1、Designation: D3443 00 (Reapproved 2015)Standard 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 revisio
2、n. 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 U.S. Department of Defense.1. Scope1.1 This test method covers the determination of
3、 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 This standard does not purport to address all of thesafety concerns, if any, a
4、ssociated 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 Method2.1 This test method is based on the determination ofionizable chloride
5、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.3.2 This test method can be used to establish production andpurchasing specific
6、ations.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 otherwise indicated, it is intended thatall reagents shall conform to the specificati
7、ons 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 purity to permit its use without lessening theaccuracy of the determination.5.2 Pur
8、ity 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 Nitrate SolutionDissolve 8.5 g of silver nitrate(AgNO3) in 500 mL of water.5.5 Sta
9、ndard 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 solutioninto a 250-mL Erlenmeyer flask. Add 20 mL of chloride-freewater and 5 drops o
10、f s-diphenylcarbazone solution. Titrate withstandard mercuric acetate solution to the faint purple end point.Then:mL NaCl 31.000mL mercuric acetate5 F 5 g Cl/mL (1)whereF = factor for the mercuric acetate solution (see 7.1).5.6 Standard Sodium Chloride SolutionDissolve 0.0660 gof sodium chloride in
11、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.5.7 Stock Mercuric Acetate SolutionDissolve 1.6 g ofmercuric acetate in 500 mLof water containing 3.5 mLof nitricacid. Di
12、lute to 1000 mL and mix.1This test method is under the jurisdiction 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, 2015. Published June 2015. Originallyapproved
13、 in 1975. Last previous edition approved in 2010 as D3443 00(2010)1.DOI: 10.1520/D3443-00R15.2Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Stand
14、ards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Procedu
15、re6.1 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, add 25 mL of chloride-free water to the sample andshake for 1 min. Transfer the sampl
16、e to a second 250-mLseparatory funnel and drain the water into a 125-mL Erlen-meyer flask. Repeat the extraction once with another 25 mL ofwater. Combine the water extracts in the Erlenmeyer flask.6.3 Warm the water extract to 60C to drive off anyremaining sample. Cool to room temperature.6.4 Add 5
17、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)where:A = millilitres of mercuric acetate solution required for thetitration,F = fac
18、tor 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 triplicates obtained by the sameanalyst on two different days) has been estimated to be 0.
19、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 results (each the average of triplicates in four differentlaboratories) has been estima
20、ted 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; trichlorotrifluoroethaneASTM International takes no position respecting the validity of any patent rights as
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23、eive careful consideration at a meeting of 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 Int
24、ernational, 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 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or thro
25、ugh the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Reports RR:D26-1000 and RR:D26-1010.D3443 00 (2015)2
