1、Designation: D509 05 (Reapproved 2011)1D509 15Standard 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
2、 number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1 NOTEFootnotes 4 and 5 were editorially updated in June 2011.1. Scope1.1 These test methods cover procedures for sampling and determining the gra
3、de of rosin delivered in commercial bags, barrels,drums or in molten form. Although developed for rosin, these methods can also be used for the grading of modified rosins androsin based resins.NOTE 1All rosin sold in interstate commerce must be described by reference to the U. S. Standards for rosin
4、, and is therefore subject to grading priorto such sale. The grading procedure described in these test methods is used for checking grades or regrading after the rosin has moved from the primarymarkets to distributing or consuming points.1.2 The values stated in SI units are to be regarded as the st
5、andard. The values given in parentheses are for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the appl
6、icability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D465 Test Methods for Acid Number of Pine Chemical Products Including Tall Oil and Other Related ProductsD1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)D5974 Test Methods for Fatty and
7、 Rosin Acids in Tall Oil Fractionation Products by Capillary Gas ChromatographyD6090 Test Method for Softening Point Resins (Mettler Cup and Ball Method)D6166 Test Method for Color of Pine Chemicals and Related Products (Instrumental Determination of Gardner Color)E28 Test Methods for Softening Poin
8、t of Resins Derived from Pine Chemicals and Hydrocarbons, by Ring-and-Ball Apparatus3. Significance and Use3.1 Rosin is an important product of the centuries old Naval Stores industry industry, now known as the Pine Chemical industry,and is produced and consumed in many countries throughout the worl
9、d. Consequently, reliable methods of sampling and gradingrosin are necessary. The test methods based on the use of the USDA Official Standards described herein, were developed manyyears ago for the sampling and grading of rosin and are similar to those included in the Naval Stores Act.33.2 Although
10、these test methods based on the use of the USDA Official Standards are still applicable, many additional testmethods are now used to grade rosin. In particular, the color of rosin is now more commonly reported using the Gardner color scalerather than the USDA Official Standards. In addition, Test Me
11、thods E28, D465, and D5974 are widely used to assess the qualityof rosin in addition to the color grading methods described in this standard.4. Sampling4.1 Number of Packages to Be SampledA preliminary sampling of 20 % of the entire lot or shipment shall be made. If thegrade of 85 % or more of the n
12、umber of such preliminary samples agrees with the grade indicated on the package or invoice, withnone of the samples disagreeing by more than one grade, the original grading shall be considered confirmed and the shipment1 These test methods are under the jurisdiction of ASTM Committee D01 on Paint a
13、nd Related Coatings, Materials, and Applications and are the direct responsibility ofSubcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.Current edition approved June 1, 2011Dec. 1, 2015. Published June 2011December 2015. Originally approved in 1938. Last previous edition approved in 200520
14、11 asD509 05.D509 05 (2011)1. DOI: 10.1520/D0509-05R11E01.10.1520/D0509-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standardsstandards Document Summary pa
15、ge on the ASTM website.3 Naval Stores Act of 1923 (42 Stat 1435.7 USC-91-99) as amended in 1951 and regulations promulgated thereunder by the United States Department of Agriculture.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of wh
16、at changes have been made to the previous version. Becauseit may 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 th
17、e official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1accepted as a good delivery. If the grades of more than 15 % of the preliminary samples are in disagreement, or if any appreciablenumber are under grade by more than
18、one grade, additional packages in the lot to make up a total equal to not less than 50 % ofthe entire shipment (preferably the entire shipment if accessible and not too great) shall be sampled. The findings on such largerquantity shall be accepted as the basis for settlement between the purchaser an
19、d the seller.4.2 Method of SamplingTake samples that are approximately cubical in shape and exactly 22.225 mm (78 in.) thick in thedirection in which they are to be viewed, by any of the following methods:(a) by cutting or cleaving the same from a lump of rosin removed from the solid mass in the bar
20、rel or drum, the top side ofwhich 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 has been placed inside the barrel or drum through an opening in the side,the top of which opening is not less than 203.2 mm (8 in.)
21、 from the top of the container, in order to provide a sample that shallhave come from a position not less than 4 in. below the surface of the rosin. The mold thus placed must be entirely within the barrelor drum and completely encased in the rosin.(c) by suspending in the barrel or drum of molten ro
22、sin a clean tin plate mold 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 in a horizontal position at least 4 in. below the surface of the rosin afterit has thoroughly cooled. Such samples shall not be spiked from the barrel until it is comple
23、tely cooled.(d) by withdrawing from a full package of 67.5 kg (150 lb) or less, a quantity of the molten rosin, and allowing the same tocool and solidify in any suitable mold. Samples representing a single charge (or intermittent distillation) of oleoresin shall be takenfrom not less than 2 packages
24、, one of which shall be selected after 14 of the rosin has been placed in the containers, and the othershall be the last package filled.(e) by withdrawing a quantity of molten rosin from a full drum, filled after a preliminary cooling period, and taken 1 h afterthe drum was filled, and pouring some
25、withdrawn portion into a suitable mold.(f) by pouring a portion of molten rosin sampled during production into a color mold.5. Apparatus5.1 Offcial Rosin StandardsThe official standards for use in grading rosin, plus three standards lighter than “X” consists ofassemblies of colored glass plates, cem
26、ented together, as issued on loan by the U.S. Department of Agriculture.4 The grades andstandards 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 fordark wood rosins. Grades XA, XB, and XC are not available from the U.S. Department of Agr
27、iculture but may be purchasedcommercially.5 The standards issued by the Department of Agriculture (except FF), consist of combinations of plates cut, ground,and polished to specified thicknesses from selected melts of Corning and Jena colored glass. The colorimetric specifications of thestandards, b
28、ased on the 1931 CIE Coordinate System, for a standard observer using standard Illuminant C, are given in Table 1.The colorimetric specifications for the U.S. Rosin Standards, Master Cubes XA, XB, and XC, are given in Table 2.4 The U.S. Rosin Standards are issued only by the Agricultural Marketing S
29、ervice, Tobacco Division, U.S. Department of Agriculture, P.O. Box 96456, Washington, DC20090-6456. To obtain a set of standards, a Form N.S.A. 2 “Request for Loan of Official United States Rosin Standards” and a security deposit of $100.00 should be sentto the above address.If an applicant is unabl
30、e to borrow a set of the U. S. Rosin Standards, because of the limited number of sets in existence, secondary sets are available. These standardsare excellent duplicates of the U. S. Rosin Standards but could not be classified as identical and do not have official recognition of the U.S. Department
31、ofAgriculture. (Note:Recent attempts to obtain either the official sets or the secondary sets at the USDAaddress listed have elicited no response and it is possible that these standards are no longeravailable.)5 Glass discs of the secondary standards and the XA, XB, and XC standards may be purchased
32、 directly from Tintometer, Ltd., Salisbury, England.TABLE 1 Colorimetric Specifications for U.S. Rosin Standards(Master Set No. 200)AGrade x y T 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 0.32
33、2 582.8 0.969K 0.5430 0.4483 0.245 585.5 0.985I 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 1.000A x and y are CIE trilinear coordinates; T is the l
34、uminous transmission factor; isthe dominant wavelength in nanometers; p is the colorimetric purity.D509 1525.2 Secondary standards or “type samples” are sometimes used for approximate grading, in the absence of permanent officialstandards of glass.5 Such samples may consist of cubes of specially sel
35、ected rosin or other colored transparent medium; solutionsare also sometimes used (Note 2).5.3 Rosin Color Molds, 22.225 mm (78 in.), standard size or Rosin Sample Trays, 22.225 by 22.225 by 22.225 mm (78 by 78by 1 in.), white cover without labels.NOTE 2It is not possible to dissolve a specified qua
36、ntity of rosin in a solvent and use such solution as a standard for grading the rosin because thereis no constant relationship between the color of the original solid rosin and the color of the rosin after being put in solution. Consequently, the color ofsuch solution is not a criterion of the color
37、 of the rosin itself.6. Color Grading with the USDA Official Standards6.1 The sample or “type” shall be compared with the appropriate standard, preferably against an open direct north sky light, orin a direction that excludes direct rays from the sun from passing through the rosin to the eye. The gr
38、ade assigned to the rosin shallbe considered that of the highest or lightest colored standard which the sample equals or excels (is lighter than) in color (Note 3).Should the color or appearance of the rosin be such that there is a doubt whether the rosin is as light or bright as the standard, thesa
39、mple and the standard shall be viewed through a suitable colorimeter. Then in case of uncertainty the rosin shall be given thebenefit of the doubt. For example, if a rosin sample is definitely darker than the WW standard but lighter than the WG standard,it is WG grade. If however, the grader is unde
40、cided whether the total color of the rosin is “as good as” or equals, or is darker thanthat of the WW standard, the grade is WW.TABLE 2 Colorimetric Specifications for U. S. Rosin Standards(Master Cubes XA, XB, and XC)AGrade x y TXA 0.4048 0.4443 0.708XB 0.3724 0.4117 0.788XC 0.3406 0.3696 0.848Ax a
41、nd y are CIE trilinear coordinates; T is the luminous transmission factor.D509 153NOTE 3The “color” of a sample of rosin is made up of three attributes: hue, saturation, and brightness. “Hue” alludes to the characteristic describedby the words “yellow” or “red.” “Saturation” describes the purity or
42、strength of the yellowness or redness of the color. “ Brightness” “Brightness” dependson the relative amount of light transmitted by the rosin. The cleanliness of the rosin affects its transparency and therefore its brightness. The terms “lighterthan” and its inverse, “darker than” are convenient to
43、 describe the difference between a sample and a standard. The rosin may be darker than the standardin one or more of the following ways: (1) a redder hue, (2) a more saturated hue, and (3) a lower brightness.6.2 A sample showing two distinct colors, usually evidenced by darker streaks through the ro
44、sin, indicates a mixture of rosinsin the package, in which case the darkest part of the sample or darkest rosin to be found in the package shall determine the grade.6.3 A check sample taken from close to the bottom of a barrel or drum shall not be considered representative, because of anatural varia
45、tion in color sometimes found between the top and bottom rosin as well as a reduced brightness of the bottom rosindue to a settling of finely divided suspended matter usually present in normal gum rosin. Should such bottom sample show notmore than one grade lower than the top sample, the latter shal
46、l determine the grade of the rosin in the barrel. If, however, thebottom-head sample is more than one grade lower than the top sample, double filling or “mixed-packing” is indicated, and thebottom-head sample shall determine the grade of the rosin in the package.6.4 Rosin that is only slightly cloud
47、y or opaque (caused by occluded moisture or separation of crystals in the solid mass) shallbe graded in the usual way if the condition is not such as to prevent an accurate evaluation of the color in comparison with thestandards. If, however, the opaqueness is of such a degree that the grade cannot
48、be definitely determined in comparison with thestandards, the rosin shall be designated “OPAQUE” and graded “OP,” in which case its acceptance and value shall be a matter forsettlement between the purchaser and the seller without reference to grade. Such opaque rosin may be further identified ordesc
49、ribed as pale, medium, or dark opaque.7. Tolerance7.1 The tolerance or allowance of 15 % variation (Note 4) described in Section 5 is necessary because careful competent gradersrarely get exact duplicate results on all individual samples when regrading a large number of rosin samples. Moreover, a regradesample, coming from a different position in the package, and after storage and weathering for an indefinite period, may be slightlydarker than the original sample on which the grade was based. An allowance for such slight variation must therefore be made.N
