1、Designation: D803 15Standard Test Methods forTesting Tall Oil1This standard is issued under the fixed designation D803; 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 parentheses indicates th
2、e 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 described test procedures
3、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 current revision, proc
4、edural 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.1.2 The procedures appear in the following order:Physical Tests SectionsViscos
5、ity:Rotational Viscometer 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 units are to be regardedas
6、 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 theresponsibility of the user of th
7、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:2D92 Test Method for Flash and Fire Points by ClevelandOpen Cup TesterD93 Test Methods for Flash Point by Pensky-Martens
8、Closed Cup TesterD269 Test Method for Insoluble Matter in Rosin and RosinDerivativesD464 Test Methods for Saponification Number of NavalStore Products Including Tall Oil and Other RelatedProductsD465 Test Methods for Acid Number of Naval StoresProducts Including Tall Oil and Other Related ProductsD8
9、90 Test Method for Water in Liquid Pine ChemicalsD1065 Test Method for Unsaponifiable Matter in NavalStores, Including Rosin, Tall Oil, and Related ProductsD1240 Test Methods for Rosin Acids Content of PineChemicals, Including Rosin, Tall Oil, and Related Prod-uctsD1466 Test Method for Sampling Liqu
10、id Oils and FattyAcids Commonly Used in Paints, Varnishes, and RelatedMaterials (Withdrawn 2003)3D1544 Test Method for Color of Transparent Liquids (Gard-ner Color Scale)D1545 Test Method for Viscosity of Transparent Liquids byBubble Time MethodD1585 Test Methods for Fatty Acids Content of NavalStor
11、es, Including Rosin, Tall Oil, and Related ProductsD2196 Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational ViscometerD3278 Test Methods for Flash Point of Liquids by SmallScale Closed-Cup ApparatusD5974 Test Methods for Fatty and Rosin Acids in Tall OilFractionation Pr
12、oducts by Capillary Gas ChromatographyD6166 Test Method for Color of Pine Chemicals and Re-lated Products (Instrumental Determination of GardnerColor)1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directrespo
13、nsibility of Subcommittee D01.34 on Pine Chemicals and HydrocarbonResins.Current edition approved July 1, 2015. Published July 2015. Originally approvedin 1944. Last previous edition approved in 2012 as D803 12. DOI: 10.1520/D0803-15.2For referenced ASTM standards, visit the ASTM website, www.astm.o
14、rg, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harb
15、or Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E300 Practice for 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
16、, and neutral materials; thelevels of these various components depend on factors such 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
17、 necessary.4. Purity of Reagents4.1 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.4Othe
18、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.4.2 Unless otherwise indicated, references to water shall beunderstood to mean distilled water or deionized water.5. Sampling5.1
19、 As with many industrial chemicals, the procedure forobtaining a representative sample 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 D1466 and Practice E300desc
20、ribe applicable methods when the tall oil contains noseparated solids or separated water. If rosin has separated, therosin can be redissolved by heating and agitating the materialto be sampled until it is homogeneous. If separated water ispresent, special procedures should be followed to ensure that
21、 arepresentative sample be obtained. The selection of an appro-priate procedure will depend on the water content and the typeof 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 o
22、ccasionally by hand, saves much time. Heat in aforced-air oven in order to dissolve any 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.Wi
23、thdraw the specimens only when all crystalline matter hasdissolved and when the entire sample becomes a homogeneousfluid after thorough stirring.VISCOSITY BY THE ROTATIONAL VISCOMETERMETHOD(Preferred Method)7. Procedure7.1 Determine the viscosity in centipoise in accordance withTest Methods D2196. T
24、he testing temperature shall be 210F(99C) unless a lower temperature is specified.VISCOSITY BY THE BUBBLE TIME METHOD(Alternative Method)8. Procedure8.1 Determine the viscosity in accordance with Test MethodD1545. The testing temperature shall be 210F (99C) unless alower temperature is specified.FLA
25、SH POINT9. Procedure9.1 Determine the flash point in accordance with anyreferenced method (see Test Methods D92, D93, and D3278).COLOR10. Procedure10.1 Determine the color in accordance with Test MethodsD1544 or D6166.MOISTURE CONTENT11. Procedure11.1 Determine the moisture content in accordance wit
26、h themethods described in Test Method D890. The Karl Fischermethod is the preferred method.INSOLUBLE MATTER12. Procedure12.1 Determine the insoluble matter in accordance with TestMethod D269.ASH13. Apparatus13.1 Platinum DishA platinum dish of 50 to 100-mLcapacity.NOTE 1A porcelain or silica dish ma
27、y be used in place of platinum,if the ash is not to be analyzed.14. Procedure14.1 Heat the 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 gent
28、ly by means of abunsen burner until the oil can be ignited at the surface (Note3). Remove the burner and allow the oil to burn completely.Burn all free carbon on the sides of the dish and heat the4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC.
29、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), Rockville,MD.D803 152residue with
30、a strong flame, or in a muffle furnace, until allcarbonaceous matter disappears. After cooling in a desiccatorweigh 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
31、lower or higher ash contents, a larger or smallersample may be used. In such cases 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 alcoho
32、lbefore heating.15. Calculation15.1 Calculate the percentage of ash as follows:Ash. % 5 R/W! 3100 (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 TestMe
33、thods D465.17. Saponification Number17.1 Determine the saponification number in accordancewith Test Methods D464.18. Rosin Acid Content18.1 Determine the rosin acid content in accordance withTest Methods D1240.19. Unsaponifiable Matter19.1 Determine the unsaponifiable matter in accordancewith Test M
34、ethod D1065.20. Fatty Acid Content20.1 Determine the fatty acid content in accordance withTest Methods D1585.21. Gas Chromatographic Analysis21.1 Analyze for rosin acids and fatty acids in accordancewith Test Methods D5974.22. Precision and Bias (General Statement)22.1 Where the test method listed i
35、n this standard referencesanother ASTM method, that method should be studied 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 oilAST
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