1、Designation: D1585 96 (Reapproved 2011)D1585 15Standard Test Methods forFatty Acids Content of Naval Stores,Pine Chemicals,Including Rosin, Tall Oil, and Related Products1This standard is issued under the fixed designation D1585; the number immediately following the designation indicates the year of
2、original 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.1. Scope1.1 These test methods cover the determination of the fatty aci
3、ds of naval stores,pine chemicals, including rosin, tall oil, andrelated products.1.2 These test methods may not be applicable to adducts or derivatives of rosin or other naval storespine chemical products.1.3 This standard does not purport to address all of the safety concerns, if any, associated w
4、ith its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D465 Test Methods for Acid Number of Pine Chemical Products Includin
5、g Tall Oil and Other Related ProductsD803 Test Methods for Testing Tall OilD890 Test Method for Water in Liquid Pine ChemicalsD1065 Test Method for Unsaponifiable Matter in Naval Stores, Including Rosin, Tall Oil, and Related ProductsD1240 Test Methods for Rosin Acids Content of Pine Chemicals, Incl
6、uding Rosin, Tall Oil, and Related ProductsE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Summary of Test Method3.1 The rosin acids content is determined using either the mo
7、dified potentiometric Wolfe Method or the modified indicatorWolfe Method described in Test Methods D1240. Rosin acids are calculated as abietic acid.3.2 The acid number is determined by either the potentiometric or the indicator method in accordance with Test Methods D465.3.3 The unsaponifiable matt
8、er is determined in accordance with the methods described in Test Method D1065.3.4 The fatty acids are calculated by two methods.3.4.1 For materials with a fatty acid content less than 5 %, fatty acid content is calculated from the rosin acids content and theacid number.3.4.2 For materials with a fa
9、tty acid content greater than 5 %, fatty acid content is calculated from the rosin acids andunsaponifiables content.3.5 The same method for end point detection, either potentiometric or indicator, should be used for acid number,unsaponifiables, and rosin acids content determination, in order to avoi
10、d slight variables that might occur.3.6 Since the fatty acids remaining in tall oil rosin, tall oil, and other naval storespine chemical products consist of oleic acidwith varying amounts of other saturated and unsaturated acids, it has become customary to calculate and report the fatty acidcontent
11、as oleic acid.1 These test methods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility ofSubcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.Current edition approved June 1, 2011Dec. 1, 2015. Published
12、 June 2011December 2015. Originally approved in 1958. Last previous edition approved in 20052011 asD1585 96 (2005).(2011). DOI: 10.1520/D1585-96R11.10.1520/D1585-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Boo
13、k of ASTM Standardsvolume information, refer to the standardsstandards Document Summary page on the ASTM website.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
14、be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Dri
15、ve, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Significance and Use4.1 These test methods are designed to broaden the scope of the previous edition of these test methods by the inclusion of talloil as a test material. Test Methods D803 currently includes methods for the determin
16、ation of the rosin acid and fatty acid contentof crude tall oil. Test Methods D803 references Test Method D1585.4.2 Rosin and tall oil are composed primarily of rosin acids and fatty acids, and the measurement of these components isimportant in establishing the composition of these materials.5. Puri
17、ty of Reagents5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conformto the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable.3 Other grades may be
18、 used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.5.2 Unless otherwise indicated, references to water shall be understood to mean deionized or distilled water.6. Preparation of Sample6.1 Homoge
19、neous liquid materials may be used without further preparation.6.2 Heat nonhomogeneous liquid materials until they are homogeneous, then take a portion for analysis.6.3 Solid samples are subject to surface oxidation which may affect the results. Prepare the sample for analysis by chippingsmall piece
20、s from a freshly exposed surface of a lump or lumps and crush to a coarse powder to facilitate weighing and solution.Prepare fresh on the same day, prior to weighing, in order to avoid changes due to surface oxidation of crushed rosin on exposureto the air.PERCENT ROSIN ACID7. Procedure7.1 Determine
21、 the percent rosin acid of the sample by the potentiometric or the indicator modified Wolfe Method in accordancewith Test Methods D1240.ACID NUMBER8. Procedure8.1 Determine the acid number by either the potentiometric or the indicator modification in accordance with Test MethodsD465.UNSAPONIFIABLE M
22、ATTER9. Procedure9.1 Determine the percentage of unsaponifiable matter by either the potentiometric or the indicator modification in accordancewith Test Method D1065.WATER10. Procedure10.1 Determine the percent water in the sample by the Karl-Fischer Method in accordance with Test Method D890.FATTY
23、ACIDS11. Calculation11.1 For materials containing less than 5 % fatty acid, calculate the percentage of fatty acids from the acid number and thepercentage of rosin acids as follows:Fatty acids as oleic acid,%5A 2R 31.855!#/1.986 (1)3 Reagent Chemicals, American Chemical Society Specifications, Ameri
24、can Chemical Society, Washington, DC. For suggestions on the testing 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. (US
25、PC), Rockville, MD.D1585 152where:A = acid number of original sample,R = rosin acids, %,1.855 = (56.1 1000)(302.4 100) (factor to convert the percentage of rosin acids to acid number), and1.986 = (56.1 1000)(282.4 100) (factor to convert acid number to percentage of oleic acid).11.2 For materials co
26、ntaining equal to or greater than 5 % fatty acid, calculate the percent fatty acid from the percent rosin acidsand unsaponifiables as follows:Fatty Acids,%51002R 2U 2W (2)where:R = rosin acids, %,U = unsaponifiable matter, %,W = water, %.11.3 Report the percentage of fatty acids determined in 11.1 o
27、r 11.2 to one decimal place.12. Precision and Bias412.1 Interlaboratory Test ProgramInterlaboratory Test ProgramAn An interlaboratory study of the fatty acid content ofthree substances, tall oil fatty acids, distilled tall oil, and rosin, was run in 1994. Each of 14 laboratories tested each of the t
28、hreematerials. The design of the experiment, similar to that of Practice E691 and a within-between analysis of the data are given inASTM Research Report RR:D01-1088RR: D01-108812.2 Test ResultTest ResultThe The precision information given below for the fatty acid content of naval storespinechemical
29、products is for the comparison of two test results, each of which is the average of three test determinations as follows:12.2.1 Repeatability Limit, Repeatability Limit,95 % (within laboratory) = 0.6 %.12.2.2 Reproducibility Limit, Reproducibility Limit,95 % (between laboratories) = 1.9 %.12.3 These
30、 terms (repeatability limit and reproducibility limit) are used as specified in Practice E177. The respective standarddeviations among test results, related to the above numbers by the factor of 2.8, are as follows:12.3.1 Repeatability standard deviation = 0.2 %.12.3.2 Reproducibility standard devia
31、tion = 0.7 %.12.4 BiasBiasTheseThese test methods have no bias because fatty acid content is defined only in terms of these testmethods.13. Keywords13.1 rosin; tall oil; tall oil fatty acids; tall oil rosin; Wolfe MethodASTM International takes no position respecting the validity of any patent right
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36、hrough the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D01-1088. Contact ASTM CustomerService at serviceastm.org.D1585 153
