Desi gnat i on:D2613±01
St a nda r dT e stMe t hodf orCa l c i um orZi nci nPa i ntDr i e r sby 1
EDTAMet hod
This standard is issued under the ®xed designation D 2613; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon ( e) indicates an editorial change since the last revision or reapproval.
5. Apparatus 1. Scope
6. Reagents
capablee 5.1 Centrifuge, capabl
This test test method method covers covers a titri titrimet metric ric 1.1 This
of developing 1000 to 2000 g.
deter determin minati ation on of calciu calcium m in liquid liquid calciu calcium m driers and zinc in liquid zinc driers that can be dissol dissolved ved in a toluen toluene-a e-alco lcohol hol mixtur mixturee and utilizes the disodium salt of 1 This test method is under the ethyle ethylened nedia iamin minete etetra traace acetic tic acid acid dihydr dihydrate ate jurisdiction jurisdiction of ASTM Committee Committee D01 on Paint and Related Coatings, (EDTA).
Materials, and Applications and is dire direct ct resp respon onsi sibi bili lity ty of Subcommittee D01.21 on Chemical blends. Anal Analys ysis is of Pain Paints ts and and Pain Paintt All cati cation onss that that can can be titr titrat ated ed with with Materials. 1.3 All Current edition edition approved approved Jan. Jan. EDTA in alkaline media interfere and must not Current 10, 2001. 2001. Published Published March 2001. 2001. be present in the sample. Originally published as D 2613 ± This stan standa dard rd does does not not purp purpor ortt to 67 T. Last previous edition D 2613 1.4 This (1994)e1. Book addr addres esss all all of the the safe safety ty conc concer erns ns,, if any, any, ± 852 Annual of ASTM
1.2 This test method is not applicable to drier the the
Standards, Vol 06.04.
associated with its use. It is the responsibility of 3 Annual of Standards,Book Vol 11.01. the user of this standard to establish appro priate safety and health practices and Annual Book of determ determine ine the applic applica-b a-bili ility ty of regula regulator toryy 4Standards, Vol 15.05. limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards:
D 600 Speci®cation for 2 Liquid Paint Driers D 1193 Speci®cation for Reagent 3 Water E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of 4 Industrial Chemicals E 300 Practice for Sampling Industrial Industrial 4 Chemicals 3. Summary of Test Method
The liqu liquid id calc calciu ium m or zinc zinc drie drierr is 3.1 The dissol dissolved ved in toluen toluenee and ethyl ethyl alcoho alcoholl and trea treate ted d with with an exce excess ss of stan standa dard rd EDTA EDTA solution. The excess is titrated with a standard zinc chloride solution using Eriochrome BlackT as the indicator. 4. Signi®cance and Use 4.1 This test method may be used to con ®rm
the stated calcium or zinc content of pure liquid calc calciu ium m or zinc zinc drie driers rs solu solubl blee in tolu toluen eneealco alcoho holl and and manu manufa fact ctur ured ed for for use use by the the coatings industry.
ASTM
ASTM
6.1 Purity
of ReagentsÐReagen Reagentt grade grade chemicals shall be used in all tests. Unless otherwise indica indicated ted,, it is intend intended ed that that all all reag reagen ents ts shal shalll conform to the speci®cations of the Commit-tee on Analytical Reagents of the American Chemical Chemical Society, Society, where such such spec specii®cati cation onss are are 5 available. Other Other grades grades may be used, provided it is ascertain ained ed that that the ®rst ascert reagent reagent is of sufficie sufficiently ntly high high purity purity to permit permit its use without without lessening lessening the accuracy of the determination. of 6.2 Purity Unless otherw otherwise ise Water ÐUnless indicate indicated, d, reference referencess to water shall be understood to mean mean reag reagen entt wate waterr conforming to Type II of Speci®cation D 1193. 6.3 Buffer SolutionÐAdd 350 mL of concentra concentrated ted ammo-nium ammo-nium hydroxide (NH 4OH, sp gr 0.90) to 54 g of ammonium chloride (NH4Cl) and dilute to 1 L with water. Standard 6.4 EDTA, Solution (0.05 M)Ð Weigh 18.62 g of EDTA, of EDTA, dissolve in water and dilute to 1 L. Store in a polyethylene or borosilicate glass bottle. 6.5 Indicator MixtureÐTriturate 0.2 g of Eriochrome BlackBlack-T T and 100 g of sodium chloride (NaCl) and store the mixture in a tightly stop stoppe pere red d bott bottle le.. This This mixture remains stable for several years.
6.6 Zinc Chloride, Standard Solution (0.05
NOTE 1ÐLiquid driers are M)ÐWeigh 3.2690 g of zinc metal to 0.5 mg normally homogeneous so that and dissolve in 50 mL of dilute hydrochloric only simple physical tests, such acid (14 mL of concentrated HCl (sp gr 1.42) to as speci®c gravity or solids 36 mL of water). Warm if necessary. Dilute to 1 content, on top and bottom samples from tanks, are L in a volumetric ¯ask. requ ired t o co n®rm that separation has not occurred. 7. Sampling Agitate drums in accordance 7.1 Take a small sample of liquid drier from with the section on Tube bulk using the procedures in Practice E 300Sampling of Practice E 300.
appropriate for the size of the container: Section 19 for tanks and tank cars or Section 23 for drums and cans.
7.2 Examine the sample of drier for sediment or
suspended 5
Reagent Chemicals, American Chemical Society Speci®cations, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, Analar Standards for see Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Co p y r i g h t©AS TM,1 0 0Ba r r Co n s h o ho c k e n ,P A1 94 2 8 2 9 5 9 , Ha r b o rD r i v e ,We s t Un i t e dSt a t e s .
1
D matter which if present is evidence of noncompliance with Speci®cation D 600.
EDTA solution into each beaker. Add 15 mL of buffer solution and 0.20 g of the indicator mixture (more or less can be added, if desired). Mix thoroughly by swirling. Titrate with the standard ZnCl 2 solution to the ®rst permanent tinge of red. Maintain vigorous swirling during the titration to ensure thorough mixing of the two phases which may appear.
7.3 If the sample is homogeneous keep it in a stoppered vessel to prevent solvent evaporation prior to analysis. 8. Standardization
2613
8.1 Zinc Chloride Standard Solution (0.05 M)ÐCalculate the exact molarity, M 1, of the solution as follows: M 1 5 S 1 /65.37
(1)
where: = zinc used, g, and 65.37 = zinc to produce a 1 M solution, g/L. 8.2 EDTA, Standard Solution (0.05 M)Ð Measure 40.0 mL of the EDTA solution into a 250-mL ¯ask that contains 10 mL of toluene and 100 mL of 95 % ethyl alcohol pure or denatured. Add 15 mL of buffer solution, 0.2 g of indicator mixture, and mix thoroughly. Titrate with the standard zinc solution to the ®rst permanent appearance of a red color. 9. Procedure 8.2.1 Calculate the molarity of the EDTA solution, M 2, as follows:
NOTE 2ÐIf a magnetic stirrer is available, it is convenient to titrate in an ordinary beaker. Stirring magnetically ensures thorough mixing during the titration. NOTE 3ÐIf the end point is overstepped, add 1.0 mL of the EDTA solution to the mixture and titrate again with standard ZnCl 2 solution. Use total volume of each solution for the calculation.
S1
M 2 5 ~V 1 3 M 1! /40.0
(2)
where: V1
40.0
= ZnCl2 solution, mL, =EDTA solution titrated, mL.
9.1 Check the clarity of the drier. If not clear, centrifuge a portion of the sample until it is clear. Keep the centrifuge tube stoppered so that the solvent will not evaporate. 9.2 From a buret place a few grams of the drier in a 50-mL Erlenmeyer ¯ask that is ®tted with a cork through which passes a dropping tube and rubber bulb or eye dropper and obtain the total 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-mL assay beakers or wide-mouth ¯asks (Note 2). Add 10 mL of toluene to each specimen and swirl to mix. Add 100 mL of 95 % ethyl alcohol and swirl again until the specimen is dissolved and well dispersed. From a buret measure 40.0 mL of
10. Calculation 10.1 Calculate the percent of Ca, A, or Zn, B, as follows:
where: V2 = = V 3 S = 4.01 = 6.54 =
A 5 @@~V 2 M 2! 2 ~V 3 M 1!# 4.01# / S
(3)
B 5 @@~V 2 M 2! 2 ~V 3 M 1!# 6.54# / S
(4)
EDTA solution, mL, ZnCl2 solution required for specimen, mL, specimen used, g, millimolar weight of Ca 3 100, and millimolar weight of Zn 3 100.
11. Precision and Bias (see Practice E 180) 11.1 Precision: 11.1.1 RepeatabilityÐTwo results, each the mean of duplicate determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 0.05 % calcium or zinc. 11.1.2 ReproducibilityÐTwo results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 0.10 % calcium or zinc. 11.2 BiasÐBias cannot be determined because there are no accepted standards for calcium and zinc in paint driers. 12. Keywords 12.1 calcium; drier analysis; EDTA analysis; zinc
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