1、Designation: D 5368 93 (Reapproved 2006)Standard Test Methods forGravimetric Determination of Total Solvent ExtractableContent (TSEC) of Solid Waste Samples1This standard is issued under the fixed designation D 5368; the number immediately following the designation indicates the year oforiginal adop
2、tion or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods describe standard procedures forgravimetrically dete
3、rmining the total nonvolatile and semi-volatile organic content of solvent extracts from soils or solidwastes. The following methods are included:SectionMethod AMicro-Determination of TSEC 11-13Method BEvaporating Dish Procedure 14-16Method CBoiling Flask Procedure 17-191.2 These methods are used af
4、ter a solvent extract isobtained from a soil or solid waste. For these methods to beapplicable, the extraction solvent must have a boiling point lessthan that of water at ambient pressure.1.3 The total solvent extractable content (TSEC) of a soil,sediment, sludge, or solid waste depends upon the sol
5、vent andmethod used for the extraction procedure.2. Referenced Documents2.1 ASTM Standards:2D 2109 Test Methods for Nonvolatile Matter in Haloge-nated Organic Solvents and Their AdmixturesD 2910 Method for Removal of Organic Matter from Waterby Activated Carbon Absorption3D 3086 Test Method for Orga
6、nochlorine Pesticides in Wa-ter3D 3445 Method of Test for Nonvolatile Matter in Trichlo-rotrifluoroethane3D 3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD 4281 Test Method for Oil and Grease (FluorocarbonExtractable Substances) by Gravimetric Determi
7、nationD 5369 Practice for Extraction of Solid Waste Samples forChemical Analysis Using Soxhlet Extraction3. Terminology3.1 Definition:3.1.1 total solvent extractable content (TSEC) the totalconcentration by weight (w/w) of organic materials that isextractable from a soil or solid waste by the select
8、ed solvent.4. Summary of Methods4.1 The sample is extracted with an organic solvent using aprocedure such as described in Practices D 5369 (SoxhletExtraction) or Test Method D 4281. The quantity of materialextracted into the solvent is determined as the residue weightafter solvent evaporation. Simil
9、ar ASTM methods are TestMethods D 2109 and D 3445, and Practice D 2910.4.1.1 Method A, Micro-Determination MethodThe resi-due weight after solvent evaporation is determined for 200 Lof solvent extract evaporated on an aluminum weighing dish.Aheat lamp is used to effect evaporation.4.1.2 Method B, Ev
10、aporating Dish ProcedureThe residueweight after solvent evaporation is determined for 1.0 to 75.0mL of solvent extract. Solvent is evaporated in an evaporatingdish by heating at 5C below the solvent boiling point. Astream of nitrogen over the surface of the solvent is used toaccelerate evaporation.4
11、.1.3 Method C, Boiling Flask MethodThe residue weightafter solvent evaporation is determined for 100 to 300 mL ofsolvent evaporated in a boiling flask. Solvent is evaporated ina water bath at the solvent boiling point.5. Significance and Use5.1 The TSEC provides a quantitative measure of the totalso
12、lvent extractable organic content of the solid waste inquestion. Based upon the TSEC, the extract may be analyzed orfurther processed (that is, further cleanup or solvent concen-tration) in preparation for analysis. Thus, the TSEC provides aquantitative measure for optimizing the extractable organic
13、concentration prior to chemical analysis.5.2 The TSEC of soil or waste material may be used as aquantitative measure for the screening and selection of samplesfor chemical analysis.1These test methods are under the jurisdiction of ASTM Committee D34 onWaste Management and are the direct responsibili
14、ty of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved Feb. 1, 2006. Published March 2006. Originallyapproved in 1993. Last previous edition approved in 2001 as D 5368 - 93(2001)2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service
15、at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3 The TSEC may be useful as a simpl
16、e and relativelyinexpensive quantitative indicator of changes occurring in thetotal extractable organic content of soil or waste materials.5.4 The detection limit of the TSEC depends upon thespecific procedures employed. Typical detection limits insolvent extracts (that is, without solvent pre-conce
17、ntration) forMethod A are more than 1000 g/g. For Method B typicaldetection limits are 20 to 100 g/g in the solvent extract. ForMethod C the typical detection limits are 3 to 20 g/g forsolutes in the solvent extract.5.5 The sensitivity of the methods can be adjusted byvarying the volume of solvent e
18、xtract prior to gravimetricresidue determination.6. Interferences6.1 Solvents, reagents, glassware, and other sample process-ing hardware may yield an unacceptable background relative tothe limit of detection required for the TSEC measurement. Amethod blank must be performed in order to demonstrate
19、theviability of the solvent and equipment used. Specific selectionof reagents and the purification of solvents by distillation inall-glass systems may be required when low levels (that is,20 % of the minimum TSEC concentration ofinterest) in the solvent will preclude the application of themethod for
20、 TSEC determinations in those cases. Residueignition and inorganic analysis are suggested to evaluate thispotential background.6.3 Organic interferences can arise from the extraction ofimpurities from inorganic drying agents. If this is suspected,the interference may be removed by rinsing the drying
21、 agentwith pure extraction solvent followed by oven drying of theinorganic drying agent.6.4 Inorganic constituents extractable from the waste by thesolvent selected will result in a positive interference in thedetermination of TSEC, unless removed prior to TSEC deter-mination. This potential for int
22、erference must be determined bythe analyst on a case by case basis using existing data and bestjudgment.7. Selection of the Extraction Solvent7.1 The selection of solvent for extraction and TSECdetermination will depend upon many factors, including thefollowing (see Table 1 for selected applications
23、):7.1.1 Boiling point of the solvent,7.1.2 Boiling point of the compounds or class of compoundsof interest,7.1.3 Tendency of the solvent and matrix to form emulsions,7.1.4 Solvent strength (that is, polarity, solubility of com-pounds of interest),7.1.5 Safety of solvent use (that is, toxicity, flamm
24、ability),7.1.6 Purity of solvent, and7.1.7 Solvent compatibility with analysis instrumentation.7.2 The analyst should demonstrate a recovery using aspiking procedure in the matrix of interest before using thisprocedure.7.3 The extract is exposed to temperatures approaching theboiling point of the so
25、lvent during the evaporation procedure.Consequently, one must ensure that heat-labile and morevolatile solutes that may be of interest are stable and recover-able by the method and the solvent of choice. Becauselow-boiling fractions are lost in solvent removal, reproducibleresults can only be obtain
26、ed by strict adherence to methoddetails.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, all reagents mustconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society where suchspeci
27、fications are available.4Other grades may be used, pro-vided it is first determined that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.8.2 When low concentrations of TSEC are to be determined(that is, 100 g/g in the waste) pesticide-gr
28、ade solvents (thatis, distilled in glass) are recommended. The solvent blank forTSEC and the specific constituents of interest must be below20 % of the reportable lower limit for the analysis.4“Reagent Chemicals, American Chemical Society Specifications,” Am. Chem.Soc., Washington, DC. For suggestio
29、ns on the testing of reagents not listed by theAmerican Chemical Society, see “Analar Standards for Laboratory U.K. Chemical,”BDH Ltd., Poole, Dorset, and the “United States Pharmacopeia.”D 5368 93 (2006)28.3 Acetone (CH3)2CO), technical grade.8.4 Explosion-Proof Oven or Furnace.8.5 Heating Mantles.
30、9. Precautions9.1 Some solvents (for example, benzene, chloroform, andcarbon tetrachloride) are suspected human carcinogens andmust be handled by approved methods.9.2 Explosive peroxides tend to form in ether solvent. Aconvenient means of testing for their presence is with E. M.Quant test paper.5Thi
31、s test should be performed beforeevaporation of any ether-bearing extract.9.3 The use of fume hoods with volatile and toxic solventsis mandatory.9.4 Flammable solvents must be protected from heat,sparks, or flames. Avoid buildup of vapors and eliminate allsources of ignition, especially nonexplosion
32、-proof electricalapparatus and heaters. Keep containers closed. Use withadequate ventilation. Store bulk solvents in safety cabinets.Remove only a one-day supply and keep it in a hood.9.5 Avoid prolonged breathing of vapor or spray mist andavoid prolonged or repeated skin contact for all organicsolv
33、ents. Consult Material Safety Data Sheets for recom-mended handling procedures and precautions.9.6 Samples containing odorous, known or suspected vola-tile materials, must be processed in a fume hood.9.7 Samples known or suspected of containing toxic orhazardous materials must be handled in a fume h
34、ood. Safetyinformation relative to the handling of any known toxicmaterials must be obtained and implemented prior to anysample handling.10. Sample and Sample Preparation10.1 Remove refrigerated solvent extract sample from stor-age and allow it to reach room temperature. Keep samplesealed to prevent
35、 evaporation.10.2 When sample has reached room temperature examineto ensure that the sample is homogeneous and does not containinsoluble matter. If necessary, remix and homogenize.10.3 Record sample identification information for the sol-vent extract. Record or measure, if necessary, the solventvolu
36、me of the extract to be analyzed. Note any changes in theextract volume from the volumetric mark, if available, on thestorage vial or container.Method AMicro-Determination of TSEC11. Apparatus11.1 Microsyringe, 250-L, or alternatively, a calibratedmicrodispenser capable of 200-L delivery. The delive
37、ry pre-cision should be to 1 %.11.2 Aluminum Foil Weighing Pans, Micro, approximately 1to 6-cm diameter. Purchase or fabricate from oil-free aluminumfoil.11.3 Analytical Semimicro Balance, capable of reading to0.00001 g.5E. M. Quant test paper, trademark of, and available from, MCB ManufacturingChem
38、ists, Inc., 2909 Highland Avenue, Cincinnati, OH 45212 has been foundsatisfactory for this purpose.TABLE 1 Selected Applications of Soxhlet Extraction for Extraction of Organic Constituents from Solid MatricesSample Matrix SolventCompounds or Constituents Extraction Time,h (cycles)Reference1) Sedime
39、nt 1,1,1-trichloro-1,2,2-trifluoroethane (freon) oil and grease 4 (80) (1)APlumb (1983)2) Sludges and similar materials 1,1,1-trichloro-1,2,2-trifluoroethane (freon) oil and grease 4 (80) (2) Standard Methods3) Sludges from sewage hexane then methanol total organic C oil, grease,fats24 (3) Strachan
40、(1983)4) Municipal wastewater suspendedsolids and activated carbonhexane/dichloromethane semi-volatile priority pollutants 24 (480) (4) Harrold (1982)5) Soil and housedust acetone/hexane (1:1) organochlorine insecticides 5 (60) (5) EPA (1980)6) Sediment dichloromethane phenols 8 (6) Goldberg (1980)7
41、) Soil a) acetone/n-hexane (1:1)b) acetonitrilec) 2-propanol/n-hexane (1:1)aldrin, dieldrinaldrin, dieldrinaldrin, dieldrin12 (554)14 (47)18 (108)(7) Chiba (1968)8) Soil chloroform/methanol (1:1) (other solventsalso studied)dieldrin 8 (160) (8) Saha (1969)9) Airborne particulates methanol (cyclohexa
42、ne also studied) gross organics 2 (9) Hill (1977)10) Airborne particulates benzene selected PAHs 46 (10) Pierce (1975)11) Airborne particulates numerous solvents studied selected PAHs 6 (11) Stanley (1967)12) Coke oven aerosol particulates benzene selected PAHs 2 (1820) (12) Broddin (1977)13) Artifi
43、cial aerosol particulates methanol/benzene selected PAHs 8 (80) (13) Cautreels (1976)methanol/benzene selected phthalates 16 (160)methanol/benzene selected aliphatics 2 (20)methanol selected nitrogen 4 (40)benzene aromatics 2 (20)selected nitrogenaromatics14) Activated carbon chloroformchloroform/et
44、hanolphenolsgross organics44 (440) (14) Pahl (1973)(15) Buelow (1973)15) Glass fiber filters 26 solvents and 24 binary mixtures total organic carbon 6 (16) Grosjean (1975)16) Surface sediments methanol then dichloromethane total oil hydrocarbon 48 (160) (17) Sporstol (1985)17) Bottom sediment hexane
45、/acetone/isooctane chlorinated benzenes 18 (18) Onuska (1985)18) Environmental particulates benzene chlorinated dioxins 16 (19) Lamparski (1980)19) Soils hexane/acetone/methanol DDT 12 (20) Nash (1972)AThe boldface numbers in parentheses refer to the list of references at the end of this standard.D
46、5368 93 (2006)311.4 Balance Table An electronic load-cell type balanceis recommended.11.5 Heating Lamp, 250-W reflector-type bulb in a heat-resistant fixture whose height above the sample may beconveniently adjusted.11.6 Forceps, 3 to 5-in., steel or nickel-plated steel.11.7 Desiccator with Desiccan
47、t.12. Procedure12.1 Dry an aluminum weighing dish for1hat1056 5C.Cool in a desiccator for 30 min. Remove the weighing dish andallow it to equilibrate in ambient air for 30 min. Continue airequilibration until a constant weight is obtained.12.2 With a 250-L syringe or microdispenser accuratelytransfe
48、r 200 L of solvent extract to a tared (or weighed)aluminum weighing dish.12.3 Place the weighing dish under a heat lamp at a distanceof 8 cm from the lamp for 1 min, or until dry, to allow thesolvent to evaporate.12.4 Place the weighing dish in a desiccator for 30 min,remove, and weigh to constant w
49、eight.12.5 If the residue weight of the 200-L solvent extractaliquot is less than 0.00010 g, then a larger volume of solventextract must be used for the TSEC determination by theapplication of Methods B or C.13. Calculation13.1 For TSEC of the sample, where no solvent pre-concentration was performed, calculate the TSEC as micro-grams of residue per gram of sample (g/g) using the followingequation:TSEC 5Rw! Ve! 106!Sw! Vr!(1)where:TSEC = total solvent extractable content, g/g,Rw = residue weight, g (that is, difference in weight ofthe tared aluminum wei
