1、Designation: D1613 06 (Reapproved 2012)Standard Test Method forAcidity in Volatile Solvents and Chemical IntermediatesUsed in Paint, Varnish, Lacquer, and Related Products1This standard is issued under the fixed designation D1613; the number immediately following the designation indicates the year o
2、foriginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department
3、of Defense.1. Scope*1.1 This test method covers the determination of totalacidity as acetic acid, in concentrations below 0.05 %, inorganic compounds and hydrocarbon mixtures used in paint,varnish, and lacquer solvents and diluents. It is known to beapplicable to such mixtures as low molecular weigh
4、t saturatedand unsaturated alcohols, ketones, ethers, esters, hydrocarbondiluents, naphtha, and other light distillate petroleum fractions.1.2 For purposes of determining conformance of an ob-served value or a calculated value using this test method torelevant specifications, test result(s) shall be
5、 rounded off “tothe nearest unit” in the last right-hand digit used in expressingthe specification limit, in accordance with the rounding-offmethod of Practice E29.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 For spe
6、cific hazard information and guidance consultsuppliers Material Safety Data Sheet.1.5 This standard does not purport to address the safetyconcerns, if any, associated with its use. It is the responsibilityof whoever uses this standard to consult and establish appro-priate safety and health practices
7、 and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D770 Specification for Isopropyl AlcoholD1193 Specification for Reagent WaterE200 Practice for Preparation, Standardization, and Storageof Standard and Reagent Solutions for Chemical A
8、nalysisE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications3. Summary of Test Method3.1 The specimen is mixed with either an equal volume ofwater or an equal volume of alcohol, and titrated with aqueoussodium hydroxide solution to the phenolphthalein end
9、 point.4. Significance and Use4.1 This test method is useful for determining low levels ofacidity, below 0.05 %, in organic compounds and hydrocarbonmixtures. The total acidity is calculated as acetic acid ormilligrams of sodium hydroxide per gram of sample.4.2 Acidity may be present as a result of
10、contamination,decomposition during storage or distribution, or manufacture.This test method may be used in assessing compliance with aspecification.5. Apparatus5.1 Buret, 10-mL, graduated in 0.05-mL subdivisions.5.2 Erlenmeyer Flask, 250-mL capacity.6. Purity of Reagents6.1 Reagent grade chemicals s
11、hall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.3Other grades may be used pro-vided it is first ascertained that t
12、he reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to Type IV ofSpecification D1193.1This test method is under the jurisdiction of ASTM C
13、ommittee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved June 1, 2012. Published July 2012. Originally approvedin 1964. Last previous edition approved i
14、n 2006 as D1613 06. DOI: 10.1520/D1613-06R12.2For 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 Chemica
15、ls, American Chemical 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 F
16、ormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17. Reagents7.1 Alcohols, refined, ethyl or isopropyl.N
17、OTE 1Isopropyl alcohol (99 % grade) conforming to SpecificationD770, or 190 proof ethyl alcohol conforming to formula No. 3A of theU.S. Bureau of Alcohol, Tobacco and Firearms is suitable for use as thesolvent. The use of methyl alcohol is not recommended.7.2 Phenolphthalein Indicator Solution (10 g
18、/L)Dissolve1 g of phenolphthalein in ethyl or isopropyl alcohol (see Note1) and dilute to 100 mL with the alcohol.7.3 Sodium Hydroxide, Standard Solution (0.05 N)Prepare and standardize a 0.05 N sodium hydroxide (NaOH)solution (Note 2) in accordance with the Preparation andStandardization of Solutio
19、ns, Precision and Bias, Preparationof 50 % of NaOH Solution and of Standard Solutions, andStandardization sections of Practice E200.NOTE 2Alternatively, KOH solution may be used.8. Procedure8.1 Measure into a 250-mL Erlenmeyer flask 50 mL ofwater, if the sample is completely water-soluble, or 50 mL
20、ofalcohol, if the sample is not completely water-soluble.8.2 Add 0.5 mL of phenolphthalein indicator solution.Titrate the water or alcohol with 0.05 N NaOH solution to thefirst perceptible pink color.8.3 Pipet 50 mL of the sample into the flask. Titrate with the0.05 N NaOH solution to the same first
21、 perceptible pink colororiginally obtained.NOTE 3It has been observed that in CO2-rich laboratory environmentsuch as those in an ethanol from corn manufacturing facility, 0.5 % CO2level or greater can cause a positive interference (higher results) whenusing this test method. If your laboratory envir
22、onment has this level ofCO2or greater, it is recommended that proper precaution(s) should betaken to minimize CO2interference.9. Calculations9.1 Calculate the acidity of the sample as follows:Acidity as acetic acid, weight% 5 VN 30.12!/D (1)or,Acidity as mg KOH per g of sample 5 VN 31.12!/D (2)where
23、:V = NaOH solution required for titration of the sample, mL,N = normality of the NaOH solution, andD = density of specimen in g/mL.10. Report10.1 Report the percent of acetic acid to the nearest0.0001 %. Duplicate runs that agree within 0.0005 %, absolute,are acceptable for averaging (95 % confidenc
24、e level).11. Precision and Bias411.1 Precision:11.1.1 The following criteria should be used for judging theacceptability of results at the 95 % confidence level:11.1.1.1 RepeatabilityThe normal range between two re-sults, each the mean of duplicate determinations, obtained bythe same analyst on diff
25、erent days, is estimated to be 0.0003 %,absolute. Two such values should be considered suspect if theydiffer by more than 0.0008 %, absolute.11.1.1.2 ReproducibilityThe normal range between tworesults, each the mean of duplicate determinations obtained byanalysts in different laboratories, is estima
26、ted to be 0.0005 %,absolute. Two such values should be considered suspect if theydiffer by more than 0.0014 %, absolute.NOTE 4The above precision estimates are based on an interlaboratorystudy on two samples each of n-butyl acetate, n-butyl alcohol, and methylethyl ketone containing 0.0058, 0.0112,
27、0.0007, 0.0046, 0.0026, and0.0067 % acetic acid, respectively. Each of four laboratories analyzed allsix samples, with two analysts in each laboratory performing duplicatedeterminations using both 99 % isopropyl alcohol and formula 3A ethanolas solvents, and repeating on a second day, for a total of
28、 384 determina-tions.11.2 BiasThe bias of this test method has not beendetermined because there is no available material with anaccepted reference value.12. Keywords12.1 acidity; solvents; total acidity as acetic acidSUMMARY OF CHANGESCommittee D01.35 has identified the location of selected changes
29、to this standard since the last issue(D1613 - 03) that may impact the use of this standard.(1) Added Note 3 after 8.3.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1041.D1613 06 (2012)2ASTM International takes no position
30、respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.Th
31、is standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM Int
32、ernational Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you 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
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