(X1.1)Volume Fill
43、Gas Initial 5Airspace Volume!% Gas Fill Initial!(X1.2)Airspace Volume 5L 2w!W 2w!t! (X1.3)Total Gas Space Volume5 Airspace Volume 1 Unfilled Spacer Volume 1 Void Spaces in Desiccant(X1.4)Unfilled Spacer Volume5 a 1 % Desiccant Fill!2L w! 1 2W w!# (X1.5)Void Space in Desiccant5 a % Desiccant Fill!% D
44、esiccant Voids!2L w! 1 2W w!#(X1.6)where:L = spacer length in the long legW = spacer length on the short legw = width of hollow tube spacert = airspace thicknessa = spacer corner cross sectionCorrected Initial Gas Fill % 5L 2w!W 2w!t!% Gas Fill!L 2w!W 2w!t!1 a1 Desiccant Fill!2L w!1 2W w!# 1aDesicca
45、nt Fill!Desiccant Voids!2L w! 1 2W w!# (X1.7)NOTE X1.1The voids present in the desiccant fill are represented inthe formula in order to acknowledge their presence. The % desiccant voidsare not actually calculated when using the formula to determine the final% gas fill.Ignoring the void space in the
46、desiccant, the equation reads:Corrected Initial Gas Fill % 5L 2w!W 2w!t!% Gas Fill!L 2w!W 2w!t! 1a1 Desiccant Fill!2L w! 1 2W w!#(X1.8)FIG. X1.2 Unfilled Spacer VolumeE2269054ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentio
47、nedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee an
48、d must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting o
49、f theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (p
