1、Designation: D 1585 96 (Reapproved 2006)Standard Test Methods forFatty Acids Content of Naval Stores, Including Rosin, TallOil, and Related Products1This standard is issued under the fixed designation D 1585; the number immediately following the designation indicates the year oforiginal adoption or,
2、 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.1. Scope1.1 These test methods cover the determination of the fattyacids of naval stores, i
3、ncluding 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
4、 this 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:2D 465 Test Methods for Acid Number of Naval StoresProducts Including Tall Oil and Other Related ProductsD 803 Test M
5、ethods for Testing Tall OilD 890 Test Method for Water in Liquid Naval StoresD 1065 Test Method for Unsaponifiable Matter in NavalStores, Including Rosin, Tall Oil, and Related ProductsD 1240 Test Methods for Rosin Acids Content of NavalStores, Including Rosin, Tall Oil, and Related ProductsE 177 Pr
6、actice for Use of the Terms Precision and Bias inASTM Test MethodsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Methods3.1 The rosin acids content is determined using either themodified potentiometric Wolfe Method or the modified
7、indica-tor Wolfe Method described in Test Methods D 1240. 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 D 465.3.3 The unsaponifiable matter is determined in accordancewith the methods
8、 described in Test Method D 1065.3.4 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 co
9、ntent is calculated 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
10、the fatty acids 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 a
11、re designed to broaden the scope ofthe previous edition of these test methods by the inclusion oftall oil as a test material. Test Methods D 803 currentlyincludes methods for the determination of the rosin acid andfatty acid content of crude tall oil. Test Methods D 803references Test Method D 1585.
12、4.2 Rosin and tall oil are composed primarily of rosin acidsand fatty acids, and the measurement of these components isimportant in establishing the composition of these materials.5. Purity of Reagents5.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended t
13、hat all reagents shallconform to the specifications of the Committee on Analytical1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.34 on Naval Stores.Current edition app
14、roved Nov. 1, 2006. Published November 2006. Originallyapproved in 1958. Last previous edition approved in 2003 as D 1585 96 (2003).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume inform
15、ation, 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, United States.Reagents of the American Chemical Society, where suchspecifications are available.3Other grades may be used, pro-v
16、ided 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 Sample6.1 Homogeneous liquid
17、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 small pieces from a freshly
18、 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 Determine the percent rosin
19、 acid of the sample by thepotentiometric or the indicator modified Wolfe Method inaccordance with Test Methods D 1240.ACID NUMBER8. Procedure8.1 Determine the acid number by either the potentiometricor the indicator modification in accordance with Test MethodsD 465.UNSAPONIFIABLE MATTER9. Procedure9
20、.1 Determine the percentage of unsaponifiable matter byeither the potentiometric or the indicator modification inaccordance with Test Method D 1065.WATER10. Procedure10.1 Determine the percent water in the sample by theKarl-Fischer Method in accordance with Test Method D 890.FATTY ACIDS11. Calculati
21、on11.1 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, %,1.855 = (56.1 3 1000)/
22、(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 acid from the percentrosi
23、n 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 Test ProgramAn interlabora
24、torystudy 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 E 691 and awithin-between analysis of the data are given i
25、n ASTMResearch Report.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, 95 % (within labora-tory) = 0.6 %.
26、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 E 177. The respectivestandard deviations among test results, related to the abovenumbers by the factor of 2.8, are as follows:12.3.1 Re
27、peatability 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 oil rosin; WolfeMethod.3Reagent Chem
28、icals, 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 Nationa
29、l Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4Support data are available from ASTM International Headquarters. RequestRR:D01 - 1088.D 1585 96 (2006)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mention
30、edin 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 technical committee and
31、 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 International Headquarters. Your comments will receive careful consideration at a meeting of
32、 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 Drive, PO Box
33、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).D 1585 96 (2006)3
