1、Designation: D6060 96 (Reapproved 2009)D6060 17Standard Practice Test Method forSampling of Process Vents with a Portable GasChromatograph1This standard is issued under the fixed designation D6060; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e 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 practice test method describes a method for direct sampling and analysis of process ve
3、nts for volatile organiccompound (VOC) vapors and permanent gases using a portable gas chromatograph (GC).1.2 This practice test method is applicable to analysis of permanent gases such as oxygen (O2), carbon dioxide (CO2) andnitrogen (N2), as well as vapors from organic compounds with boiling point
4、s up to 125C.1.3 The detection limits obtained will depend on the portable gas chromatograph and detector used. Detectors available includebut are not limited to thermal conductivity, photoionization, argon ionization, and electron capture. For instruments equipped withthermal conductivity detectors
5、, typical detection limits are one to two parts per million by volume (ppm(v) with an applicableconcentration range to high percent by volume levels. For instruments with photoionization detectors detection limit of one to tenparts per billion by volume (ppb(v) are obtainable with a concentration ra
6、nge from 1000 to 2000 ppm(v). The argon ionizationdetector has an achievable detection limit of one (ppb(v), while the electron capture detector has an achievable detection limit ofone part per trillion by volume (ppt(v) for chlorinated compounds.1.4 The applicability of this practice test method sh
7、ould be evaluated for each VOC by determining stability, reproducibility,and linearity.1.5 The appropriate concentration range must also be determined for each VOC, as the range will depend on the vapor pressureof the particular VOC.1.6 The values stated in SI units are to be regarded as standard. N
8、o other units of measurement are included in this standard.1.7 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 safety, health, and healthenvironmental practices
9、 and determine theapplicability of regulatory limitations prior to use. Refer to Section 8 on Hazards for additional safety precautions.1.8 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles f
10、or the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1356 Terminology Relating to Sampling and Analysis of AtmospheresD3154 Test Method for Average Veloc
11、ity in a Duct (Pitot Tube Method)D3464 Test Method for Average Velocity in a Duct Using a Thermal AnemometerE355 Practice for Gas Chromatography Terms and Relationships2.2 Other Document:NFPA 70 National Electrical Code3NFPA 496 Standard for Purged and Pressurized Enclosures for Electrical Equipment
12、31 This test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.03 on Ambient Atmospheresand Source Emissions.Current edition approved Oct. 1, 2009Oct. 1, 2017. Published December 2009October 2017. Originally approved in 1996. L
13、ast previous edition approved in 20012009as D6060 96 (2001).(2009). DOI: 10.1520/D6060-96R09.10.1520/D6060-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the sta
14、ndards Document Summary page on the ASTM website.3 Available from National Fire Protection Association (NFPA), 1 Batterymarch Park, Quincy, MA 02169-7471, http:/www.nfpa.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what chang
15、es 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 appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the offici
16、al document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminology3.1 DefinitionsFor the definition of terms used in this practice, refer to Terminology D1356 and Practice E355.3.1 DefinitionsFor the definition of terms used i
17、n this test method, refer to Terminology D1356 and Practice E355.3.2 Definitions of Terms Specific to This Standard:3.2.1 portableportable, nrefers to gas chromatograph with internal battery, internal sample pump, and internal/rechargeablecarrier gas supply cylinder.4. Summary of PracticeTest Method
18、4.1 One end of a sampling line (typically 6 mm (14 in.) outside diameter TFE-fluorocarbon tubing) is connected to a tee in aprocess vent and the other end to a condensation trap (see 6.1), which is connected to a gas sampling bulb. The outlet of the gassampling bulb is connected to a sampling pump s
19、et at a flow rate of 0.5 to 2 L/min. The sample line from the portable gaschromatograph is inserted through the septum port of the gas sampling bulb. At user selected intervals, the internal pump of theportable gas chromatograph is activated and process vapors drawn through the injection valve of th
20、e gas chromatograph andanalyzed.5. Significance and Use5.1 This practice test method has been widely used to obtain mass balance data for process scrubbers, to determine the efficiencyof VOC emission control equipment, and to obtain data to support air permit applications.5.2 This practice test meth
21、od will have applications to the MACT MaximumAchievable Control Technology (MACT) Rule andmay have applications to ComplianceAssurance Monitoring verification required by the 1990 CleanAirAct Title IIIAmendments.5.3 This practice, test method, when used with Test Methods D3464 or D3154 or on-line pr
22、ocess flow meter data, can be usedto calculate detailed emission rate profiles for VOCs from process vents.5.4 This practice test method provides nearly real time results that can detect process changes or upsets that may be missed usingconventional sorbent tube or integrated gas sampling bag sampli
23、ng.6. Interferences6.1 Water or liquid in the process line will plug the sample line of the gas chromatograph, since the injection valve of mostportable GCs is not heated. The condensation trap is designed to protect the portable gas chromatograph if liquids are present oroccur during process upset.
24、FIG. 1 Schematic of Process Sampling EquipmentD6060 1726.2 Interferences sometimes result from analytes having similar retention times during gas chromatography.6.3 General approaches which can be followed to resolve such interferences are given below:6.3.1 Change the type of column, length of colum
25、n, or operating conditions.6.3.2 Analyze using a nonpolar methyl silicone column which separates according to boiling point of the compounds and a polarcolumn whose separations are influenced by the polarity of the compounds.46.3.3 Use a mass spectrometer to verify the identity of peaks.7. Apparatus
26、7.1 A schematic drawing of a typical sampling setup is shown in Fig. 1. The laptop computer may be physically located nearthe gas chromatograph as shown in Fig. 1, or located remotely. In addition, some portable gas chromatographs have an integralcomputer. Use a short piece of 1.5 mm (116 in.) outsi
27、de diameter by 1 mm (0.04 in.) inside diameter stainless steel tubing as thesampling probe line from the gas sampling bulb to the GC inlet.7.2 Portable Gas Chromatograph (GC), with a thermal conductivity, photoionization, argon ionization, electron capture or otherappropriate detector, internal/rech
28、argeable carrier gas supply, and internal sampling pump.7.2.1 Portable gas chromatographs are typically equipped with particulate filters which should be replaced periodically.7.3 Data Logger, device used for automated storage of output from a flow measurement device.7.4 Gas Sampling Bulb, 125 mL ca
29、pacity with septum port.7.5 Personal Sampling Pump.7.6 Gas-Tight Syringe, 1, 10, 100, 500 mL capacity or other convenient sizes for preparing standards.7.7 Microlitre Syringes, 10, 25, 50, 100 L or other convenient sizes for preparing standards.7.8 Gas Sampling Bags, for preparation of gas standards
30、. Bags constructed of various polymer films, such as polyvinylidenefluoride, fluorinated ethylenepropylene, (tetrafluoroethylene)-fluorocarbon, polyvinylidene chloride, polyethylene and mixedpolymer multilayers, with a variety of fittings and capacities (typically 1 to 200 L) are available.7.9 Therm
31、al Anemometer, Vane Anemometer, Mass Flowmeter or Pitot Tube, for measurement of vent velocity.7.10 Condensation Trap, Filtering Flask, 250 or 500 mL polypropylene fitted with a stopper.7.11 TFE-Fluorocarbon Tubing, 6 mm (14 in.) outside diameter by 5 mm (316 in.) inside diameter.7.12 Data System, a
32、n integral or external computer used for control of operation of a portable gas chromatograph, datareduction, and storage of results.8. Hazards8.1 See NFPA496 for use of electrical equipment in areas classified as hazardous byArticle 500 of NFPA70, National ElectricalCode. 70. A purged and pressuriz
33、ed enclosure is required.9. Calibration9.1 Suitable knowns analytes at known concentrations may be prepared by the filling of a gas sampling bag with a knownvolume of air. Inject a known volume of gas or liquid containing the analyte(s) of interest into the bag and knead the bag to mix.Permeation tu
34、bes or rigid chambers may also be used for preparation of gas standards. Reference standards in compressed gascylinders certified as to concentration and analytic uncertainty by the manufacturer are also available. Refer to Methods of AirSampling and Analysis5 for applicable guidelines for all of th
35、ese gas standard preparation techniques.9.2 Although standards of some compounds prepared in gas bags are very stable, others show sample loss during storage dueto permeation permeation, reactivity, or surface adsorption. As a general guideline prepare standards fresh daily.9.3 Prepare at least two
36、reference standards containing varying concentrations of each component. Bracket the expectedconcentrations of each component in the testing of the process vent, if known.9.3.1 Connect the gas sampling bag to the inlet or the calibration port of the GC and initiate the analysis. Perform at leasttrip
37、licate injections of each standard.9.3.2 The quantitative response (calibration) of a GC detector may be determined by the measurement of the peak height or peakarea using the Data System or electronic integrator.69.3.3 Following the standardcalibration, analyze a gas sampling bag containing air onl
38、y (blank). If carryover is 1 % increasethe sampling period (internal GC pump time). Typical sampling periods are 20 to 45 s, however, this parameter must be optimizedfor each VOC analyzed.4 The columns in most portable gas chromatographs are easily interchanged. One manufacturer has an instrument th
39、at simultaneously injects onto two user selected columnmodules.5 Lodge, James P., ed., Methods of Air Sampling and Analysis, Intersociety Committee, Lewis Publishers, Inc., 3rd ed., 1988, pp. 1526.6 Most portable GCS are equipped with data systems that automatically generate a calibration curve.D606
40、0 17310. Procedure10.1 Preparation of the Gas Chromatograph:10.1.1 Fill the internal carrier gas reservoir as described by the manufacturer.10.1.2 Select a carrier gas flow or column pressure and column temperature compatible with the column selected for theseparation.10.1.3 Calibrate the chromatogr
41、aphic columnsystem to determine the relative retention times and response of the variouscompounds of interest.10.2 Preparation of the Sampling Train:10.2.1 Assemble the sampling train as shown in Fig. 1. Stainless steel or glass may be substituted for the TFE-fluorocarbontransfer line.710.2.2 For pr
42、ocess vents containing high concentrations of higher boiling (125C) low vapor pressure (115 %, repeat the analysis of the vent after identifying source of the problem.Typical causes of poor recovery include leak in sample train, partially or completely plugged instrument filter, improper internalpum
43、p or injection valve operation, and detector malfunction.10.3.5 Data reduction, either by peak height or peak area measurement, may now be performed. Some portable GCsautomatically developtypically produce files that can be directly loaded into an EXCEL a Microsoft Excel9 or Lotusotherspreadsheet fo
44、rmat. Most data loggers for recording of flow also developproduce files that can be easily loaded into spreadsheets,which can be combined into one spreadsheet to developproduce a detailed emission rate profile for each organic compound. Anexample of a typical spreadsheet is given in Appendix X1.10.3
45、.6 By direct sampling of process vents with a portable gas chromatograph, process trends and conditions can be monitoredand more easily and quickly optimized. A graphical display illustrating how simultaneous monitoring of the inlet and outlet of awater scrubber using two portable gas chromatographs
46、 aided optimization of flow rate required to remove an organic compoundfrom a vent stream is shown in Appendix X2. This chart was created in EXCELMicrosoft Excel from the data shown in AppendixX1.11. Calculations11.1 Calculation of the Concentration of Organic Chemical Vapor Standards in Gas Samplin
47、g Bags:11.1.1 Calculate the concentration C in parts per million by volume (ppm(v) as follows:c 5L 3D 31000324.45MW3V (1)where:L = volume of liquid added to bag, L,D = density of liquid, kg/m3,7 Heated steel lines will degrade or destroy chlorinated organic compounds.8 Method 18Measurement of Gaseou
48、s Organic Compound Emissions by Gas Chromatography, 40 CFR 60, App. A, 1994, pp. 792821.9 Microsoft Excel is a trademark of the Microsoft Corporation, Redmond, WA.D6060 17424.45 = molar volume of ideal gas, L/mole, at 25C and 101.3 kPa pressure (760 mm Hg),MW = molecular weight of compound, g/mol, a
49、ndV = total volume = volume air in bag plus volume of vaporized liquid added, L, and1000 = 1000 mL/L.11.2 Calculate the vent flow rate at standard conditions.11.2.1 For instruments that correct to standard conditions calculate as follows:F 5V 3A 31000 (2)where:F = flow, L/min at 25C and 101.3 kPa pressure (760 mm Hg),V = air velocity, m/min, andA = vent cross sectional area, m2.11.2.2 For instruments that do not automatically correct to standard conditions:F 5V 3A 3P 329831000101.33T1273! (3)where:P = pressure of vent in kPa, andT = temperature of vent,
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