1、Designation: D2613 01 (Reapproved 2012)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.2. Referenced Documents2.1 ASTM Standards:2D600 Specification for Liquid Paint DriersD1193 Specification for Reagent WaterE180 Practice for Determining the Precision of ASTMMethods for Analysis a
6、nd Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)3E300 Practice for Sampling Industrial Chemicals3.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 excess is titrated with a
7、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 industry.5. Apparatus5
8、.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 the American Chemical So
9、ciety,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, referencesto water shall be unde
10、rstood 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 ofEDTA, dissolve in water
11、and dilute to 1 L. Store in apolyethylene or borosilicate glass bottle.6.5 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 remainsstable for several years.6.6 Zinc Chloride, Standard Solution (
12、0.05 M)Weigh3.2690 g of zinc metal to 0.5 mg and dissolve in 50 mL of1This 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 Paints and Paint Materials.Cu
13、rrent edition approved June 1, 2012. Published July 2012. Originally approvedin 1967. Last previous edition approved in 2006 as D2613 01 (2006). DOI:10.1520/D2613-01R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annua
14、l 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 Society, Washington, DC. For
15、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.Copyright ASTM Internatio
16、nal, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1dilute 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 sample of liquid drier from bulk using thepro
17、cedures 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 top and bottomsamples from tanks, are r
18、equired 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 D600.7.3 If the sample is homogeneous keep
19、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 produce a 1 M solution, g/L.8.2 EDTA, Standard
20、 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 zinc solution to thefirst permanent appeara
21、nce 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 until it is clear. Keep the centrifuge
22、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 difference two or three 1-g specimens(10
23、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. From a buret measure 40.0 mLofEDTA solution
24、 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 the titration to ensurethorough mixing o
25、f 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 EDTAsolution to the mixture and titrate again with
26、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 required for specimen, mL,S = specimen used, g,
27、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 should be considered suspect if they differ b
28、y 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 cannot be determined because there are noacce
29、pted standards for calcium and zinc in paint driers.12. Keywords12.1 calcium; drier analysis; EDTA analysis; zincD2613 01 (2012)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard ar
30、e 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 is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not
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32、u 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 standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United
33、 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D2613 01 (2012)3
