ASTM_D_1794_-_89_scan.pdf

ASTM DI794 89 0759510 002324b 4 W 7 An Amerkan National Standard Modiftcatkn of Technlcai Assodatlon AMERICAN SOCIETV FOR TESTINO AND MATERIALS 1016 Rrer GI.,PhWphk,P I.10103 If no(lislod In Ihr c u m comMmd inda,WHi w u in ihr mxl edttmn.41)Designation:D 1794-89 Repprinlsd Imin the Annunt Book o(ASTM Standards,Copyrighi Standard Test Method for Alcohol-Benzene Soluble Matter in Cellulose This standard is issued under the futed designation D 1794;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 napprov&A superscript epsilon(e)indicates an editorial change since the last revision or reapproval.1.Scope 1.1 This test method covers the determination of alcohol-benzene soluble matter in cellulose and is applicable to dis-solving-type cellulose pulps prepared from cotton or wood,1.2 This standard may involve hazardous materials,oper-ations,and equipment.This standard does not purport to address all o f the safity problems associated with its use.It is the responsibility o f the user o f this standard to establish appropriate safity and health practices and determine the applicability o f regulatory limitations prior to use.2.Referenced Document 2.1 ASTM Standard:D 1348 Test Methods for Moisture in Cellulose2 2.2 Other Documents:Occupational Safety and Health Standards and Interpreta-tions,Part i9103 3.Summary of Test Method 3.1 A sample is extracted with a 1+2 alcohol-benzene solution in a Soxhlet apparatus as a measure of the waxes,fats,resins,and oils present.4.Significance and Use 4.1 This test method provides an estimate of waxes,lipids,resins,and other organic soluble residues that were not removed from the fiber during the pulping process.5.Apparatus 5.1 Extraction Apparatus,Soxhlet,consisting of a 300-mL flask,an extractor with a 50 by 250-mm body,and a Hopkins type condenser.5.2 Extraction Thimble,either(I)standard thickness pa-per,43 by 123 mrn,(2)Alundum,45 by 127 mm,medium-porosity,or(3)glass with coarse-porosity fritted-glass disk,45 by 130 mm.5.3 Extraction Heater alrd Support,heater with three-heat switches.5.4 Oven,gravity-convection,maintained at 105 f 3C.This test method is under the jurisdiction of ASTM Committee DI on Paint and Related Coatings and Materials and is the direct responsibility of Subcom-mittee W1.36 on Cellulosics.Current edition approved Oct.27,1989.Published December 1989.Originally published as D 1794-62.Last previous edition D 1794-62(1985)(.Replaces Anniial Book oJASTM Standards,Vol 06.02.Available from Superinfendent of Documents,US.Government Printing D 1794-60 T.Office,Washington,DC 20402.5.5 Dish,evaporating,milk,aluminum,75 mm in diam-eter by 20 mm deep,5.6 Desiccator with efficient desiccant such as anhydrous calcium sulfate,activated alumina,or magnesium perchlo-rate.Calcium chloride is not satisfactory.6.Reagent.30 ethyl alcohol with 2 volumes of benzene.outlined in OSHA Regulations.7.Procedure 7.1 Weigh 8 to 12 g of loose pulp,to the nearest 0.01 g,into an extractor thimble that has previously been extracted with the alcohol-benzene solvent.For sheet pulp,cut a sample into strips about V4 in.(6.4 mm)wide and 3 in,(76 mm)long,and weigh about 20 g into a thimble.Weigh a separate portion for a moisture determination in accordance with Methods D 1348.7.2 Place the extraction thimble with speccimen in the ex-tractor and connect the flask.Pour 250 mL of the alcohol-benzene solvent into the body of the extractor.Connect the assembled extractor to the condenser and place the flask on the extraction heater.Turn on the cooling water to the condenser and adjust the heater to cause the solvent to reflux at such a rate as to cause siphoning 6 to 8 times/h.Continue the extraction for 5 h,beginning the timing when the solvent first begins to drop from the condenser into the extractor.7.3 When the extraction is complete,turn o f f the heater,Disconnect the flask at a timb when most of the solvent has collected in the extractor.7.4 Heat the evaporating dish in the oven at 105C for 30 min,cool in a desiccator,and weigh to the nearest 0.0001 g.Filter the solution from the flask through a sheet of qualita-tive paper into the weighed drying dish.Rinse the flask and filter with three 5-mL portions of the alcohol-benzene solvent.7.5 Place the dish on a steam bath and evaporate just to dryness.Then place the dish in the oven at 105C for 1 h,cool in a desiccafor,and weigh.8.Calculation matter,S,on the dry basis as follows:where:A=weight of dish and residue,g,B=weight of dish,g,W=weight of specimen,g,and 6.1 Alcohol-Benzene Solvent-Mix 1 volume of Formula NOTE 1:Caution-Benzene i s regdated as a cancer hazard as 8.1 Calculate the percent of alcohol-benzene soluble s=(A-B)/WX(loo-M)/loo)x loo NOTICE:This standard has either been superseded and replaced by a new version or discontinued.Contact ASTM International(www.astm.org)for the latest information.A