1、Designation: D1585 96 (Reapproved 2011)Standard Test Methods forFatty Acids Content of Naval Stores, Including Rosin, TallOil, and Related Products1This standard is issued under the fixed designation D1585; the number immediately following the designation indicates the year oforiginal adoption or, i
2、n 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 fattyacids of naval stores, incl
3、uding rosin, tall oil, and relatedproducts.1.2 These test methods may not be applicable to adducts orderivatives of rosin or other naval stores products.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of th
4、is standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D465 Test Methods for Acid Number of Naval StoresProducts Including Tall Oil and Other Related ProductsD803 Test Method
5、s for Testing Tall OilD890 Test Method for Water in Liquid Naval StoresD1065 Test Method for Unsaponifiable Matter in NavalStores, Including Rosin, Tall Oil, and Related ProductsD1240 Test Methods for Rosin Acids Content of NavalStores, Including Rosin, Tall Oil, and Related ProductsE177 Practice fo
6、r Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Method3.1 The rosin acids content is determined using either themodified potentiometric Wolfe Method or the modified indica-tor
7、Wolfe Method described in Test Methods D1240. Rosinacids are calculated as abietic acid.3.2 The acid number is determined by either the potentio-metric or the indicator method in accordance with Test Meth-ods D465.3.3 The unsaponifiable matter is determined in accordancewith the methods described in
8、 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 andthe acid number.3.4.2 For materials with a fatty acid content greater than5 %, fatty acid content is calcu
9、lated from the rosin acids andunsaponifiables content.3.5 The same method for end point detection, either poten-tiometric or indicator, should be used for acid number, unsa-ponifiables, and rosin acids content determination, in order toavoid slight variables that might occur.3.6 Since the fatty acid
10、s remaining in tall oil rosin, tall oil,and other naval stores products consist of oleic acid withvarying amounts of other saturated and unsaturated acids, it hasbecome customary to calculate and report the fatty acid contentas oleic acid.4. Significance and Use4.1 These test methods are designed to
11、 broaden the scope ofthe previous edition of these test methods by the inclusion oftall oil as a test material. Test Methods D803 currently includesmethods for the determination of the rosin acid and fatty acidcontent of crude tall oil. Test Methods D803 references TestMethod D1585.4.2 Rosin and tal
12、l oil are composed primarily of rosin acidsand fatty acids, and the measurement of these components isimportant in establishing the composition of these materials.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are th
13、e directresponsibility of Subcommittee D01.34 on Pine Chemicals and HydrocarbonResins.Current edition approved June 1, 2011. Published June 2011. Originallyapproved in 1958. Last previous edition approved in 2005 as D1585 96 (2005).DOI: 10.1520/D1585-96R11.2For referenced ASTM standards, visit the A
14、STM 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, Uni
15、ted States.5. Purity of Reagents5.1 Reagent grade chemicals shall 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.3Othe
16、r grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.5.2 Unless otherwise indicated, references to water shall beunderstood to mean deionized or distilled water.6. Preparation of Sa
17、mple6.1 Homogeneous liquid materials may be used withoutfurther preparation.6.2 Heat nonhomogeneous liquid materials until they arehomogeneous, then take a portion for analysis.6.3 Solid samples are subject to surface oxidation whichmay affect the results. Prepare the sample for analysis bychipping
18、small pieces from a freshly exposed surface of a lumpor lumps and crush to a coarse powder to facilitate weighingand solution. Prepare fresh on the same day, prior to weighing,in order to avoid changes due to surface oxidation of crushedrosin on exposure to the air.PERCENT ROSIN ACID7. Procedure7.1
19、Determine the percent rosin acid of the sample by thepotentiometric or the indicator modified Wolfe Method inaccordance with Test Methods D1240.ACID NUMBER8. Procedure8.1 Determine the acid number by either the potentiometricor the indicator modification in accordance with Test MethodsD465.UNSAPONIF
20、IABLE MATTER9. Procedure9.1 Determine the percentage of unsaponifiable matter byeither the potentiometric or the indicator modification inaccordance with Test Method D1065.WATER10. Procedure10.1 Determine the percent water in the sample by theKarl-Fischer Method in accordance with Test Method D890.F
21、ATTY ACIDS11. Calculation11.1 For materials containing less than 5 % fatty acid,calculate the percentage of fatty acids from the acid numberand the percentage of rosin acids as follows:Fatty acids as oleic acid, % 5 A 2 R 3 1.855!#/1.986 (1)where:A = acid number of original sample,R = rosin acids, %
22、,1.855 = (56.1 3 1000)/(302.4 3 100) (factor to convertthe percentage of rosin acids to acid number), and1.986 = (56.1 3 1000)/(282.4 3 100) (factor to convertacid number to percentage of oleic acid).11.2 For materials containing equal to or greater than 5 %fatty acid, calculate the percent fatty ac
23、id from the percentrosin acids and unsaponifiables as follows:Fatty Acids, % 5 100 2 R 2 U 2 W (2)where:R = rosin acids, %,U = unsaponifiable matter, %,W = water, %.11.3 Report the percentage of fatty acids determined in 11.1or 11.2 to one decimal place.12. Precision and Bias12.1 Interlaboratory Tes
24、t ProgramAn interlaboratorystudy of the fatty acid content of three substances, tall oil fattyacids, distilled tall oil, and rosin, was run in 1994. Each of 14laboratories tested each of the three materials. The design ofthe experiment, similar to that of Practice E691 and a within-between analysis
25、of the data are given in ASTM ResearchReport RR: D01-1088.412.2 Test ResultThe precision information given belowfor the fatty acid content of naval stores products is for thecomparison of two test results, each of which is the average ofthree test determinations as follows:12.2.1 Repeatability Limit
26、, 95 % (within labora-tory) = 0.6 %.12.2.2 Reproducibility Limit, 95 % (between laborato-ries) = 1.9 %.12.3 These terms (repeatability limit and reproducibilitylimit) are used as specified in Practice E177. The respectivestandard deviations among test results, related to the abovenumbers by the fact
27、or of 2.8, are as follows:12.3.1 Repeatability standard deviation = 0.2 %.12.3.2 Reproducibility standard deviation = 0.7 %.12.4 BiasThese test methods have no bias because fattyacid content is defined only in terms of these test methods.13. Keywords13.1 rosin; tall oil; tall oil fatty acids; tall o
28、il rosin; WolfeMethod.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 Un
29、ited States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1088.D1585 96 (2011)2ASTM International takes no position respecting th
30、e 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.This standard i
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32、adquarters. 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 below.This s
33、tandard is copyrighted by ASTM International, 100 Barr Harbor 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D1585 96 (2011)3
