1、Designation: D 3443 00 (Reapproved 2005)Standard Test Method forChloride in Trichlorotrifluoroethane1This standard is issued under the fixed designation D 3443; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the determination of c
3、hloride intrichlorotrifluoroethane and other halocarbons that are liquid atroom temperature.1.2 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 pract
4、ices 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 by titration with mercuric acetate solutionusing s-diphenylcarbazone as the indicator.3. Significance and Use3.1 This test met
5、hod determines ionizable chloride that canbe aqueously extracted from trichlorotrifluoroethane.3.2 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.
6、 Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise 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 g
7、rades 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 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean halide-free distilled water.5.3 s-Diphe
8、nylcarbazone 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 Standard Mercuric Acetate SolutionDilute 40 mL ofstock mercuric acetate solution, reagent 2, to 1000 mL andadjust the pH to 1.6 w
9、ith 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 of s-diphenylcarbazone solution. Titrate withstandard mercuric acetate solution to the faint purple end point.Then:mL NaCl 3 1.
10、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 water and dilute to 1000 mL. Pipet 25mL of this solution into a 1000-mL volumetric flask, dilute tovolume, and mix. One milli
11、litre 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. Dilute to 1000 mL and mix.1This test method is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and
12、Fire Extinguishing Agents and is the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 1, 2005. Published June 2005. Originallyapproved in 1975. Last previous edition approved in 2000 as D 3443 00.2Reagent Chemicals, American Chemical Society Specifications, A
13、mericanChemical 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., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (
14、USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 Tr
15、ansfer 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 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 t
16、he 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 drops of s-diphenylcarbazone solution and titratewith standard mercuric acetate solution to the pale purple endpoint.7. Calculation7.1 Calculate parts per
17、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 = factor for the solution (see 5.5.1),S = millilitres of sample, andG = specific gravity of the sample.8. Precision and Bias8.1 Repeatability (Single Analyst):
18、The standard deviationof results (each the average of triplicates 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 Repro
19、ducibility (Multilaboratory): The standard devia-tion of results (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. pp
20、m.9. Keywords9.1 CFC-113; chloride; trichlorotrifluoroethaneASTM 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 pa
21、tent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited ei
22、ther for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair
23、 hearing you shouldmake your views known to the ASTM Committee 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 or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 3443 00 (2005)2
