1、Designation: D 1613 06Standard Test Method forAcidity in Volatile Solvents and Chemical IntermediatesUsed in Paint, Varnish, Lacquer, and Related Products1This standard is issued under the fixed designation D 1613; the number immediately following the designation indicates the year oforiginal adopti
2、on or, in the case of revision, the year of 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.This standard has been approved for use by agencies of the Department of Defense.1. S
3、cope*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 weight saturatedand
4、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 rounded off “t
5、othe 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 specific hazard in
6、formation 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 and determine
7、the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 770 Specification for Isopropyl AlcoholD 1193 Specification for Reagent WaterE 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysisE29
8、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 point.4. S
9、ignificance 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 contaminati
10、on,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 shall be use
11、d 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 the reagent
12、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 D 1193.7. Reagents7.1 Alcohols, refined, ethyl or isopropyl.1This test
13、 method is under the jurisdiction of ASTM Committee 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 April 1, 2006. Published April 2006. Originallyappro
14、ved in 1964. Last previous edition approved in 2003 as D 1613 03.2For 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 webs
15、ite.3Reagent Chemicals, 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 Pharma
16、copeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.NOTE 1Isopropyl alcohol (99 % gr
17、ade) conforming to SpecificationD 770, 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/L)Dissolve1 g of phenolphtha
18、lein 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 Solutions, Precision and Bias, Prepa
19、rationof 50 % of NaOH Solution and of Standard Solutions, andStandardization sections of Practice E 200.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 ofalcohol, if the sample is
20、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 perceptible pink colororigi
21、nally 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 environment has this level ofCO2o
22、r 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 VN3 0.12!/D (1)or,Acidity as mg KOH per g of sample 5 VN 3 1.12!/D (2)where:V = NaOH solution require
23、d 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 % confidence level).11. Precision and
24、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 different days, is estimated to
25、 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 estimated to be 0.0005 %,absolute
26、. 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, 0.0007, 0.0046, 0.0026, and
27、0.0067 % 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 384 determina-tions.11.2 B
28、iasThe 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 to this standard since the
29、last issue(D 1613 - 03) that may impact the use of this standard.(1) Added Note 3 after 8.3.4Supporting data are available from ASTM International Headquarters. RequestRR: D01-1041.D1613062ASTM International takes no position respecting the validity of any patent rights asserted in connection with a
30、ny 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.This standard is subject to revision at any time by the responsible technica
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32、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 below.This standard is copyrighted by ASTM International, 100 Barr Harbor
33、 Drive, PO Box C700, West Conshohocken, PA 19428-2959,United 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).D1613063
