1、Designation: D 803 03Standard 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 parentheses indicates
2、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 test procedures to beapplied to whole tall oils or refined tall oils. Previous editionsof these test methods have described test procedur
3、es 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, p
4、rocedural 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 order:Physical T
5、ests 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 This standard does not purport to address all of t
6、hesafety concerns, if any, associated with its use. It is theresponsibility 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:D 92 Test Method for Flash
7、and Fire Points by ClevelandOpen Cup2D 93 Test Methods for Flash Point by Pensky-MartensClosed Tester2D 269 Test Method for Insoluble Matter in Rosin and RosinDerivatives3D 464 Test Methods for Saponification Number of NavalStore Products Including Tall Oil and Other RelatedProducts3D 465 Test Metho
8、ds for Acid Number of Naval StoreProducts Including Tall Oil and Other Related Products3D 890 Test Method for Water in Liquid Naval Stores3D 1065 Test Method for Unsaponifiable Matter in NavalStores, Including Rosin, Tall Oil, and Related Products3D 1240 Test Methods for Rosin Acids Content of Naval
9、Stores, Including Rosin, Tall Oil, and Related Products3D 1466 Test 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)4D 1545 Test Method for Viscosity of Transparent Liquids
10、by Bubble Time Method3D 1585 Test Methods for Fatty Acids Content of NavalStores Including Rosin, Tall Oil, and Related Products3D 2196 Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield type) Vis-cometer4D 3278 Test Methods for Flash Point of Liquids by Sma
11、llScale Closed-Cup Apparatus4D 5974 Test Methods for Fatty and Rosin Acids in Tall OilFractionation Products By Capillary Gas Chromatogra-phy3D 6166 Test Method for Color of Naval Stores and RelatedProducts (Instrumental Determination of Gardner Color)3E 300 Practice for Sampling Industrial Chemical
12、s53. 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; the1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related
13、 Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.34 on Naval Stores.Current edition approved May 10, 2003. Published June 2003. Originallyapproved in 1944. Last previous edition approved in 2002 as D 803 02.2Annual Book of ASTM Standards, Vol 05.01.3Annual
14、Book of ASTM Standards, Vol 06.03.4Annual Book of ASTM Standards, Vol 06.01.5Annual Book of ASTM Standards, Vol 15.05.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.levels of these various components depend on factors such asthe spe
15、cies 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.Unless o
16、therwise 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.6Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh
17、 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 of tall
18、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 water. If
19、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 depend on
20、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 any crystal
21、line 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 sample b
22、ecomes 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 THE BUBBL
23、E 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 Test Met
24、hods D 92, D 93, 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.INSOLU
25、BLE 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 the plati
26、num 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 the bu
27、rner 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 desiccatorweigh the dish to the nearest 0.0001 g. Repeat the heating untila constant we
28、ight 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 cases the result shall be specified or reportedas follows: “Ash (.g sample) . percent.”NOTE 3To avoid foaming
29、and loss of sample in the case of samplescontaining moisture, it is advisable to add 1 to 2 mL of absolute alcoholbefore heating.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the America
30、n 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.D80303215. Calculation15.1 Calculate the percentage of ash as follows:Ash. % 5 R/W! 3 10
31、0(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 accordancewith T
32、est 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 accordance withTes
33、t 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 studied todetermine th
34、e 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 rights asserted in
35、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 any time by the res
36、ponsible 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 will receive caref
37、ul 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 ASTM International
38、, 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).D803033
