ASTM D2613-2001(2006) Standard Test Method for Calcium or Zinc in Paint Driers by EDTA Method《EDTA法测定涂料催干剂中钙或锌的标准试验方法》.pdf

1、Designation: D 2613 01 (Reapproved 2006)Standard Test Method forCalcium or Zinc in Paint Driers by EDTA Method1This standard is issued under the fixed designation D 2613; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of

2、last revision. A number 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 a titrimetric determination ofcalcium in liquid calcium driers and zinc in liquid zinc driers

3、that 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

5、-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 600 Specification for Liquid Paint DriersD 1193 Specification for Reagent WaterE 180 Practice for Determining the Precision of ASTMMethods for Anal

6、ysis and Testing of Industrial and Spe-cialty ChemicalsE 300 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 standard zi

7、nc 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. Apparatus5.1 Centrifu

8、ge, 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 Society,where

9、 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, referencesto water shall be understood to m

10、ean reagent water conformingto Type II of Specification D 1193.6.3 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 and dilut

11、e 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.1This test method is under the jurisdiction of

12、ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved June 1, 2006. Published June 2006. Originallyapproved in 1967. Last previous edition approve

13、d in 2001 as D 2613 01.2For 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.3Reagent Chemicals, American Chemical

14、Society Specifications, AmericanChemical Society, 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. Pharmac

15、opeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 o

16、f 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 theprocedures in Practice E 300 appropriate for the size of thecontainer: Section 19 for tanks and tank cars or Section 23 fordr

17、ums 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 required to confirm that separation has notoccurred. Agitate drums in accordance with the section on Tube Samplingof Pract

18、ice E 300.7.2 Examine the sample of drier for sediment or suspendedmatter which if present is evidence of noncompliance withSpecification D 600.7.3 If the sample is homogeneous keep it in a stopperedvessel to prevent solvent evaporation prior to analysis.8. Standardization8.1 Zinc Chloride Standard

19、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 Solution (0.05 M) Measure 40.0 mLof the EDTA solution into a 250-mL flask that contains 10 mLof toluene and 100 mLof

20、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 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= ZnCl

21、2solution, 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 tubestoppered so that the solvent will not evaporate.9.2 From a buret place a few grams of the drier in a 50-mLErlenm

22、eyer 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 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 ofto

23、luene 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 mL ofEDTA solution into each beaker. Add 15 mL of buffer solutionand 0.20 g of the indicator mixture (more or less can be added,if des

24、ired). Mix thoroughly by swirling. Titrate with thestandard ZnCl2solution to the first permanent tinge of red.Maintain vigorous swirling during 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 ordinar

25、y 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 standard ZnCl2solution. Usetotal volume of each solution for the calculation.10. Calculation10.1 Calculate the perce

26、nt 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,4.01 = millimolar weight of Ca 3 100, and6.54 = millimolar weight of Zn 3 100.11. Precision and Bias (see Practice E 1

27、80)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 by more than0.05 % calcium or zinc.11.1.2 ReproducibilityTwo results, each the mean of du-plicate determinations,

28、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 noaccepted standards for calcium and zinc in paint driers.12. Keywords12.1 calcium; drier analysis; EDTA analysis; zinc

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