1、Designation: D 803 03 (Reapproved 2008)Standard Test Methods forTesting Tall Oil1This standard is issued under the fixed designation D 803; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in pare
2、ntheses 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 test procedures to beapplied to whole tall oils or refined tall oils. Previous editionsof these test methods have descri
3、bed test procedures that areused to test tall oil fatty acid, rosin, and other tall oil-derivedproducts as well as test crude and refined tall oil. Consequently,these test methods are widely cited in reference books andindustry literature for the testing of tall oil-derived products.1.1.1 In this cu
4、rrent revision, procedural details of some ofthe often-cited test methods have been removed and the testmethods consolidated with other existing test methods. In suchcases the consolidated methods, applicable to all tall oil-derived products, are referenced.1.2 The procedures appear in the following
5、 order:Physical Tests SectionsViscosity:Brookfield Method (Preferred Method) 7Bubble Time Method 8Flash Point 9Color 10Moisture: 11Insoluble Matter 12Ash 13Chemical AnalysisAcid Number 16Saponification Number 17Rosin Acids 18Unsaponifiable Matter 19Fatty Acids 201.3 The values stated in inch-pound u
6、nits are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is therespons
7、ibility of the user of 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:2D92 Test Method for Flash and Fire Points by ClevelandOpen Cup TesterD93 Test Methods for Flas
8、h Point by Pensky-MartensClosed Cup TesterD 269 Test Method for Insoluble Matter in Rosin and RosinDerivativesD 464 Test Methods for Saponification Number of NavalStore Products Including Tall Oil and Other RelatedProductsD 465 Test Methods for Acid Number of Naval StoresProducts Including Tall Oil
9、and Other Related ProductsD 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 ProductsD 1466 Te
10、st Method for Sampling Liquid Oils and FattyAcids Commonly Used in Paints, Varnishes, and RelatedMaterials3D 1544 Test Method for Color of Transparent Liquids(Gardner Color Scale)D 1545 Test Method for Viscosity of Transparent Liquidsby Bubble Time MethodD 1585 Test Methods for Fatty Acids Content o
11、f NavalStores, Including Rosin, Tall Oil, and Related ProductsD 2196 Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield type) Vis-cometerD 3278 Test Methods for Flash Point of Liquids by SmallScale Closed-Cup ApparatusD 5974 Test Methods for Fatty and Rosin
12、Acids in Tall OilFractionation Products by Capillary Gas Chromatography1These 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 approved June
13、1, 2008. Published June 2008. Originallyapproved in 1944. Last previous edition approved in 2003 as D 803 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 sta
14、ndards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.D 6166 Test Method for Color of Naval Stores and RelatedProducts (Instrumental Determination of Gardner Color)E 300 Practice f
15、or Sampling Industrial Chemicals3. Significance and Use3.1 Tall oil, both crude and refined, is an important by-product of the alkaline (kraft) pulping of pine wood. It consistsprimarily of fatty acids, resin acids, and neutral materials; thelevels of these various components depend on factors such
16、asthe species of pine tree, geographic location, climate, etc.3.1.1 Tall oil is used primarily as a commercial source offatty acids and rosin, and, therefore, reliable methods for theanalysis of these components is necessary.4. Purity of Reagents4.1 Reagent grade chemicals shall be used in all tests
17、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.4Other grades may be used, pro-vided it is first ascertained that the reagent is of suffici
18、entlyhigh purity to permit its use without lessening the accuracy ofthe determination.4.2 Unless otherwise indicated, references to water shall beunderstood to mean distilled water or deionized water.5. Sampling5.1 As with many industrial chemicals, the procedure forobtaining a representative sample
19、 of tall oil depends on thecontainer to be sampled and the uniformity of the material to besampled. No specific standard procedure for sampling tall oilhas been developed but Test Method D 1466 and PracticeE 300 describe applicable methods when the tall oil containsno separated solids or separated w
20、ater. If rosin has separated,the rosin can be redissolved by heating and agitating thematerial to be sampled until it is homogeneous. If separatedwater is present, special procedures should be followed toensure that a representative sample be obtained. The selectionof an appropriate procedure will d
21、epend on the water contentand the type of container being sampled.6. Conditioning6.1 Heat the entire sample in a closed container fitted witha capillary vent or its equivalent. Some kind of agitation, evenif done occasionally by hand, saves much time. Heat in aforced-air oven in order to dissolve an
22、y crystalline material. Atemperature of 100C is usually sufficient to dissolve crystalspresent in crude tall oil, but a temperature as high as 160Cmay be required to remove rosin crystals from distilled tall oil.Withdraw the specimens only when all crystalline matter hasdissolved and when the entire
23、 sample becomes a homogeneousfluid after thorough stirring.VISCOSITY BY THE BROOKFIELD METHOD(Preferred Method)7. Procedure7.1 Determine the viscosity in centipoise in accordance withTest Methods D 2196. The testing temperature shall be 210F(99C) unless a lower temperature is specified.VISCOSITY BY
24、THE BUBBLE TIME METHOD(Alternative Method)8. Procedure8.1 Determine the viscosity in accordance with Test MethodD 1545. The testing temperature shall be 210F (99C) unlessa lower temperature is specified.FLASH POINT9. Procedure9.1 Determine the flash point in accordance with anyreferenced method (see
25、 Test Methods D92, D93, and D 3278).COLOR10. Procedure10.1 Determine the color in accordance with Test MethodsD 1544 or D 6166.MOISTURE CONTENT11. Procedure11.1 Determine the moisture content in accordance with themethods described in Test Method D 890. The Karl Fischermethod is the preferred method
26、INSOLUBLE MATTER12. Procedure12.1 Determine the insoluble matter in accordance with TestMethod D 269.ASH13. Apparatus13.1 Platinum DishA platinum dish of 50 to 100-mLcapacity.NOTE 1A porcelain or silica dish may be used in place of platinum,if the ash is not to be analyzed.14. Procedure14.1 Heat th
27、e platinum dish to redness and, after cooling ina desiccator, weigh to the nearest 0.0001 g. Place an approxi-mately 20-g sample of tall oil in the dish and weigh to thenearest 0.1 g (Note 2). Heat the dish gently by means of abunsen burner until the oil can be ignited at the surface (Note3). Remove
28、 the burner and allow the oil to burn completely.Burn all free carbon on the sides of the dish and heat theresidue with a strong flame, or in a muffle furnace, until allcarbonaceous matter disappears. After cooling in a desiccator4Reagent Chemicals, American Chemical Society Specifications, American
29、Chemical 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 National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC),
30、Rockville,MD.D 803 03 (2008)2weigh the dish to the nearest 0.0001 g. Repeat the heating untila constant weight is obtained.NOTE 2This size is suitable for ash contents in the range from 0.02 to0.2 %, but in the case of lower or higher ash contents, a larger or smallersample may be used. In such case
31、s the result shall be specified or reportedas follows: “ Ash (.g sample) . percent.”NOTE 3To avoid foaming and loss of sample in the case of samplescontaining moisture, it is advisable to add 1 to 2 mL of absolute alcoholbefore heating.15. Calculation15.1 Calculate the percentage of ash as follows:A
32、sh. % 5 R/W! 3 100(1)where:R = residue, g, andW = sample, dry basis, g.15.2 Report the percentage of ash to the third decimal place.CHEMICAL ANALYSIS16. Acid Number16.1 Determine the acid number in accordance with TestMethods D 465.17. Saponification Number17.1 Determine the saponification number in
33、 accordancewith Test Methods D 464.18. Rosin Acid Content18.1 Determine the rosin acid content in accordance withTest Methods D 1240.19. Unsaponifiable Matter19.1 Determine the unsaponifiable matter in accordancewith Test Method D 1065.20. Fatty Acid Content20.1 Determine the fatty acid content in a
34、ccordance withTest Methods D 1585.21. Gas Chromatographic Analysis21.1 Analyze for rosin acids and fatty acids in accordancewith Test Methods D 5974.22. Precision and Bias (General Statement)22.1 Where the test method listed in this standard referencesanother ASTM method, that method should be studi
35、ed todetermine the precision and bias. Other methods listed are wellestablished, and determination of precision and bias is notpractical.23. Keywords23.1 acid number; fatty acids; rosin acids; saponificationnumber; tall oilASTM International takes no position respecting the validity of any patent ri
36、ghts 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 is subject to revision at an
37、y time by the responsible technical committee and 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 w
38、ill 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 standard is copyrighted by A
39、STM 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).D 803 03 (2008)3
