1、Designation: D509 05 (Reapproved 2011)1Standard Test Methods ofSampling and Grading Rosin1This standard is issued under the fixed designation D509; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、 in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEFootnotes 4 and 5 were editorially updated in June 2011.1. Scope1.1 These test methods cover procedures for sampling anddetermining the grade of ros
3、in delivered in commercial bags,barrels, drums or in molten form. Although developed forrosin, these methods can also be used for the grading ofmodified rosins and rosin based resins.NOTE 1All rosin sold in interstate commerce must be described byreference to the U. S. Standards for rosin, and is th
4、erefore subject tograding prior to such sale. The grading procedure described in these testmethods is used for checking grades or regrading after the rosin hasmoved from the primary markets to distributing or consuming points.1.2 The values stated in SI units are to be regarded as thestandard. The v
5、alues given in parentheses are for informationonly.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 this standard to establish appro-priate safety and health practices and determine the applica-bility of
6、regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D465 Test Methods for Acid Number of Naval StoresProducts Including Tall Oil and Other Related ProductsD1544 Test Method for Color of Transparent Liquids(Gardner Color Scale)D5974 Test Methods for Fatty and Rosin Acids in
7、 Tall OilFractionation Products by Capillary Gas ChromatographyD6090 Test Method for Softening Point Resins (MettlerCup and Ball Method)D6166 Test Method for Color of Naval Stores and RelatedProducts (Instrumental Determination of Gardner Color)E28 Test Methods for Softening Point of Resins Derivedf
8、rom Naval Stores by Ring-and-Ball Apparatus3. Significance and Use3.1 Rosin is an important product of the centuries old NavalStores industry and is produced and consumed in manycountries throughout the world. Consequently, reliable meth-ods of sampling and grading rosin are necessary. The testmetho
9、ds based on the use of the USDA Official Standardsdescribed herein, were developed many years ago for thesampling and grading of rosin and are similar to those includedin the Naval Stores Act.33.2 Although these test methods based on the use of theUSDA Official Standards are still applicable, many a
10、dditionaltest methods are now used to grade rosin. In particular, thecolor of rosin is now more commonly reported using theGardner color scale rather than the USDA Official Standards.In addition, Test Methods E28, D465, and D5974 are widelyused to assess the quality of rosin in addition to the color
11、grading methods described in this standard.4. Sampling4.1 Number of Packages to Be SampledA preliminarysampling of 20 % of the entire lot or shipment shall be made.If the grade of 85 % or more of the number of such preliminarysamples agrees with the grade indicated on the package orinvoice, with non
12、e of the samples disagreeing by more thanone grade, the original grading shall be considered confirmedand the shipment accepted as a good delivery. If the grades ofmore than 15 % of the preliminary samples are in disagree-ment, or if any appreciable number are under grade by morethan one grade, addi
13、tional packages in the lot to make up a totalequal to not less than 50 % of the entire shipment (preferablythe entire shipment if accessible and not too great) shall besampled. The findings on such larger quantity shall be acceptedas the basis for settlement between the purchaser and the seller.4.2
14、Method of SamplingTake samples that are approxi-mately cubical in shape and exactly 22.225 mm (78 in.) thick inthe direction in which they are to be viewed, by any of thefollowing methods:1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, an
15、d Applications and are the directresponsibility of Subcommittee D01.34 on Pine Chemicals and HydrocarbonResins.Current edition approved June 1, 2011. Published June 2011. Originallyapproved in 1938. Last previous edition approved in 2005 as D509 05. DOI:10.1520/D0509-05R11.2For referenced ASTM stand
16、ards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Naval Stores Act of 1923 (42 Stat 1435.7 USC-91-99) as amended in 1951 andregulations
17、promulgated thereunder by the United States Department ofAgriculture.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.(a) by cutting or cleaving the same from a lump of rosinremoved from the solid mass in the barrel or drum, the top s
18、ideof which lump shall come from not less than 101.6 mm (4 in.)below the surface of the rosin.(b) by means of a tin mold of suitable design which hasbeen placed inside the barrel or drum through an opening in theside, the top of which opening is not less than 203.2 mm (8 in.)from the top of the cont
19、ainer, in order to provide a sample thatshall have come from a position not less than 4 in. below thesurface of the rosin. The mold thus placed must be entirelywithin the barrel or drum and completely encased in the rosin.(c) by suspending in the barrel or drum of molten rosin aclean tin plate mold
20、22.225 mm2(78 in.2) (inside) and 38.1 mm(1.5 in.) or more in length, in such a manner that it will be ina horizontal position at least 4 in. below the surface of the rosinafter it has thoroughly cooled. Such samples shall not be spikedfrom the barrel until it is completely cooled.(d) by withdrawing
21、from a full package of 67.5 kg (150 lb)or less, a quantity of the molten rosin, and allowing the sameto cool and solidify in any suitable mold. Samples representinga single charge (or intermittent distillation) of oleoresin shallbe taken from not less than 2 packages, one of which shall beselected a
22、fter14 of the rosin has been placed in the containers,and the other shall be the last package filled.(e) by withdrawing a quantity of molten rosin from a fulldrum, filled after a preliminary cooling period, and taken 1 hafter the drum was filled, and pouring some withdrawn portioninto a suitable mol
23、d.(f) by pouring a portion of molten rosin sampled duringproduction into a color mold.5. Apparatus5.1 Offcial Rosin StandardsThe official standards for usein grading rosin, plus three standards lighter than “X” consistsof assemblies of colored glass plates, cemented together, asissued on loan by the
24、 U.S. Department of Agriculture.4Thegrades and standards are designated as follows: XC, XB, XA,X, WW, WG, N, M, K, I, H, G, F, E, and D. A special grade,FF, is used for dark wood rosins. Grades XA, XB, and XC arenot available from the U.S. Department of Agriculture but maybe purchased commercially.5
25、The standards issued by theDepartment of Agriculture (except FF), consist of combina-tions of plates cut, ground, and polished to specified thick-nesses from selected melts of Corning and Jena colored glass.The colorimetric specifications of the standards, based on the1931 CIE Coordinate System, for
26、 a standard observer usingstandard Illuminant C, are given in Table 1. The colorimetricspecifications for the U.S. Rosin Standards, Master Cubes XA,XB, and XC, are given in Table 2.5.2 Secondary standards or “type samples” are sometimesused for approximate grading, in the absence of permanentofficia
27、l standards of glass.5Such samples may consist of cubesof specially selected rosin or other colored transparent me-dium; solutions are also sometimes used (Note 2).5.3 Rosin Color Molds, 22.225 mm (78 in.), standard size orRosin Sample Trays, 22.225 by 22.225 by 22.225 mm (78 by78by 1 in.), white co
28、ver without labels.NOTE 2It is not possible to dissolve a specified quantity of rosin in asolvent and use such solution as a standard for grading the rosin becausethere is no constant relationship between the color of the original solidrosin and the color of the rosin after being put in solution. Co
29、nsequently,the color of such solution is not a criterion of the color of the rosin itself.6. Color Grading with the USDA Official Standards6.1 The sample or “type” shall be compared with theappropriate standard, preferably against an open direct northsky light, or in a direction that excludes direct
30、 rays from thesun from passing through the rosin to the eye. The gradeassigned to the rosin shall be considered that of the highest orlightest colored standard which the sample equals or excels (islighter than) in color (Note 3). Should the color or appearanceof the rosin be such that there is a dou
31、bt whether the rosin is aslight or bright as the standard, the sample and the standard shallbe viewed through a suitable colorimeter. Then in case ofuncertainty the rosin shall be given the benefit of the doubt. Forexample, if a rosin sample is definitely darker than the WWstandard but lighter than
32、the WG standard, it is WG grade. Ifhowever, the grader is undecided whether the total color of therosin is “as good as” or equals, or is darker than that of the WWstandard, the grade is WW.4The U.S. Rosin Standards are issued only by the Agricultural MarketingService, Tobacco Division, U.S. Departme
33、nt of Agriculture, P.O. Box 96456,Washington, DC 20090-6456. To obtain a set of standards, a Form N.S.A. 2“Request for Loan of Official United States Rosin Standards” and a security depositof $100.00 should be sent to the above address.If an applicant is unable to borrow a set of the U. S. Rosin Sta
34、ndards, becauseof the limited number of sets in existence, secondary sets are available. Thesestandards are excellent duplicates of the U. S. Rosin Standards but could not beclassified as identical and do not have official recognition of the U.S. Department ofAgriculture. (Note: Recent attempts to o
35、btain either the official sets or the secondarysets at the USDAaddress listed have elicited no response and it is possible that thesestandards are no longer available.)5Glass discs of the secondary standards and the XA, XB, and XC standards maybe purchased directly from Tintometer, Ltd., Salisbury,
36、England.TABLE 1 Colorimetric Specifications for U.S. Rosin Standards(Master Set No. 200)AGrade xyTl pX 0.4339 0.4663 0.609 575.0 0.755WW 0.4579 0.4732 0.531 576.8 0.851WG 0.4785 0.4741 0.466 578.5 0.905N 0.5001 0.4704 0.396 580.5 0.944M 0.5212 0.4619 0.322 582.8 0.969K 0.5430 0.4483 0.245 585.5 0.98
37、5I 0.5649 0.4310 0.178 588.7 0.993H 0.5879 0.4102 0.1114 592.4 0.997G 0.6116 0.3874 0.0723 596.8 0.999F 0.6364 0.3632 0.0398 602.1 1.000E 0.6640 0.3358 0.0131 609.4 1.000D 0.6943 0.3057 0.0021 621.4 1.000Ax and y are CIE trilinear coordinates; T is the luminous transmission factor; lis the dominant
38、wavelength in nanometers; p is the colorimetric purity.TABLE 2 Colorimetric Specifications for U. S. Rosin Standards(Master Cubes XA, XB, and XC)AGrade xyTXA 0.4048 0.4443 0.708XB 0.3724 0.4117 0.788XC 0.3406 0.3696 0.848Ax and y are CIE trilinear coordinates; T is the luminous transmission factor.D
39、509 05 (2011)12NOTE 3The “color” of a sample of rosin is made up of threeattributes: hue, saturation, and brightness. “Hue” alludes to the character-istic described by the words “yellow” or “red.” “Saturation” describes thepurity or strength of the yellowness or redness of the color. “ Brightness”de
40、pends on the relative amount of light transmitted by the rosin. Thecleanliness of the rosin affects its transparency and therefore its brightness.The terms “lighter than” and its inverse, “darker than” are convenient todescribe the difference between a sample and a standard. The rosin may bedarker t
41、han the standard in one or more of the following ways: (1) a redderhue, ( 2) a more saturated hue, and (3) a lower brightness.6.2 A sample showing two distinct colors, usually evi-denced by darker streaks through the rosin, indicates a mixtureof rosins in the package, in which case the darkest part
42、of thesample or darkest rosin to be found in the package shalldetermine the grade.6.3 A check sample taken from close to the bottom of abarrel or drum shall not be considered representative, becauseof a natural variation in color sometimes found between the topand bottom rosin as well as a reduced b
43、rightness of the bottomrosin due to a settling of finely divided suspended matterusually present in normal gum rosin. Should such bottomsample show not more than one grade lower than the topsample, the latter shall determine the grade of the rosin in thebarrel. If, however, the bottom-head sample is
44、 more than onegrade lower than the top sample, double filling or “mixed-packing” is indicated, and the bottom-head sample shalldetermine the grade of the rosin in the package.6.4 Rosin that is only slightly cloudy or opaque (caused byoccluded moisture or separation of crystals in the solid mass)shal
45、l be graded in the usual way if the condition is not such asto prevent an accurate evaluation of the color in comparisonwith the standards. If, however, the opaqueness is of such adegree that the grade cannot be definitely determined incomparison with the standards, the rosin shall be designated“OPA
46、QUE” and graded “OP,” in which case its acceptance andvalue shall be a matter for settlement between the purchaserand the seller without reference to grade. Such opaque rosinmay be further identified or described as pale, medium, or darkopaque.7. Tolerance7.1 The tolerance or allowance of 15 % varia
47、tion (Note 4)described in Section 5 is necessary because careful competentgraders rarely get exact duplicate results on all individualsamples when regrading a large number of rosin samples.Moreover, a regrade sample, coming from a different positionin the package, and after storage and weathering fo
48、r anindefinite period, may be slightly darker than the originalsample on which the grade was based. An allowance for suchslight variation must therefore be made.NOTE 4This tolerance is that recognized by the Federal Governmentin the administration of the U.S. Naval Stores Act.8. Color Grading by Gar
49、dner Color Scale8.1 Determine the color on the Gardner scale in accordancewith Test Methods D1544 or D6166.9. Softening Point9.1 Determine the softening point in accordance with TestMethods E28.9.2 Test Method D6090 may be used to determine thesoftening point provided the user determines the startingtemperature and heating rate that give results equivalent to thering and ball softening point in Test Methods E28.10. Acid Number10.1 Determine the acid number in accordance with TestMethods D465.11. Gas Chromatographic Analysis11.1 Determine the amounts of the major ro
