1、Designation: D3443 00 (Reapproved 2010)1Standard Test Method forChloride in Trichlorotrifluoroethane1This standard is issued under the fixed designation D3443; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1NOTEAdded research report information to Section 8 editoria
3、lly in September 2010.1. Scope1.1 This test method covers the determination of chloride intrichlorotrifluoroethane and other halocarbons that are liquid atroom temperature.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3
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. Summary of Test
5、Method2.1 This test method is based on the determination ofionizable chloride by titration with mercuric acetate solutionusing s-diphenylcarbazone as the indicator.3. Significance and Use3.1 This test method determines ionizable chloride that canbe aqueously extracted from trichlorotrifluoroethane.3
6、.2 This test method can be used to establish production andpurchasing specifications.4. Apparatus4.1 Separatory Funnels, two 250-mL, with polytetra-fluoroethylene stopcocks.4.2 Erlenmeyer Flask, 125-mL.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwi
7、se indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.2Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purit
8、y to permit its use without lessening theaccuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean halide-free distilled water.5.3 s-Diphenylcarbazone SolutionDissolve 0.5 g ofs-diphenylcarbazone, in 100 mL of methanol.5.4 Silver Nitr
9、ate SolutionDissolve 8.5 g of silver nitrate(AgNO3) in 500 mL of water.5.5 Standard Mercuric Acetate SolutionDilute 40 mL ofstock mercuric acetate solution, reagent 2, to 1000 mL andadjust the pH to 1.6 with nitric acid. Standardize as follows:5.5.1 Pipet 10.00 mL of standard sodium chloride solutio
10、ninto a 250-mL Erlenmeyer flask. Add 20 mL of chloride-freewater and 5 drops of s-diphenylcarbazone solution. Titrate withstandard mercuric acetate solution to the faint purple end point.Then:mL NaCl 3 1.000mL mercuric acetate5 F 5 g Cl/mL (1)whereF = factor for the mercuric acetate solution (see 7.
11、1).5.6 Standard Sodium Chloride SolutionDissolve 0.0660 gof sodium chloride in water and dilute to 1000 mL. Pipet 25mL of this solution into a 1000-mL volumetric flask, dilute tovolume, and mix. One millilitre of this solution contains 1.00g of chloride ion.1This test method is under the jurisdictio
12、n of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents and is the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 1, 2010. Published July 2010. Originally approvedin 1975. Last previous edition approved in 2005 as D3443 00(2005)
13、. DOI:10.1520/D3443-00R10E01.2Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., an
14、d the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.7 Stock Mercuric Acetate SolutionDissolve 1.6 g ofmercuric acetate in
15、500 mLof water containing 3.5 mLof nitricacid. Dilute to 1000 mL and mix.6. Procedure6.1 Wash all glassware with chloride-free water until 10 mLof the washings show no trace of turbidity when 1 mL of silvernitrate solution is added.6.2 Transfer 100 mL of the sample into a 250-mL separatoryfunnel, ad
16、d 25 mL of chloride-free water to the sample andshake for 1 min. Transfer the sample to a second 250-mLseparatory funnel and drain the water into a 125-mL Erlenm-eyer flask. Repeat the extraction once with another 25 mL ofwater. Combine the water extracts in the Erlenmeyer flask.6.3 Warm the water e
17、xtract to 60C to drive off anyremaining sample. Cool to room temperature.6.4 Add 5 drops of s-diphenylcarbazone solution and titratewith standard mercuric acetate solution to the pale purple endpoint.7. Calculation7.1 Calculate parts per million chloride as follows:Chloride, ppm 5 A 3 F!/S 3 G! (2)w
18、here:A = millilitres of mercuric acetate solution required for thetitration,F = factor for the solution (see 5.5.1),S = millilitres of sample, andG = specific gravity of the sample.8. Precision and Bias38.1 Repeatability (Single Analyst): The standard deviationof results (each the average of triplic
19、ates obtained by the sameanalyst on two different days) has been estimated to be 0.005wt. ppm at four degrees of freedom. Two such values should beconsidered suspect (95 % confidence level) if they differ bymore than 0.02 wt. ppm.8.2 Reproducibility (Multilaboratory): The standard devia-tion of resu
20、lts (each the average of triplicates in four differentlaboratories) has been estimated to be 0.06 wt. ppm at threedegrees of freedom. Two such values should be consideredsuspect (95 % confidence level) if they differ by more than 0.3wt. ppm.9. Keywords9.1 CFC-113; chloride; trichlorotrifluoroethaneA
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24、e 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 o
25、r at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting RR:D26-1000 and RR:D26-1010.D3443 00 (2010)12
