1、Designation: D1613 06 (Reapproved 2012)D1613 17Standard 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 th
2、e year oforiginal 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 U.S
3、. Department of Defense.1. Scope*1.1 This test method covers the determination of total acidity as acetic acid, in concentrations below 0.05 %, in organiccompounds and hydrocarbon mixtures used in paint, varnish, and lacquer solvents and diluents. It is known to be applicable to suchmixtures as low
4、molecular weight saturated and unsaturated alcohols, ketones, ethers, esters, hydrocarbon diluents, naphtha, andother light distillate petroleum fractions.1.2 For purposes of determining conformance of an observed value or a calculated value using this test method to relevantspecifications, test res
5、ult(s) shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing the specificationlimit, in accordance with the rounding-off method of Practice E29.1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for informati
6、on only.1.4 For specific hazard information and guidance consult suppliers Material suppliers Safety Data Sheet.1.5 This standard does not purport to address the safety concerns, if any, associated with its use. It is the responsibility ofwhoever uses this standard to consult and establish appropria
7、te safety and health practices and determine the applicability ofregulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D770 Specification for Isopropyl AlcoholD1193 Specification for Reagent WaterE200D4806 Practice for Preparation, Standardization, and Storage of Standard an
8、d Reagent Solutions for Chemical Analysis-Specification for Denatured Fuel Ethanol for Blending with Gasolines for Use as Automotive Spark-Ignition Engine FuelD7795 Test Method for Acidity in Ethanol and Ethanol Blends by TitrationE29 Practice for Using Significant Digits in Test Data to Determine C
9、onformance with SpecificationsE200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis3. Summary of Test Method3.1 The specimen is mixed with either an equal volume of water or an equal volume of alcohol, and titrated with aqueoussodium hydr
10、oxide solution to the phenolphthalein end point.4. Significance and Use4.1 This test method is useful for determining low levels of acidity, below 0.05 %, in organic compounds and hydrocarbonmixtures. The total acidity is calculated as acetic acid or milligrams of sodium hydroxide per gram of sample
11、.4.2 Acidity may be present as a result of contamination, decomposition during storage or distribution, or manufacture. This testmethod may be used in assessing compliance with a specification.1 This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials
12、, and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved June 1, 2012Feb. 1, 2017. Published July 2012February 2017. Originally approved in 1964. Last previous edition approved in 20062012 asD1613 06.D161
13、3 06 (2012). DOI: 10.1520/D1613-06R12.10.1520/D1613-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standardsstandards Document Summary page on the ASTM websi
14、te.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior
15、editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*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-
16、2959. United States15. 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 used in all tests. Unless otherwise indicated, it is intended that all reagents shall conformto the specifications of th
17、e Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable.3 Other grades may be used provided it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.6.2 Unless othe
18、rwise indicated, references to water shall be understood to mean reagent water conforming to Type IV ofSpecification D1193.7. Reagents7.1 Alcohols, refined, ethyl or isopropyl.NOTE 1Isopropyl alcohol (99 % grade) conforming to Specification D770, or 190 proof ethyl alcohol conforming to formula No.
19、3A of the U.S.Bureau of Alcohol, Tobacco and Firearms is suitable for use as the solvent. The use of methyl alcohol is not recommended.7.2 Phenolphthalein Indicator Solution (10 g/L)Dissolve 1 g of phenolphthalein in ethyl or isopropyl alcohol (see Note 1) anddilute to 100 mL with the alcohol.7.3 So
20、dium Hydroxide, Standard Solution (0.05 N)Prepare and standardize a 0.05 N sodium hydroxide (NaOH) solution (Note2) in accordance with the Preparation and Standardization of Solutions, Precision and Bias, Preparation of 50 % of NaOH Solutionand of Standard Solutions, and Standardization sections of
21、Practice E200.NOTE 2Alternatively, KOH solution may be used.8. Procedure8.1 Measure into a 250-mL Erlenmeyer flask 50 mL of water, if the sample is completely water-soluble, or 50 mL of alcohol,if the sample is not completely water-soluble.8.2 Add 0.5 mL of phenolphthalein indicator solution. Titrat
22、e the water or alcohol with 0.05 N NaOH solution to the firstperceptible pink color.8.3 Pipet 50 mL of the sample into the flask. Titrate with the 0.05 N NaOH solution to the same first perceptible pink colororiginally obtained.8.3.1 If the sample is fuel ethanol or denatured fuel ethanol, as define
23、d in Specification D4806, purge the sample for 2 min with400 mL/mn of nitrogen prior to pipetting (see Test Method D7795 for additional information on purging the sample).NOTE 3It is well known that carbon dioxide is highly soluble in ethanol solutions. Carbon dioxide can be dissolved into the ethan
24、ol solution duringproduction (especially fermentation processes), during transportation or during laboratory analysis. The dissolved carbon dioxide is a known interferencefor this test method creating incorrect elevated acidity values. If the dissolved carbon dioxide is not removed from a sample, er
25、roneously high results canbe experienced which can exceed the specification limit. It is recommended that Test Method D7795 be used for the determination of acidity in fuelethanol and denatured fuel ethanol; furthermore, as is codified in Specification D4806, Test Method D7795 should be considered t
26、he referee method:It has been observed that in COSection 8.4.1 2-rich laboratory environment such as those in an ethanol from cornfrom SpecificationD4806manufacturing facility, 0.5 % : “Dissolved carbon dioxide is a known interference and can cause a false high reading when using Test MethodD1613. I
27、n the absence of dissolved CO2 level or greater,Test Method D1613 can cause a positive interference (higher results) when using this test method.If your laboratory environment has this level ofis an acceptable method. If a sample is known to have dissolved CO2 or greater, it isif dissolved CO2recomm
28、ended that proper precaution(s) should becan be present, Test Method D7795 taken to minimize COis the preferred method.2 interference.In casesof differing results between the two test methods, Test Method D7795 shall be the referee method.”9. Calculations9.1 Calculate the acidity of the sample as fo
29、llows:Acidity as acetic acid,weight%5VN30.12!/D (1)or,Acidity as mg KOH per gof sample5VN31.12!/D (2)where:V = NaOH solution required for titration of the sample, mL,3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testi
30、ng of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D1613 172N = normality of the NaOH solution, an
31、dD = density of specimen in g/mL.where: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 nearest 0.0001 %. Duplicate runs that agree within 0.0005 %, absolute, area
32、cceptable for averaging (95 % confidence level).11. Precision and Bias411.1 Precision:11.1.1 The following criteria should be used for judging the acceptability of results at the 95 % confidence level:11.1.1.1 RepeatabilityThe normal range between two results, each the mean of duplicate determinatio
33、ns, obtained by the sameanalyst on different days, is estimated to be 0.0003 %, absolute. Two such values should be considered suspect if they differ bymore than 0.0008 %, absolute.11.1.1.2 ReproducibilityThe normal range between two results, each the mean of duplicate determinations obtained byanal
34、ysts in different laboratories, is estimated to be 0.0005 %, absolute. Two such values should be considered suspect if they differby more than 0.0014 %, absolute.NOTE 4The above precision estimates are based on an interlaboratory study on two samples each of n-butyl acetate, n-butyl alcohol, and met
35、hyl ethylketone containing 0.0058, 0.0112, 0.0007, 0.0046, 0.0026, and 0.0067 % acetic acid, respectively. Each of four laboratories analyzed all six samples, withtwo analysts in each laboratory performing duplicate determinations using both 99 % isopropyl alcohol and formula 3Aethanol as solvents,
36、and repeatingon a second day, for a total of 384 determinations.11.2 BiasThe bias of this test method has not been determined because there is no available material with an acceptedreference value.12. Keywords12.1 acidity; solvents; total acidity as acetic acidSUMMARY OF CHANGESCommittee D01.35D01 h
37、as identified the location of selected changes to this standard since the last issue(D1613 - 03D161306(2012) that may impact the use of this standard. (Approved February 1, 2017.)(1) Added Note 3 afterD4806 Specification 8.3.for Denatured Fuel Ethanol for Blending with Gasolines for Use as Automotiv
38、eSpark-Ignition Engine Fuel as a referenced document in Section 2.(2) Added D7795 Standard Test Method for Acidity in Ethanol and Ethanol Blends by Titration as a referenced document inSection 2.(3) Added new section 8.3.1 to give specific direction for using Test Method D1613 on fuel ethanol or den
39、atured fuel ethanol.(4) Updated Note 3 to give specific directions for the purge conditions required when using Test Method D1613 on fuel ethanolor denatured fuel ethanol.4 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D01-104
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