1、Designation: D2613 01 (Reapproved 2017)Standard Test Method forCalcium or Zinc in Paint Driers by EDTA Method1This standard is issued under the fixed designation D2613; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st 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 covers a titrimetric determination ofcalcium in liquid calcium driers and zinc in liquid zinc drierstha
3、t can be dissolved in a toluene-alcohol mixture and utilizesthe disodium salt of ethylenediaminetetraacetic acid dihydrate(EDTA).1.2 This test method is not applicable to drier blends.1.3 All cations that can be titrated with EDTA in alkalinemedia interfere and must not be present in the sample.1.4
4、The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 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-pr
5、iate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of Interna
6、tional Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D600 Specification for Liquid Paint DriersD1193 Specification for Reagent WaterE180 Practice for Determining the Precision of AST
7、MMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)3E300 Practice for Sampling Industrial Chemicals3. Summary of Test Method3.1 The liquid calcium or zinc drier is dissolved in tolueneand ethyl alcohol and treated with an excess of standard EDTAsolution. The exc
8、ess is titrated with a standard zinc chloridesolution using Eriochrome Black-T as the indicator.4. Significance and Use4.1 This test method may be used to confirm the statedcalcium or zinc content of pure liquid calcium or zinc drierssoluble in toluene-alcohol and manufactured for use by thecoatings
9、 industry.5. Apparatus5.1 Centrifuge, capable of developing 1000 to 2000 g.6. Reagents6.1 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 t
10、he American Chemical Society,where such specifications are available.4Other 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, reference
11、sto water shall be understood to mean reagent water conformingto Type II of Specification D1193.6.3 Buffer SolutionAdd 350 mL of concentrated ammo-nium hydroxide (NH4OH, sp gr 0.90) to 54 g of ammoniumchloride (NH4Cl) and dilute to 1 L with water.6.4 EDTA, Standard Solution (0.05 M)Weigh 18.62 g ofE
12、DTA, dissolve in water and dilute to 1 L. Store in apolyethylene or borosilicate glass bottle.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, andApplications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Pain
13、ts and Paint Materials.Current edition approved July 1, 2017. Published July 2017. Originally approvedin 1967. Last previous edition approved in 2012 as D2613 01 (2012). DOI:10.1520/D2613-01R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at s
14、erviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Soci
15、ety, 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. (USPC), Rockville,MD.
16、Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of Inter
17、national Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.16.5 Indicator MixtureTriturate 0.2 g of EriochromeBlack-T and 100 g of sodium chloride (NaCl) and store themixture in a tightly stoppered bottle. This mixture remainssta
18、ble for several years.6.6 Zinc Chloride, Standard Solution (0.05 M)Weigh3.2690 g of zinc metal to 0.5 mg and dissolve in 50 mL ofdilute hydrochloric acid (14 mL of concentrated HCl (sp gr1.42) to 36 mL of water). Warm if necessary. Dilute to 1 L ina volumetric flask.7. Sampling7.1 Take a small sampl
19、e of liquid drier from bulk using theprocedures in Practice E300 appropriate for the size of thecontainer: Section 19 for tanks and tank cars or Section 23 fordrums and cans.NOTE 1Liquid driers are normally homogeneous so that only simplephysical tests, such as specific gravity or solids content, on
20、 top and bottomsamples from tanks, are required to confirm that separation has notoccurred.Agitate drums in accordance with the section on Tube Samplingof Practice E300.7.2 Examine the sample of drier for sediment or suspendedmatter which if present is evidence of noncompliance withSpecification D60
21、0.7.3 If the sample is homogeneous keep it in a stopperedvessel to prevent solvent evaporation prior to analysis.8. Standardization8.1 Zinc Chloride Standard Solution (0.05 M)Calculatethe exact molarity, M1, of the solution as follows:M15 S1/65.37 (1)where:S1= zinc used, g, and65.37 = zinc to produc
22、e a 1 M solution, g/L.8.2 EDTA, Standard Solution (0.05 M)Measure 40.0 mLof the EDTA solution into a 250-mL flask that contains 10 mLof toluene and 100 mLof 95 % ethyl alcohol pure or denatured.Add 15 mL of buffer solution, 0.2 g of indicator mixture, andmix thoroughly. Titrate with the standard zin
23、c solution to thefirst permanent appearance of a red color.8.2.1 Calculate the molarity of the EDTA solution, M2,asfollows:M25 V13 M1!/40.0 (2)where:V1= ZnCl2solution, mL,40.0 = EDTA solution titrated, mL.9. Procedure9.1 Check the clarity of the drier. If not clear, centrifuge aportion of the sample
24、 until it is clear. Keep the centrifuge tubestoppered so that the solvent will not evaporate.9.2 From a buret place a few grams of the drier in a 50-mLErlenmeyer flask that is fitted with a cork through which passesa dropping tube and rubber bulb or eye dropper and obtain thetotal weight. Weigh by d
25、ifference two or three 1-g specimens(10 drops weigh about 0.2 g) to the nearest 0.5 mg into 400-mLassay beakers or wide-mouth flasks (Note 2). Add 10 mL oftoluene to each specimen and swirl to mix. Add 100 mL of95 % ethyl alcohol and swirl again until the specimen isdissolved and well dispersed. Fro
26、m a buret measure 40.0 mLofEDTA solution into each beaker. Add 15 mL of buffer solutionand 0.20 g of the indicator mixture (more or less can be added,if desired). Mix thoroughly by swirling. Titrate with thestandard ZnCl2solution to the first permanent tinge of red.Maintain vigorous swirling during
27、the titration to ensurethorough mixing of the two phases which may appear.NOTE 2If a magnetic stirrer is available, it is convenient to titrate inan ordinary beaker. Stirring magnetically ensures thorough mixing duringthe titration.NOTE 3If the end point is overstepped, add 1.0 mL of the EDTAsolutio
28、n to the mixture and titrate again with standard ZnCl2solution. Usetotal volume of each solution for the calculation.10. Calculation10.1 Calculate the percent of Ca, A,orZn,B, as follows:A 5 V2M2! 2 V3M1!# 4.01#/S (3)B 5 V2M2! 2 V3M1!# 6.54#/S (4)where:V2= EDTA solution, mL,V3= ZnCl2solution require
29、d for specimen, mL,S = specimen used, g,4.01 = millimolar weight of Ca 100, and6.54 = millimolar weight of Zn 100.11. Precision and Bias (see Practice E180)11.1 Precision:11.1.1 RepeatabilityTwo results, each the mean of dupli-cate determinations, obtained by the same operator on differentdays shoul
30、d be considered suspect if they differ by more than0.05 % calcium or zinc.11.1.2 ReproducibilityTwo results, each the mean of du-plicate determinations, obtained by operators in different labo-ratories should be considered suspect if they differ by morethan 0.10 % calcium or zinc.11.2 BiasBias canno
31、t be determined because there are noaccepted standards for calcium and zinc in paint driers.12. Keywords12.1 calcium; drier analysis; EDTA analysis; zincD2613 01 (2017)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin
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