1、Designation: D 3316 06Standard Test Method forStability of Perchloroethylene with Copper1This standard is issued under the fixed designation D 3316; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numbe
2、r in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the evaluation of the corrosive-ness to copper metal by perchloroethylene.1.2 This standard does not purport to add
3、ress 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. Referenced Documents2.1 ASTM Standards:2E 200 Practic
4、e for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysis3. Summary of Test Method3.1 Clean copper strips are subjected to the action of liquidand vapor phases of boiling perchloroethylene for 72 h in thepresence of light. Weight loss of copper strips an
5、d acidformation are determined at the end of the test period.4. Significance and Use4.1 This test method is to be used as a guide in selecting oreliminating certain grades of perchloroethylene used for dry-cleaning fabrics or degreasing metal parts.5. Apparatus5.1 Flask, 300-mL, 24/40 standard-taper
6、 joint.5.2 Soxhlet Extractor, 30-mm inside diameter, 24/40standard-taper bottom joint, 34/45 standard-taper upper joint.5.3 Allihn Condenser, bulb type, 34/45 standard-taper bot-tom joint.5.4 Bottle, wide-mouth, 8 oz.5.5 Funnel, 8-mm outside diameter stem, 35-mm diameteropening.5.6 Heater, variable
7、control.5.7 Light Bulb, 100 W.5.8 Beaker, 400 mL.5.9 Analytical Balance.6. Reagents and Materials6.1 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 Re
8、agents of the American Chemical Society,where such specifications are available.3Other 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.6.2 Purity of WaterUnless otherwise indicated
9、, referencesto water shall be understood to mean distilled water or water ofequal purity.6.3 Acetone, practical grade.6.4 Copper, electrolytic foil, 0.05 mm thick. Cut threecopper strips, 20 by 75 mm. Immerse the strips in concentratedHCl until the surface is bright and free of tarnish. Scribeconsec
10、utive identification numbers on the strips. Rinse thor-oughly in running water and dry with a towel. Weigh the stripsto the nearest 0.1 mg on an analytical balance.6.5 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (HCl). Handle the concentrated HCl solution asindicated in the supplie
11、rs direction.6.6 Sodium Hydroxide, Standard Solution (0.01 N 60.001)Dissolve 0.4 6 0.04 g of anhydrous sodium hydroxide(NaOH) in 1 L of water and standardize in accordance withPractice E 200.6.7 Phenolphthalein IndicatorDissolve5gofphenol-phthalein in 500 mL of 95 % ethanol, dilute to 1 L withdistil
12、led water, and mix thoroughly.7. Procedure7.1 Clean the flask and Soxhlet extractor with soap andwater. Should any residue be present, clean thoroughly with1This test method is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents and is the direct
13、responsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 1, 2006. Published June 2006. Originallyapproved in 1974 as D 3316 74 T. Last previous edition approved in 2000 asD 3316 96(2000).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM C
14、ustomer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents
15、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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C70
16、0, West Conshohocken, PA 19428-2959, United States.acid and rinse with water. Flush out the condenser with water.Rinse the flask, Soxhlet, and condenser with acetone and dryby means of a stream of filtered air.7.2 Place one of the strips in the flasks, one in the Soxhlet,and the third in the condens
17、er. Bend the condenser striplengthwise in the form of a U and force it into the condenser sothat approximately half of it is inside. Measure 100 mL of thesolvent into the flask and add 0.2 mL of water. Assemble theapparatus as shown in Fig. 1. Fill the wide-mouth bottleapproximately half full of wat
18、er (about 100 mL) and insert thefunnel so that it is less than14 in. from the water surface. Usea slotted cork to hold the funnel and provide a means ofreleasing pressure. Turn on the condenser cooling water andadjust the heat source so that the Soxhlet siphon cycle isbetween 8 and 10 min. Place the
19、 light bulb 1 in. from thevertical center of the Soxhlet sidearm vapor tube. Continuerefluxing for 72 h.7.3 Turn off the heat source and allow the apparatus to coolfor 15 min. By means of a funnel, pour the contents of thewide-mouth bottle into the top of the condenser. This will washany acid-formin
20、g materials from the condenser and Soxhletinto the flask. Remove the flask, thoroughly shake, and transferthe contents to a 400-mL beaker. Titrate the aqueous layerusing 0.01N NaOH solution to a phenolphthalein end point.Record the millilitres of NaOH required to reach the pink endpoint. Wash the co
21、pper strips individually in concentrated HClFIG. 1 Copper Stability Apparatus for PerchloroethyleneD3316062until substantially free of all corroded matter. Rinse withrunning water and dry thoroughly by wiping with a towel.Weigh to the nearest 0.1 mg.8. Report8.1 Report any acidity as millilitres of
22、0.01N NaOH solu-tion. Report loss in weight in milligrams, of the respectivecopper strips as “Flask loss,” “Soxhlet loss,” and“ Condenserloss.” This provides an indication of the quality of theperchloroethylene.9. Precision and Bias9.1 Results of duplicate determinations should not differmore than 2
23、0 % on acidity as millilitres of 0.01N NaOHsolution or on weight losses of copper strips in the respectivelocations.10. Keywords10.1 acidity; copper; corrosion; dilute hydrochloric acid;dilute sodium hydroxide; indicator; perchloroethylene; weightlossASTM International takes no position respecting t
24、he 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 patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard
25、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 either for revision of this standard or for additional standardsand should be addressed to ASTM International H
26、eadquarters. 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 hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This
27、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).D3316063
