1、Designation: D803 03 (Reapproved 2008) D803 12Standard 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 i
2、n 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 test procedures to be applied to whole tall oils or refined tall oils. Previous editions of thesetest methods have
3、 described test procedures that are used to test tall oil fatty acid, rosin, and other tall oil-derived products as wellas test crude and refined tall oil. Consequently, these test methods are widely cited in reference books and industry literature forthe testing of tall oil-derived products.1.1.1 I
4、n this current revision, procedural details of some of the often-cited test methods have been removed and the test methodsconsolidated with other existing test methods. In such cases the consolidated methods, applicable to all tall oil-derived products,are referenced.products.1.2 The procedures appe
5、ar in the following 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 sta
6、ted in inch-pound units are to be regarded as standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information only and are not considered standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its
7、 use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D92 Test Method for Flash and Fire Points by Cleveland Open Cup TesterD93 T
8、est Methods for Flash Point by Pensky-Martens Closed Cup TesterD269 Test Method for Insoluble Matter in Rosin and Rosin DerivativesD464 Test Methods for Saponification Number of Naval Store Products Including Tall Oil and Other Related ProductsD465 Test Methods for Acid Number of Naval Stores Produc
9、ts Including Tall Oil and Other Related ProductsD890 Test Method for Water in Liquid Naval StoresD1065 Test Method for Unsaponifiable Matter in Naval Stores, Including Rosin, Tall Oil, and Related ProductsD1240 Test Methods for Rosin Acids Content of Naval Stores, Including Rosin, Tall Oil, and Rela
10、ted Products1 These test methods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility ofSubcommittee D01.34 on Naval StoresPine Chemicals and Hydrocarbon Resins.Current edition approved June 1, 2008Nov. 1, 2012.
11、 Published June 2008December 2012. Originally approved in 1944. Last previous edition approved in 20032008 asD803 03.D803 03 (2008). DOI: 10.1520/D0803-03R08.10.1520/D0803-12.2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. F
12、or Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may
13、not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor
14、 Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Related Materials(Withdrawn 2003)3D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)D1545 Test Method for Visc
15、osity of Transparent Liquids by Bubble Time MethodD1585 Test Methods for Fatty Acids Content of Naval Stores, Including Rosin, Tall Oil, and Related ProductsD2196 Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield type) ViscometerD3278 Test Methods for Flash
16、 Point of Liquids by Small Scale Closed-Cup ApparatusD5974 Test Methods for Fatty and Rosin Acids in Tall Oil Fractionation Products by Capillary Gas ChromatographyD6166 Test Method for Color of Naval StoresPine Chemicals and Related Products (Instrumental Determination of GardnerColor)E300 Practice
17、 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 consists primarilyof fatty acids, resin acids, and neutral materials; the levels of these various components depend on factors su
18、ch as the species ofpine tree, geographic location, climate, etc.3.1.1 Tall oil is used primarily as a commercial source of fatty acids and rosin, and, therefore, reliable methods for the analysisof these components is necessary.4. Purity of Reagents4.1 Reagent grade chemicals shall be used in all t
19、ests. Unless otherwise indicated, it is intended that all reagents shall conformto the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable.4 Other grades may be used, provided it is first ascertained that the reagent is of s
20、ufficiently high purity to permit its usewithout lessening the accuracy of the determination.4.2 Unless otherwise indicated, references to water shall be understood to mean distilled water or deionized water.5. Sampling5.1 As with many industrial chemicals, the procedure for obtaining a representati
21、ve sample of tall oil depends on the containerto be sampled and the uniformity of the material to be sampled. No specific standard procedure for sampling tall oil has beendeveloped but Test Method D1466 and Practice E300 describe applicable methods when the tall oil contains no separated solidsor se
22、parated water. If rosin has separated, the rosin can be redissolved by heating and agitating the material to be sampled untilit is homogeneous. If separated water is present, special procedures should be followed to ensure that a representative sample beobtained. The selection of an appropriate proc
23、edure will depend on the water content and the type of container being sampled.6. Conditioning6.1 Heat the entire sample in a closed container fitted with a capillary vent or its equivalent. Some kind of agitation, even ifdone occasionally by hand, saves much time. Heat in a forced-air oven in order
24、 to dissolve any crystalline material. A temperatureof 100C is usually sufficient to dissolve crystals present in crude tall oil, but a temperature as high as 160C may be required toremove rosin crystals from distilled tall oil. Withdraw the specimens only when all crystalline matter has dissolved a
25、nd when theentire sample becomes a homogeneous fluid after thorough stirring.VISCOSITY BY THE BROOKFIELD METHOD(Preferred Method)7. Procedure7.1 Determine the viscosity in centipoise in accordance with Test Methods D2196. The testing temperature shall be 210F(99C) unless a lower temperature is speci
26、fied.VISCOSITY BY THE BUBBLE TIME METHOD(Alternative Method)8. Procedure8.1 Determine the viscosity in accordance with Test Method D1545. The testing temperature shall be 210F (99C) unless alower temperature is specified.3 The last approved version of this historical standard is referenced on www.as
27、tm.org.4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States
28、Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D803 122FLASH POINT9. Procedure9.1 Determine the flash point in accordance with any referenced method (see Test Methods D92, D93, and D3278).COLOR10. Procedure10.1 Determine the color in accordance with Tes
29、t Methods D1544 or D6166.MOISTURE CONTENT11. Procedure11.1 Determine the moisture content in accordance with the methods described in Test Method D890. The Karl Fischer methodis the preferred method.INSOLUBLE MATTER12. Procedure12.1 Determine the insoluble matter in accordance with Test Method D269.
30、ASH13. Apparatus13.1 Platinum DishA platinum dish of 50 to 100-mL capacity.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 platinum dish to redness and, after cooling in a desiccator, weigh to the nearest 0.0001 g. Place
31、an approximately20-g sample of tall oil in the dish and weigh to the nearest 0.1 g (Note 2). Heat the dish gently by means of a bunsen burner untilthe oil can be ignited at the surface (Note 3). Remove the burner and allow the oil to burn completely. Burn all free carbon on thesides of the dish and
32、heat the residue with a strong flame, or in a muffle furnace, until all carbonaceous matter disappears. Aftercooling in a desiccator weigh the dish to the nearest 0.0001 g. Repeat the heating until a constant weight is obtained.NOTE 2This size is suitable for ash contents in the range from 0.02 to 0
33、.2 %, but in the case of lower or higher ash contents, a larger or smaller samplemay be used. In such cases the result shall be specified or reported as follows: “ Ash “Ash (.g sample) . percent.”NOTE 3To avoid foaming and loss of sample in the case of samples containing moisture, it is advisable to
34、 add 1 to 2 mL of absolute alcohol beforeheating.15. Calculation15.1 Calculate the percentage of ash as follows:Ash. %5R/W! 3100 (1)where: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
35、acid number in accordance with Test Methods D465.17. Saponification Number17.1 Determine the saponification number in accordance with Test Methods D464.D803 12318. Rosin Acid Content18.1 Determine the rosin acid content in accordance with Test Methods D1240.19. Unsaponifiable Matter19.1 Determine th
36、e unsaponifiable matter in accordance with Test Method D1065.20. Fatty Acid Content20.1 Determine the fatty acid content in accordance with Test Methods D1585.21. Gas Chromatographic Analysis21.1 Analyze for rosin acids and fatty acids in accordance with Test Methods D5974.22. Precision and Bias (Ge
37、neral Statement)22.1 Where the test method listed in this standard references another ASTM method, that method should be studied to determinethe precision and bias. Other methods listed are well established, and determination of precision and bias is not practical.23. Keywords23.1 acid number; fatty
38、 acids; rosin acids; saponification number; tall oilASTM International takes no position respecting the 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 rig
39、hts, 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 must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for
40、 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 theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing
41、 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 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/).D803 124
