ASTM_D_3009_-_93_scan.pdf

ASTM D3009 93-0759530 052L5L4 T50-Designation:D 3009-93 AMEHICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race St Philadelphia,Pa 19103 Reprinted from the Annual Book of ASTM Standards.Copyright ASTM If not Med in the cwrent combined Index,will appear in the neti edition.Standard Test Method for Composition of Turpentine by Gas Chromatography This standard is issued under the fixed designation D 3009;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 last reapproval.A superscript epsilon(0 indicates an editorial change since the last revision or reapproval.1.Scope 1.1 This test method covers the determination of the composition,specifically the a-pinene and&pinene content,of wood,gum,and sulfate turpentine by packed column gas chromatography.Terms are defined in Terminology D 804.1.2 This standard does not purport to address all of the safety problems,if any,associated with its use.It is the responsibility 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 Documents 2.1 ASTM Standards:D I3 Specification for Spirits of Turpentine2 D804 Terminology Relating to Naval Stores,Including Tall Oil and Related Products2 3.Summary of Test Method 3.1 A weighted mixture of the sample and internal stan-dard is prepared,an aliquot is injected into a 75C chromato-graphic column,and the temperature programmed to 2OoC to obtain the chromatogram.The peak areas for the compo-nents to be determined and also for the internal standard are measured.The percentages of the components present are calculated from the product of the peak area of the compo-nent,weight of internal standard,and the calibration factor divided by the product of the weight of sample and peak area of the internal standard.4.Significance and Use 4.1 Earlier methods for characterizing turpentine were based on physical properties based on physical properties such as those in Specification D 13.As turpentine became widely used as a chemical raw material its chemical compo-sition,especially its cY-pinene and-pinene content,became more important.The gas chromatographic technique de-scribed in this test method is a rapid and convenient method to perform this analysis.When measurement of the other minor component is required the use of capillary column gas chromatography is recommended.5.Apparatus 5.1 Linear Programmed Temperature Gas Chromatog-raph-Any instrument with programming features and ei-I This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings,Materials,and Applications and is the direct responsibility of Subcommittee WI.34 on Naval Stores.Current edition approved April IS,1993.Published June 1993.Originally published as D 3009-72.Last previous edition D 3009-72(198 I).”2 Anmtal Book oJASTM Standards,Vol 06.03.ther a thermal conductivity detector or a flame ionization detector and adaptable to the following conditions:Detector cell temperature,C 250 Injection port temperature,C 200 Carrier gas(helium)flow at exit,cm/min 50 Programmed temperature details:Starting column temperature,%75 Colimn heating rate,?C/rein hold for 16 min 4 Upper column temperature,C 200 hold for 20 min 5.2 Recorder-A I-mV recorder with a full-scale response of 1 s and a chart speed of 30 in./h.5.3 Integrating Equipment-In order of preferences based on accuracy:electronic,disk,planimeter,or other acceptable methods.5.4 Column-A 12-fi length of 3.18 to 6.35-mm(I/a to G-in.)outside diameter,2.15 to 5.33-mm(0.085 to 0.210-in.)inside diameter,0.5 l-mm(0.020in.)wall,stainless steel tubing specially tempered for easy handling and packed with 20 weight%of polyethylene glycol having a molecular weight of 20 0003%,on 60 to 80 mesh diatomaceous silica4(nonacid washed).Condition at 210C for about 4 h before use.5.5 Microsyringe-Having a fixed needle,with a capacity large enough to deliver a sample sufficient for the chosen conditions.6.Reagents 6.1 Purity of Reagents-Unless otherwise indicated,it is intended that all reagents shall conform to the specifications established by the Committee on Analytical Reagents of the American Chemical Sqciety,where such specifications are available.5 6.2 Calibration Liquid:6.2.1 cY-pinene,purity of at least 99%.6.2.2 8-pinene,purity of at least 99%.6.3 Column Packing-Prepare a 20 weight%mixture of polyethylene glycol on 60/80 mesh diatomaceous silica in accordance with gas chromatographic practice.6.4 Liquid Phase-polyethylene glycol.6.5 Solid Support-diatomaceous silica(non-acid washed),60/80 mesh.6.6 Reference Standard-n-decane,purity of at least 99%.3 Polyethylene glycol such as Carbowax 2OM.manufactured by Union Carbide is available from most scientific supply houses.4 Diatomaceous silica such as Chromosorb W,manufactured by Johns-Mansville Products Corp.,is available f