1、Designation: F1374 92 (Reapproved 2012)Standard Test Method forIonic/Organic Extractables of Internal Surfaces-IC/GC/FTIRfor Gas Distribution System Components1This standard is issued under the fixed designation F1374; the number immediately following the designation indicates the year oforiginal ad
2、option or, in the 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.INTRODUCTIONSemiconductor clean rooms are serviced by high-purity gas distribution
3、 systems. This test methodpresents a procedure that may be applied for the evaluation of one or more components considered foruse in such systems.1. Scope1.1 This test method establishes a procedure for testingcomponents used in ultra-high-purity gas distribution systemsfor ionic and organic surface
4、 residues.1.2 This test method applies to in-line components contain-ing electronics grade materials in the gaseous form.1.3 Limitations:1.3.1 This test method is limited by the sensitivity of thedetection instruments and by the available levels of purity inextracting solvents. While the ion and gas
5、 chromatographicmethods are quantitative, the Fourier transform infrared spec-troscopy (FTIR) method can be used as either a qualitative ora quantitative tool. In addition, the gas chromatography (GC)and FTIR methods are used to detect hydrocarbons andhalogenated substances that remain as residues o
6、n componentinternal surfaces. This eliminates those materials with highvapor pressures, which are analyzed per the total hydrocarbonstest, from this test method.1.3.2 This test method is intended for use by operators whounderstand the use of the apparatus at a level equivalent totwelve months of exp
7、erience.1.4 The values stated in SI units are to be regarded as thestandards. The inch-pound units given in parentheses are forinformation only.1.5 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 standa
8、rd to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardstatements are given in Section 6.2. Referenced Documents2.1 ASTM Standards:2E1151 Practice for Ion Chromatography Terms and Rela-tionships2.2 Union Carbid
9、e Standard:Techniques for Measuring Trace Gas Impurities in HighPurity Gases33. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 spool piecea null component, consisting of a straightpiece of electropolished tubing and appropriate fittings, used inplace of the test component to est
10、ablish the baseline.3.1.2 standard conditions101.3 kPa, 0.0C (14.73 psia,32.0F).3.1.3 test componentany device being tested, such as avalve, regulator, or filter.3.1.4 test fluid blanka volume of test solvent adequate foranalysis.3.1.4.1 DiscussionThis is used to determine the back-ground impurity c
11、oncentrations in the test fluid. This fluid isdrawn at the same time as the fluid that is used to fill the spoolpiece and test component. It must be held in a container thatdoes not contaminate the fluid blank.3.2 Abbreviations:3.2.1 FTIRFourier transform infrared spectroscopy.1This test method is u
12、nder the jurisdiction of ASTM Committee F01 onElectronics and is the direct responsibility of Subcommittee F01.10 on Contamina-tion Control.Current edition published July 1, 2012. Published August 2012. Originallyapproved in 1992. Last previous edition approved in 2005 as F137492(2005). DOI:10.1520/
13、F1374-92R12.2For referenced ASTM standards, 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.3Available from Linde Division Union Carbide, 175
14、 E. Park Drive, Tonawanda,NY 14151.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.2 GCgas chromatography.3.2.3 ICion chromatography.3.2.4 IPAisopropanol (2-propanol).3.2.5 MSmass spectrometry.3.2.6 ppbvparts per billion by volume
15、 (such as nL/L).3.2.7 ppbwparts per billion by weight (such as ng/g).3.2.8 ppmvparts per million by volume (such as L/L).3.2.9 ppmwparts per million by weight (such as g/g).3.2.10 psidpounds per square inch differential.3.2.11 scfmstandard cubic feet per minute.3.2.12 slpmstandard litre per minute.
16、The gas volumetricflow rate measured in litres per minute at 0.0C (32F) and101.3 kPa (1 atm).4. Significance and Use4.1 The purpose of this test method is to define a procedurefor testing electropolished stainless steel components beingconsidered for installation into a high-purity gas distributions
17、ystem. Application of this test method is expected to yieldcomparable data among components tested for the purposes ofqualification for this installation.5. Apparatus5.1 Materials:5.1.1 Test FluidThe purity of fluid used for the extractionswill determine the detection limit of the test. Therefore,ex
18、tremely high purity fluids are required. At least 18.0 MVwater corrected for 18C (64F) must be used for the ionicextractables determination. Total oxidizable carbon must beless than 50 ppbw. The water must be filtered through a 0.2-m(or finer) filter. Electronics grade (or better) IPA is to be usedf
19、or the organic extractables determination.5.1.2 Spool Piece a straight run of electropolished 316-Lstainless steel tubing with no restrictions. The length of thespool piece shall be approximately 200 mm. The spool pieceshould be the same diameter as the test component.5.1.3 Capsused to seal the ends
20、 of the test component andspool piece are to be of 316-L stainless steel. For stub endcomponents, 316-L stainless steel compression fittings withnylon or polytetraflouroethylene ferrules are to be used. Forface seal fittings, stainless steel gaskets must be used.5.1.4 Glovesmade of powder free latex
21、 or natural rubberand resistant to the test fluids used in this test method.FIG. 1 Ionic/Organic Contribution Data Table IllustrationFIG. 2 Ionic/Organic Contribution Data Table IllustrationF1374 92 (2012)25.2 Instrumentation:5.2.1 Ion ChromatographThe IC is an analytical instru-ment that detects io
22、nic species in deionized (DI) water. Theeluant is passed through a column containing ion exchangeresin. A conductivity detector is used to detect the ionicspecies. The retention times of the various ionic species areused to identify the species. The area under the respective peakyields the quantity
23、of the species in the eluant. This test methoduses a column for mono- and polyvalent anions and a columnfor mono- and polyvalent cations.Asuppressor column may beused to increase sensitivity.5.2.2 Gas chromatographThe GC is an analytical instru-ment that detects organic species in the gas phase. A l
24、iquidsample is injected and heated to the vapor phase. The sampleis then passed through a column containing an adsorbent. Acarrier gas is used as the mobile phase. The retention times ofthe various peaks help to identify the organic species. The areaunder the respective peak yields the quantity of t
25、he species inthe mobile phase.NOTE 1Since the peak of the solvent will be large, it will obscurethose species that have a carbon number or retention time below that of thesolvent.5.2.3 Fourier transform infrared spectrometerThe FTIRis an analytical instrument that qualitatively or quantitativelyiden
26、tifies contaminants based on characteristic frequencies ofabsorption of infrared radiation. By identifying combinationsof absorption frequencies, identification of contaminants canbe made (see Appendix X1).6. Hazards6.1 It is required that the user have a working knowledge ofthe respective instrumen
27、tation and proper handling of testcomponents for trace analysis. Good laboratory practices mustalso be followed.6.2 Use safety precautions such as proper ventilation anddisposal when handling solvents.6.3 Gloves are to be worn at all times. After use, the glovesare to be rinsed in the appropriate te
28、st fluid.NOTE 2An alternative could be the use of disposable gloves, using anew glove for each test.7. Calibration7.1 Calibrate instruments using standard laboratory prac-tices and manufacturers recommendations.8. Test Procedure8.1 Temperature The test component and the spool pieceare to be tested a
29、t a constant temperature 6 2C in the range of26C (18 to 78F). Solvents used must be at the sametemperature.8.2 Rinse the outside of the spool piece with the test fluid(DI water (ionic) or IPA (organic) to be used for analysis.Rinse the caps and rinse any gaskets or ferrules to be used withthe respec
30、tive test fluid.8.3 Remove the caps accompanying the spool piece. Installthe stainless steel cap, rinsed as in 8.1, on one end of the spoolpiece. Using a buret or graduated pipet, measure the amount oftest fluid required to completely fill the internal volume of thespool piece. Extreme care must be
31、taken to avoid overfillingthe spool piece. Overfilling invalidates the test. Cap the openend.8.4 Invert the spool piece 20 times across the long axis, oneinversion every 30 s. Allow the spool piece to rest along thehorizontal axis for 24 h at a constant temperature 6 2C (see8.1).NOTE 3Since air is l
32、ikely to be introduced when capping, theinversion insures uniformity of the fluid.8.5 After 24 h, invert the spool piece 20 times across thelong axis, one inversion every 30 s.8.6 Remove one cap and sample the fluid. Recap the spoolpiece immediately to limit evaporation of the solvent. Ifmultiple sa
33、mples are to be run, agitate the spool piece (fourinversions in accordance with 8.4) prior to each sample.8.7 If any species are detected, the spool piece is to becleaned with the appropriate test fluid and analysis to berepeated until it is suitable for use as a control.8.8 Repeat 8.2-8.6 simultane
34、ously with the test componentand the spool piece.8.9 For the following components, observe the given guide-lines.8.9.1 RegulatorsWind the handle fully counter clockwise(or fully clockwise for a back pressure regulator). This willclose the regulator. Fully fill the inlet side first with test fluid.FI
35、G. 3 Ionic/Organic Contribution Data Table IllustrationF1374 92 (2012)3Then cap the inlet end. Turn the regulator over and prepare tofill the outlet end. Prior to adding the test fluid, turn the handlein the reverse direction to open the regulator. Now fully fill theoutlet end. Cap the outlet and be
36、gin the extraction. Duringextraction, the regulator must be resting on its side. Due to thesmall orifice separating the high and low pressure sides of aregulator, take samples from both the inlet and outlet.8.9.2 ValvesMake sure that all valves are fully openbefore starting the test. If the minimum
37、orifice is 20 % of thetube nominal diameter, take samples from both ends.8.9.3 Electropolished TubingAn entire random length(stick) of tubing must be used for this test. This is to ensure thatthe sample is representative of the entire tube. If it is notpossible to invert the sample, it may be rolled
38、.8.9.4 FiltersWith the outlet end capped, fully fill the inletside with test fluid. Then cap the inlet end. Turn the filter overand fill the outlet end. During the filling operation, slightly tiltand gently shake the filter to release air bubbles that may betrapped in the filter structure. Cap the o
39、utlet and begin theextraction. During extraction, the filter must be resting on itsside. Take samples from both the inlet and outlet.8.10 Analyze as follows, using the appropriate method:8.10.1 ICInject the water sample into the IC using theappropriate injection method. Use three injections for cati
40、onsand three injections for anions. Record the identification andquantify by the appropriate mathematical method.8.10.2 GCInject the IPA sample into the GC using theappropriate injection method. Use three injections. Record theidentification and quantify by appropriate mathematicalmethod. Only analy
41、ze for those components resolved withretention times greater than the solvent IPA peak.8.10.3 FTIRAnalyze the sample by the appropriatemethod to minimize solvent interference peaks (such as evapo-ration on a salt plate).9. Report9.1 Report the following information:9.1.1 ICReport the IC data as micr
42、ograms of ion per litreextract fluid, tabulated by ionic species (for example Na+,SO42). Also report the data as mass of each ionic species pertest component in the same table, (see Fig. 1).9.1.2 GCReport the GC data as total mass of organicsdetected per litre extract fluid and total mass of organic
43、s pertest component, (see Fig. 2).9.1.3 FTIRReport the FTIR data in tabular form, listingfrequency of absorption band and organic specie with matchingcharacteristic absorption bands. Analysis of the spectrumleading to identification of materials in the residue will alsoinclude reference spectra, (se
44、e Fig. 3).9.2 Attach the spectra for reference. A proper subtraction ofthe fluid blank spectrum from the sample spectra is acceptable,provided that proper interpretation techniques are followed andthe spool piece and fluid blank spectra are virtually identical.10. Precision and Bias10.1 Precision an
45、d bias for this test method are beingdetermined.11. Keywords11.1 components; contamination; extraction; gas distribu-tion components; ionic extractables; organic extractables; sur-face contaminationAPPENDIX(Nonmandatory Information)X1. ALTERNATIVE TESTSX1.1 Liquid Chromatography/Mass Spectrometry (L
46、C/MS)In addition to gas chromatography and Fourier trans-form infrared spectroscopy, these are quantitative or qualitativemethods, or both, that allow resolution and identification oforganic compounds.X1.2 Quadrapole Mass Spectrometer (QMS)The quadra-pole mass spectrometer accurately detects hydroca
47、rbon speciesby ionizing organic moieties in a vacuum. The ionized frag-ments are detected semi-quantitatively and individually.X1.3 Graphite Furnace Atomic Absorption Spectroscopy(GFAAS)This instrument quantitatively determines the massof species based on their absorption of specific wavelengths.An
48、elemental lamp emits the specific radiation that is passed toa photodetector after being absorbed by the sample in thefurnace. It is highly sensitive to cations but limited in scope foranions.X1.4 Inductively Coupled Plasma Atomic Emission Spec-troscopy (ICP-AES) This instrument quantitatively deter
49、-mines the mass of the species based on the emission spectra ofthe sample placed in the plasma. It is highly sensitive to cationsbut limited in scope for anions.F1374 92 (2012)4ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin 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
