1、ASTM D3008 40 a 0759510 OObb85s 2-#Tb Designation:D 3008-90 Standard Test Method Resin Acids in Rosin AMERICAN SOCIETY FOR TESTING AN0 MATERIALS 1916 Race SI.Phlladalpha.Pa 19103 RaPrintad from tha Annual Book d ASTM Standards.Copyright ASTM If not listed in tha currant combirwtd indax,will appear i
2、n tha next adiikn.for by Gas-Liquid Chromatography This standard is issued under the fixed designation D 3008;the number immediately following the designation indicates the year of original adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of la
3、st reapproval.A supcrsctipt epsilon(c)indicates an editorial change since the last revision or reapproval.1.Scope 1.1 This test method covers the determination of the resin acids in tall oil,gum,or wood rosin after conversion to their methyl esters.1.2 The composition is calculated from the ratio of
4、 each peak area to the total area of all peaks obtained.Rosins generally contain nonvolatile or polymeric materials for which no peaks are obtained under the conditions used.On the other hand,volatile neutral materials elute in the general region of resin acid methyl esters and can result in errors
5、in the calculated composition.More reliable data is obtained by removal of neutral materials before gas chromatography.2 1.3 This standard does not purport to address all of the safety problems associated with its use.It is the responsibility of the user of this standard to establish appropriate saf
6、ety and health practices and determine the applicability of regulatory limitations prior to use.Specific hazards are given in Note 2.2.Referenced Documents 2.1 ASTM Standards:D 1193 Specification for Reagent Wat$D3257 Test Method for Aromatics in Mineral Spirits by Gas Chromatography3-E 260 Practice
7、 for Packed Column Chromatography4 3.Summary of Test Method.3.1 A portion of the sample is prepared by either con-verting it to the tetramethylammonium salts or esterifying it with diazomethane.A specimen of the prepared sample is injected into a 275C injection port to a 200C column of ethylene glyc
8、ol succinate silicone copolymer(EGSS-X)or diethylene glycol succinate on silanized diatomaceous earth solid support.If added as the tetramethylammonium salt,the sample is pyrolyzed to the methyl ester.The pyrolyzed esters or the prepared esters are carried through the column with nitrogen or helium
9、carrier gas and the chromatogram is obtained using a flame ionization detector.3.2 The peak areas are obtained by any of the conven-tional means and the percent of the respective resin in acids is calculated from the ratios of the areas of the individual peaks to the total area of all peaks.4.Appara
10、tus 4.1 Gas Chromatograph-Any gas-liquid chromatograph having a flame ionization detector that can be operated at the conditions given in Table 1.4.2 Column-Six to 10 ft(1.8 to 3 m)of/S-in.(3.2-mm)outside diameter,0.085-in.(2.15-mm)inside diameter,0.020in.(0.52-mm)wall-thickness stainless steel tubi
11、ng specifically tempered for easy handling and packed with the material as described in 8.1.4.3 Recorder-A recording potentiometer with a full-scale deflection of 0 to 1-mV full-scale response time of 1 s or less,chart speeds of 1/z to 1 in.(12 to 25 mm)/min,and sufficient sensitivity and stability
12、to meet the requirements of 4.1.4.4 Specimen Introduction System-Any system capable of introducing a representative specimen into the column.Microsyringes,lO+L capacity,with fixed needle have been found satisfactory.4.5 Integrating Equipment-In order of preferences based on accuracy,electronic,disk,
13、planimeter,or rule.5.Reagents and Materials 5.1 Purity of Reagents-Reagent grade chemicals shall be used in all tests unless otherwise specified.Unless otherwise indicated,it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Che
14、mical Society,where such specifications are available.Other grades may be used,provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determi-nation.5.2 Purity of Water-Unless otherwise indicated,refer-ences to water s
15、hall be understood to mean reagent water conforming to Type II of Specification D 1193.5.3 Toluene.5.4 N-Methyl-N-Nitroso-p-Toluenesulfonamide.6 5.5 Diethyl Ether,Anhydrous.5.6 2-Ethoxyethanol.5.7 Liquid Phase-Diethylene glycol succinate(DEGS)or ethylene glycol succinate-silicon copolymer(EGSS-X,low
16、-silicone content).NOTE l-EGSS-X is the preferred liquid phase because of its greater stability.5.8 Methanol.This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom-mittee WI.34 on Naval Stores.Current edition approved May 25,1990.Published July 1990.Originally published as D 3008-72.Last orevious edition D 3008-82.z Zinkel,D.F.,and Han,J.,avalSforesReview,Vol96(2),pp.14-19(1986).3 Annual Book of ASTM
