1、Designation: D3316 06 (Reapproved 2011)Standard Test Method forStability of Perchloroethylene with Copper1This standard is issued under the fixed designation D3316; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last r
2、evision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 The values stated in S
3、I 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, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health
4、 practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E200 Practice for Preparation, Standardization, and Storageof Standard and Reagent Solutions for Chemical Analysis3. Summary of Test Method3.1 Clean copper strips are subject
5、ed to the action of liquidand vapor phases of boiling perchloroethylene for 72 h in thepresence of light. Weight loss of copper strips and 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 certai
6、n grades of perchloroethylene used for dry-cleaning fabrics or degreasing metal parts.5. Apparatus5.1 Flask, 300-mL, 24/40 standard-taper 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 stan
7、dard-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 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
8、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.3Other grades may beused, provided it is first ascertained that the reagent is ofsu
9、fficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, 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.
10、 Cut threecopper strips, 20 by 75 mm. Immerse the strips in concentratedHCl until the surface is bright and free of tarnish. Scribeconsecutive 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
11、.6.5 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (HCl). Handle the concentrated HCl solution asindicated in the suppliers 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 ac
12、cordance withPractice E200.6.7 Phenolphthalein IndicatorDissolve5gofphenol-phthalein in 500 mL of 95 % ethanol, dilute to 1 L withdistilled water, and mix thoroughly.1This test method is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents and is
13、the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved Aug. 1, 2011. Published November 2011. Originallyapproved in 1974. Last previous edition approved in 2006 as D3316 06. DOI:10.1520/D3316-06R11.2For referenced ASTM standards, visit the ASTM website, www.astm.org
14、, orcontact ASTM Customer 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 t
15、esting 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.1Copyright ASTM International, 100 Barr Harbo
16、r Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Procedure7.1 Clean the flask and Soxhlet extractor with soap andwater. Should any residue be present, clean thoroughly withacid and rinse with water. Flush out the condenser with water.Rinse the flask, Soxhlet, and condenser wi
17、th 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 condenser. 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 thes
18、olvent 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 water (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 ofrel
19、easing pressure. Turn on the condenser cooling water andadjust the heat source so that the Soxhlet siphon cycle isbetween 8 and 10 min. Place the 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 apparatu
20、s 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-forming materials from the condenser and Soxhletinto the flask. Remove the flask, thoroughly shake, and transferthe contents to a 400-mL beaker. Titrate the aque
21、ous layerusing 0.01N NaOH solution to a phenolphthalein end point.Record the millilitres of NaOH required to reach the pink endFIG. 1 Copper Stability Apparatus for PerchloroethyleneD3316 06 (2011)2point. Wash the copper strips individually in concentrated HCluntil substantially free of all corroded
22、 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 0.01N NaOH solu-tion. Report loss in weight in milligrams, of the respectivecopper strips as “Flask loss,” “Soxhlet loss,” and“ Condenserloss.” Thi
23、s provides an indication of the quality of theperchloroethylene.9. Precision and Bias9.1 Results of duplicate determinations should not differmore than 20 % on acidity as millilitres of 0.01N NaOHsolution or on weight losses of copper strips in the respectivelocations.10. Keywords10.1 acidity; coppe
24、r; corrosion; dilute hydrochloric acid;dilute sodium hydroxide; indicator; perchloroethylene; weightlossASTM 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
25、determination of the validity of any such patent 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 reapprove
26、d or withdrawn. Your comments are invited either 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
27、 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 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual repri
28、nts (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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D3316 06 (2011)3
