1、Designation: D4301 05 (Reapproved 2013)Standard Test Method forTotal Chlorine in Epoxy Resins and Compounds1This standard is issued under the fixed designation D4301; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、 revision. 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 describes a procedure for the determi-nation of total chlorine in epoxy resins and glycidyl ethers.1.2 Th
3、e 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, associated with its use. It is theresponsibility of the user of this standard to establish appro-pria
4、te safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD6440 Terminology Relating to Hydrocarbon ResinsE691 Practice for Condu
5、cting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Other Document:OSHA Regulations, 29 CFR paragraphs 1910.1000 and1910.120033. Terminology3.1 Definitions: For definitions of terms used in thisstandard, See Terminology D6440.4. Summary of Test Method4.1 The material, dissol
6、ved in dimethoxyethane (DME) orother suitable inert solvent, is reacted with sodium biphenyl toconvert bound organic chlorine to the water soluble chloride.The excess reagent is decomposed with isopropyl alcohol. Thechloride ion is then titrated potentiometrically with silvernitrate.5. Significance
7、and Use5.1 The presence of residual chlorine in epoxy resins isdeleterious to final product properties. This test method hasbeen found to be applicable to resins or ethers with chlorinecontents ranging from 50 ppm to 35 % by weight. Otherhalogen compounds react with the reagent but are distin-guishe
8、d from chlorine by the final potentiometric titration.Epoxy and other functional groups will consume reagent but donot affect the results.6. Apparatus6.1 Potentiograph.6.2 Beaker, of appropriate size.6.3 Buret, of appropriate size.6.4 Stirrer, magnetic or paddle.7. Reagents7.1 Purity of ReagentsReag
9、ent 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.4Other grades may beused, provided it is fi
10、rst ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Type II of Specification D1193.1This test metho
11、d is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.33 on Polymers and Resins.Current edition approved Nov. 1, 2013. Published November 2013. Originallyapproved in 1984. Last previous edition
12、approved in 2005 as D4301 05. DOI:10.1520/D4301-05R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3A suit
13、able mechanical holder is available from the Gardner Laboratory, Inc.,5521 Landy Lane, Washington, DC, Item 660.4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Socie
14、ty, 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. Unit
15、ed States17.3 Sodium Biphenyl Reagent5(in ether solution).NOTE 1Store in a refrigerator when not in use to prevent loss ofactivity.7.4 Nitric Acid (HNO3) (1 + 1), aqueous solution.7.5 1,2-Dimethoxyethane.7.6 Silver Nitrate (AgNo3), 0.1 and 0.01 N standardizedsolutions.7.7 Methyl Red Indicator (0.2 %
16、 alcohol solution), dissolve0.2 g of methyl red in 100 mL of methanol, ethanol, orisopropanol.7.8 Isopropyl Alcohol.8. Hazards8.1 Consult current OSHA Regulations, Suppliers MaterialSafety Data Sheets, and local regulations for all materials usedin this test method.9. Procedure9.1 Pipet 5 mL of 1,2-
17、dimethoxyethane into a clean, dry250-mL beaker. Add a weighed amount of sample. (If thematerial is anticipated to be low in total chlorine, use 0.40 g ofsample. For materials high in chlorine, weigh 0.1 to 0.2 g ofsample.) Gently swirl to dissolve.9.2 Add about 15 mL (one bottle) of sodium biphenylr
18、eagent and mix thoroughly. If the solution loses its dark blueor green color within 5 min, add another 15 mL of reagent.Allow to react for 5 min.9.3 Add 100 mL of isopropanol to decompose the excessreagent and to serve as the titrating medium. Add 3 to 5 dropsof methyl red solution and neutralize wi
19、th HNO3(1 + 1). Add5 to 8 drops of acid in excess; start the stirrer.9.4 Titrate the solution potentiometrically using standardAgNO3solution. (For low chlorine content, titrate with 0.01 NAgNO3and for high chlorine content use 0.10 N AgNO3). Thescale of the titration curve will depend on the instrum
20、ent usedbut should give a curve of the approximate scale of 0.25mL/cm and 30 mV/cm. The end point is selected as the middleof the steepest portion of the curve.NOTE 2It may be preferable to use the first or second derivative todetermine the end point providing appropriate equipment is available.9.5
21、Repeat the determination and also run a blank using allreagents but omitting the specimen.10. Calculation10.1 Calculate the weight percent of chlorine, C, as follows:C 5V 2 B! 3 N 33.546Swhere:V = titration of specimen, mL,B = titration of blank, mL,N = normality of AgNO3solution, andS = weight of s
22、pecimen, g.10.2 Calculate the mean of the two runs.11. Precision11.1 On the basis of an interlaboratory study, in accordancewith Specification E691, of this test method in which oneoperator in each of three laboratories analyzed in duplicate ontwo different days five materials containing 0.1 to 0.3
23、% totalchlorine, for a total of 60 determinations, the within-laboratorystandard deviation was found to be 5 % relative and thebetween-laboratories standard deviation 7 % relative. Based onthese standard deviations the following criteria should be usedfor judging the acceptability of results at the
24、95 % confidencelevel:11.2 RepeatabilityTwo results, each the mean of two runs,obtained by the same operator should be considered suspect ifthey differ by more than 13.9 % relative.11.3 ReproducibilityTwo results, each the mean of tworuns, obtained by operators in different laboratories should becons
25、idered suspect if they differ by more than 19.4 % relative.12. Keywords12.1 chlorine; glycidyl ethers; liquid epoxy resinsASTM 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 expre
26、ssly 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 is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised
27、, either reapproved 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 a
28、ttend. 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 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States
29、. 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). Permission rights to photocopy the standard may also be se
30、cured from the ASTM website (www.astm.org/COPYRIGHT/).5The sole source of supply of the reagent, (in small bottles (15-mL) known tothe committee at this time is Southwestern Analytical Chemicals, P. O. Box 485,Austin 63, TX. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend. It may also be prepared as described in Analytical Chemistry,Vol26, p. 748.D4301 05 (2013)2
