1、Designation: E806 17Standard Test Method forCarbon Tetrachloride and Chloroform in Liquid Chlorine byDirect Injection (Gas Chromatographic Procedure)1This standard is issued under the fixed designation E806; the number immediately following the designation indicates the year oforiginal adoption or,
2、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.1. Scope*1.1 This test method is designed for the determination ofcarbon tetrachloride (CCl4)
3、 and chloroform (CHCl3) in liquidchlorine. The lower limit of detection is dependent on thesample size and the instrument used; five ppm (w/w) isachievable.1.2 Review the current Safety Data Sheet (SDS) for detailedinformation concerning toxicity, first aid procedures, and safetyprecautions.1.3 The
4、values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.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
5、 safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Section 7 and in 9.2.3.2. Referenced Documents2.1 ASTM Standards:2E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Indus
6、trial and Spe-cialty Chemicals (Withdrawn 2009)32.2 Federal Standard:449 CFR 173 Code of Federal Regulations Title 49 Transpor-tation; ShippersGeneral Requirements for Shipments andPackagings, including Sections:173.304 Charging of Cylinders with Liquefied CompressedGas173.314 Requirements for Compr
7、essed Gases in Tank Cars173.315 Compressed Gases in Cargo Tanks and PortableTank Containers2.3 Other Document:Chlorine Institute Pamphlet No. 1 Chlorine Basics53. Summary of Test Method3.1 A sample of liquid chlorine is injected into a gaschromatograph (GC), equipped with a column capable ofseparati
8、ng CCl4and CHCl3from Cl2and other impurities,using a suitable syringe. The amounts of CCl4and CHCl3inthe sample are determined by comparison of the areas of thepeaks, obtained with the samples, to areas of peaks obtainedwith suitable calibration standards, under the same conditions.4. Significance a
9、nd Use4.1 CCl4and CHCl3may be present in trace amounts inliquid chlorine. The use of chlorine to purify water would thentransfer these compounds to the water. Therefore, when theconcentrations of the CCl4and CHCl3in the liquid chlorine areknown, the maximum amounts contributed to the water by thechl
10、orine can be estimated.5. Apparatus5.1 Gas Chromatograph, equipped with:5.1.1 Injection Port, must be lined with glass, Monel,6ornickel; or column must be installed for on-column injection.5.1.2 Septa, from Viton.7Silicone septa may produce arti-facts that may interfere with the analysis.5.1.3 Colum
11、n, Column Materials, and Packing, must becompatible with chlorine. Silanized supports and silanizedglass wool must be avoided. Column must be able to separateCl2, CCl4, and CHCl3. Columns that have been found to besuitable are:1This test method is under the jurisdiction of ASTM Committee D16 onAroma
12、tic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.16 on Industrial and Specialty Product Standards.Current edition approved March 1, 2017. Published March 2017. Originallyapproved in 1981. Last previous edition approved in 2008 as E806 08. DOI:10.1520/E0806-1
13、7.2For 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.3The last approved version of this historical standard is r
14、eferenced onwww.astm.org.4Available from U.S. Government Printing Office, Superintendent ofDocuments, 732 N. Capitol St., NW, Washington, DC 20401-0001, http:/www.access.gpo.gov.5Available from The Chlorine Institute Inc., 1300 Wilson Blvd., Suite 525,Arlington, VA 22209, https:/www.chlorineinstitut
15、e.org.6Monel is a registered trademark of Special Metals Corporation.7Viton is a registered trademark of The Chemours Company.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United St
16、atesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to T
17、rade (TBT) Committee.15.1.3.1 Nickel Tubing, 3.05 m by 3.175 mm outsidediameter, packed with 10 % sodium chloride solution onPorasil C8(see Appendix X1 for packing preparation). This isthe preferred packing.5.1.3.2 Polytetrafluoroethylene Tubing, 3.05mby2mminside diameter, packed with 20 % Kel-F9No.
18、 10 oil on 60/80mesh Chromosorb10WAW.5.1.3.3 Glass Tubing, 3.05 m by 2 mm inside diameter,packed with 20 % Halocarbon111025 on 60/80 mesh Chromo-sorb W AW.5.1.4 Flame Ionization Detector.5.1.5 Recorder, compatible with the GC detector output.5.1.6 Electronic Integrator (optional), compatible with th
19、eGC detector output.5.2 Balance, capacity 5000 g, reading to 6 1g.126. Reagents and Materials6.1 Purity of ReagentsUnless otherwise indicated, it isintended that all reagents shall conform to the specifications ofthe Committee onAnalytical Reagents of theAmerican Chemi-cal Society, where such specif
20、ications are available.13Othergrades may be used, provided it is first ascertained that thereagent is of sufficiently high purity to permit its use withoutlessening the accuracy of the determination.6.2 Chlorine, liquid, with less than 10 g/g each of CCl4andCHCl3. This may be prepared by condensing
21、the gaseous phaseabove regular production chlorine.146.3 Carbon Tetrachloride, reagent grade.146.4 Chloroform, reagent grade.146.5 Sample Cylinder Assembly (Fig. 1), consisting of:6.5.1 Sample Cylinders;15nickel, Monel, or tantalum (Note1), 400-mL capacity, double-ended, specially cleaned (Note 2).6
22、.5.2 Valves, having a packing resistant to liquid chlorine.166.5.3 Holder for a Septum, that can be easily assembled.17NOTE 1Carbon or stainless steel cylinders and fittings are not suitableas CHCl3is unstable in the presence of FeCl3and Cl2.NOTE 2A procedure for cleaning cylinders and valves, for u
23、se withliquid chlorine, is given in Appendix X2.6.6 Fittings, for transferring chlorine from one cylinder toanother.6.7 Syringe, 10 to 100-L, capable of holding liquid chlo-rine under pressure, with 26-gage disposable needle.NOTE 3Disposable needles are recommended because corrosion withpermanent ne
24、edles may cause problems.7. Hazards7.1 Chlorine is a corrosive and toxic material. A well-ventilated fume hood should be used to house all testequipment, except the gas chromatograph, when this product isanalyzed in the laboratory.7.2 The analysis should be attempted only by persons whoare thoroughl
25、y familiar with the handling of chlorine, and evenan experienced person should not work alone. The operatormust be provided with adequate eye protection and a respirator.Splashes of liquid chlorine destroy clothing and, if suchclothing is next to the skin, will produce irritations and burns.7.3 When
26、 sampling and working with chlorine out of doors,people downwind from such operation should be warned of thepossible release of chlorine vapors.8Porasil is a trademark of Waters Associates, Inc.9Kel-F is a registered trademark of 3M Company.10Chromosorb is a registered trademark of Imerys Minerals C
27、alifornia, Inc.11Halocarbon is a registered trademark of Halocarbon Products Corporation.12A 400-mL nickel cylinder filled with liquid chlorine weighs about 4000 g.13Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing
28、of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.14This reagent is used for calibration purposes only
29、.15If samples are to be shipped outside any plant, cylinders approved by the U.S.Department of Transportation must be used.16Packing made from Teflon, registered trademark of The Chemours Company,Viton, Kel-F, or equivalent have been found suitable for this purpose.17Swagelok, registered trademark o
30、f Swagelok Company, or equivalent fittingshave been found suitable for this purpose.FIG. 1 Sample Cylinder AssemblyE806 1727.4 It is recommended that means be available for disposalof excess chlorine in an environmentally safe and acceptablemanner. If chlorine cannot be disposed of in a chlorinecons
31、uming process, a chlorine absorption system should beprovided. When the analysis and sampling regimen requires aninitial purging of chlorine from a container, the purged chlorineshould be similarly handled. Purging to the atmosphere shouldbe avoided.7.5 In the event chlorine is inhaled, first aid sh
32、ould besummoned immediately and oxygen administered withoutdelay.8. Sampling8.1 Sampling from tank cars, barges, storage tanks, andlarge cylinders presents unique problems. Each facility,however, must be capable of delivering a liquid sample (notgas) for test. See Chlorine Institute Pamphlet No. 1.8
33、.2 Since the location of these larger facilities may not be atthe immediate site of analysis, sample collection in a suitablesecondary container is recommended to facilitate its safetransport to the laboratory for tests (DOT regulations may beapplicable).8.3 It is recommended that samples be collect
34、ed from thesefacilities in small-size cylinders, with cylinders and valvesfabricated of tantalum, Monel, or nickel (carbon or stainlesssteel are unsuitable), and capable of being negotiated in thelaboratory fume hood. Proper and safe sampling techniquesmust be followed. Do not allow the sample cylin
35、der to becomeliquid full. A good rule is that the weight of the chlorine in thecylinder should not be more than 125 % of the weight of thewater that the cylinder could contain. This rule is stated inaccordance with 49 CFR 173.9. Preparation of Standards for Calibration9.1 Prepare standards in liquid
36、 chlorine, so that matrixeffects of the chlorine on the gas chromatographic column anddetector are compensated.9.2 Method of AdditionsAdd CCl4and CHCl3to cylindercontaining liquid chlorine as follows:9.2.1 Obtain a supply cylinder of liquid chlorine that hasless than 10 ppm each of CCl4and CHCl3, an
37、d that contains atleast 5000 g of chlorine. Label this cylinder No. 1.9.2.2 Obtain a clean, evacuated, sample cylinder equippedwith a septum on one of the valves. Label this cylinder No. 2and weigh it to 6 1g.9.2.3 Connect cylinder No. 1 to cylinder No. 2 by means offittings (6.6) such that the liqu
38、id phase of chlorine can flowfrom 1 to 2. Open the valves between the cylinders and coolcylinder No. 2 with ice. Liquid chlorine will be transferredfrom cylinder No. 1 to cylinder No. 2. Close the valves whensufficient chlorine has been transferred. Disconnect the cylin-ders and weigh cylinder No. 2
39、 to 6 1 g to determine the weightof chlorine transferred. (WarningDo not allow cylinder No.2 to become liquid full. A good rule is that the weight ofchlorine in the cylinder should not be more than 125 % of theweight of water that the cylinder could contain.)9.2.4 Retain cylinder No. 1 to prepare fu
40、rther standards.9.2.5 Prepare an approximately 50/50 mix of CCl4andCHCl3and record amounts of each added. Calculate thevolume of this mixture needed to prepare one level of standardfor calibration, using a calculation similar to that given in 9.3.9.2.6 Fill the high-pressure syringe (6.7) with appro
41、xi-mately the volume of the CCl4/CHCl3mixture as calculated in9.3.3. Weigh the syringe plus liquid to 6 0.1 mg. Transfer theliquid mixture through the septum into the vapor space ofcylinder No. 2. Keep a finger tightly over the plunger toprevent blow out. Immediately remove and reweigh the syringeto
42、 6 0.1 mg. The difference between the two weights is thetotal weight of CCl4and CHCl3added.9.2.7 Shake cylinder No. 2 to assure complete solution ofthe CCl4and CHCl3in the chlorine.9.2.8 Calculate the added concentration of CCl4and CHCl3in the spiked standard as indicated in 9.4.9.2.9 Prepare at lea
43、st three standards containing three dif-ferent levels of CCl4and CHCl3, bracketing the expected level.Also, transfer some of the original chlorine into a samplecylinder without adding CCl4or CHCl3.9.2.10 The long term stability of the calibration standardshas not been evaluated.9.3 Example of amount
44、s of CCl4and CHCl3to be added toliquid chlorine to produce desired standard:9.3.1 Proposed mixture of CCl4and CHCl3(average densityabout 1.5 g/mL, or 1.5 mg/L)CCl447.55 gCHCl344.40 gTotal 91.95 g9.3.2 To prepare 500 g of chlorine with spiked levels of 20ppm each of CCl4and CHCl3(total of 40 g/g), th
45、e necessarygrams (W) of the CCl4/CHCl3mixture is as follows:W500540106(1)orW 5 0.020 g 5 20 mg (2)9.3.3 The necessary volume in L (V) is then:V 5Wdensity5201.55 13 L (3)9.4 Example of calculation of spiked amounts of CCl4andCHCl3added:9.4.1 The weight of mixture added is:Initial syringe weight with
46、13 L 17.6715gWeight of syringe after transfer 17.6529gCCl4/CHCl3added 0.0186g9.4.2 The weight of cylinder No. 2:Weight with chlorine 3575gWeight empty 3088gWeight of chlorine 487g9.4.3 Weight of CCl4added:0.0186!47.5591.955 0.0096 g (4)9.4.4 Concentration of CCl4in the spiked chlorine:0.0096487106!
47、5 19.7 g/g w/w! (5)E806 1739.4.5 Weight of CHCl3added:0.0186!44.4091.955 0.0090 g (6)9.4.6 Concentration of CHCl3in the spiked chlorine:0.0090487106! 5 18.5 g/g w/w! (7)10. Chromatographic Conditions10.1 ColumnNaCl on Porasil or equivalent:10.1.1 DetectorFlame ionization.10.1.2 Detector Temperature1
48、50C.10.1.3 Carrier GasNitrogen at 30 mL/min.10.1.4 Column TemperatureProgrammed, 60 to 200C at15C/min.10.1.5 Injector Temperature90C.10.2 ColumnKel F on Chromosorb or equivalent:10.2.1 DetectorFlame ionization.10.2.2 Detector Temperature150C.10.2.3 Carrier GasNitrogen at 30 mL/min.10.2.4 Column Temp
49、erature60C.10.2.5 Injector Temperature75C.10.3 ColumnHalocarbon on Chromosorb or equivalent:10.3.1 DetectorFlame ionization.10.3.2 Detector Temperature150C.10.3.3 Carrier GasNitrogen at 30 mL/min.10.3.4 Column Temperature55C.10.3.5 Injector Temperature90C.NOTE 4The conditions listed have produced acceptable results. Theseparameters serve only as a guide in optimizing conditions for the columnused.11. Preparation of Calibration Curve11.1 Obtaining Sample from Cylinders Containing Calibra-tion Standards:11.1.1 Invert the cylinder
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