ASTM D5368-93(2006)
(Test Method)Standard Test Methods for Gravimetric Determination of Total Solvent Extractable Content (TSEC) of Solid Waste Samples
Standard Test Methods for Gravimetric Determination of Total Solvent Extractable Content (TSEC) of Solid Waste Samples
SIGNIFICANCE AND USE
The TSEC provides a quantitative measure of the total solvent extractable organic content of the solid waste in question. Based upon the TSEC, the extract may be analyzed or further processed (that is, further cleanup or solvent concentration) in preparation for analysis. Thus, the TSEC provides a quantitative measure for optimizing the extractable organic concentration prior to chemical analysis.
The TSEC of soil or waste material may be used as a quantitative measure for the screening and selection of samples for chemical analysis.
The TSEC may be useful as a simple and relatively inexpensive quantitative indicator of changes occurring in the total extractable organic content of soil or waste materials.
The detection limit of the TSEC depends upon the specific procedures employed. Typical detection limits in solvent extracts (that is, without solvent pre-concentration) for Method A are more than 1000 μg/g. For Method B typical detection limits are 20 to 100 μg/g in the solvent extract. For Method C the typical detection limits are 3 to 20 μg/g for solutes in the solvent extract.
The sensitivity of the methods can be adjusted by varying the volume of solvent extract prior to gravimetric residue determination.
SCOPE
1.1 These test methods describe standard procedures for gravimetrically determining the total nonvolatile and semi-volatile organic content of solvent extracts from soils or solid wastes. The following methods are included: SectionMethod A-Micro-Determination of TSECMethod B-Evaporating Dish ProcedureMethod C-Boiling Flask Procedure
1.2 These methods are used after a solvent extract is obtained from a soil or solid waste. For these methods to be applicable, the extraction solvent must have a boiling point less than 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 solvent and method used for the extraction procedure.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5368 − 93(Reapproved 2006)
Standard Test Methods for
Gravimetric Determination of Total Solvent Extractable
Content (TSEC) of Solid Waste Samples
This standard is issued under the fixed designation D5368; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D5369 Practice for Extraction of Solid Waste Samples for
Chemical Analysis Using Soxhlet Extraction
1.1 These test methods describe standard procedures for
gravimetrically determining the total nonvolatile and semi-
3. Terminology
volatile organic content of solvent extracts from soils or solid
3.1 Definitions:
wastes. The following methods are included:
3.1.1 total solvent extractable content (TSEC)— the total
Section
concentration by weight (w/w) of organic materials that is
Method A—Micro-Determination of TSEC 11-13
Method B—Evaporating Dish Procedure 14-16
extractable from a soil or solid waste by the selected solvent.
Method C—Boiling Flask Procedure 17-19
1.2 These methods are used after a solvent extract is
4. Summary of Methods
obtained from a soil or solid waste. For these methods to be
4.1 The sample is extracted with an organic solvent using a
applicable,theextractionsolventmusthaveaboilingpointless
procedure such as described in Practices D5369 (Soxhlet
than that of water at ambient pressure.
Extraction) or Test Method D4281. The quantity of material
1.3 The total solvent extractable content (TSEC) of a soil,
extracted into the solvent is determined as the residue weight
sediment, sludge, or solid waste depends upon the solvent and
after solvent evaporation. Similar ASTM methods are Test
method used for the extraction procedure.
Methods D2109 and D3445, and Practice D2910.
4.1.1 MethodA,Micro-DeterminationMethod—Theresidue
2. Referenced Documents
weight after solvent evaporation is determined for 200 µL of
solvent extract evaporated on an aluminum weighing dish. A
2.1 ASTM Standards:
heat lamp is used to effect evaporation.
D2109 Test Methods for Nonvolatile Matter in Halogenated
4.1.2 Method B, Evaporating Dish Procedure—The residue
Organic Solvents and Their Admixtures
weight after solvent evaporation is determined for 1.0 to 75.0
D2910 Method for Removal of Organic Matter from Water
mL of solvent extract. Solvent is evaporated in an evaporating
by Activated Carbon Absorption (Withdrawn 1991)
dish by heating at 5°C below the solvent boiling point. A
D3086 Test Method for Organochlorine Pesticides in Water
stream of nitrogen over the surface of the solvent is used to
(Withdrawn 1996)
accelerate evaporation.
D3445 Method of Test for Nonvolatile Matter in Trichloro-
4.1.3 Method C, Boiling Flask Method—The residue weight
trifluoroethane (Withdrawn 1991)
after solvent evaporation is determined for 100 to 300 mL of
D3694 Practices for Preparation of Sample Containers and
solvent evaporated in a boiling flask. Solvent is evaporated in
for Preservation of Organic Constituents
a water bath at the solvent boiling point.
D4281 Test Method for Oil and Grease (Fluorocarbon Ex-
tractable Substances) by Gravimetric Determination
5. Significance and Use
5.1 The TSEC provides a quantitative measure of the total
These test methods are under the jurisdiction of ASTM Committee D34 on
solvent extractable organic content of the solid waste in
Waste Management and are the direct responsibility of Subcommittee D34.01.06 on
question.BasedupontheTSEC,theextractmaybeanalyzedor
Analytical Methods.
further processed (that is, further cleanup or solvent concen-
Current edition approved Feb. 1, 2006. Published March 2006. Originally
approved in 1993. Last previous edition approved in 2001 as D5368 - 93(2001)
tration) in preparation for analysis. Thus, the TSEC provides a
DOI: 10.1520/D5368-93R06.
quantitative measure for optimizing the extractable organic
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
concentration prior to chemical analysis.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
5.2 The TSEC of soil or waste material may be used as a
the ASTM website.
quantitativemeasureforthescreeningandselectionofsamples
The last approved version of this historical standard is referenced on
www.astm.org. for chemical analysis.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5368 − 93 (2006)
5.3 The TSEC may be useful as a simple and relatively interest) in the solvent will preclude the application of the
inexpensive quantitative indicator of changes occurring in the method for TSEC determinations in those cases. Residue
total extractable organic content of soil or waste materials. ignition and inorganic analysis are suggested to evaluate this
potential background.
5.4 The detection limit of the TSEC depends upon the
6.3 Organic interferences can arise from the extraction of
specific procedures employed. Typical detection limits in
solvent extracts (that is, without solvent pre-concentration) for impurities from inorganic drying agents. If this is suspected,
the interference may be removed by rinsing the drying agent
Method A are more than 1000 µg/g. For Method B typical
detection limits are 20 to 100 µg/g in the solvent extract. For with pure extraction solvent followed by oven drying of the
inorganic drying agent.
Method C the typical detection limits are 3 to 20 µg/g for
solutes in the solvent extract.
6.4 Inorganic constituents extractable from the waste by the
solvent selected will result in a positive interference in the
5.5 The sensitivity of the methods can be adjusted by
determination of TSEC, unless removed prior to TSEC deter-
varying the volume of solvent extract prior to gravimetric
mination.Thispotentialforinterferencemustbedeterminedby
residue determination.
the analyst on a case by case basis using existing data and best
judgment.
6. Interferences
6.1 Solvents,reagents,glassware,andothersampleprocess-
7. Selection of the Extraction Solvent
inghardwaremayyieldanunacceptablebackgroundrelativeto
7.1 The selection of solvent for extraction and TSEC
the limit of detection required for the TSEC measurement. A
determination will depend upon many factors, including the
method blank must be performed in order to demonstrate the
following (see Table 1 for selected applications):
viability of the solvent and equipment used. Specific selection
7.1.1 Boiling point of the solvent,
of reagents and the purification of solvents by distillation in
7.1.2 Boilingpointofthecompoundsorclassofcompounds
all-glass systems may be required when low levels (that is,
of interest,
<100 µg/g) of TSEC are of interest.
7.1.3 Tendencyofthesolventandmatrixtoformemulsions,
6.1.1 Glassware should be cleaned by washing with deter-
7.1.4 Solvent strength (that is, polarity, solubility of com-
gent or non-chromate cleaning solution, rinsing first with tap
pounds of interest),
water, then reagent water, then redistilled acetone, and finally
7.1.5 Safety of solvent use (that is, toxicity, flammability),
with pesticide quality solvent (that is, the solvent used for
7.1.6 Purity of solvent, and
extraction). For additional information, see Practices D3694.If
7.1.7 Solvent compatibility with analysis instrumentation.
the type and size of glassware permits, it may be cleaned by
7.2 The analyst should demonstrate a recovery using a
heating in a muffle furnace at 400°C for 15 to 30 min.
spiking procedure in the matrix of interest before using this
Alternatively, glassware may be oven dried at 103°C for at
procedure.
least 1 h, after solvent rinsing and draining. Volumetric
glassware should not be heated in a muffle furnace.
7.3 The extract is exposed to temperatures approaching the
6.1.2 Plastics,exceptPTFE-fluorocarbon,canbeasourceof
boiling point of the solvent during the evaporation procedure.
serious interference, especially when specific organic constitu-
Consequently, one must ensure that heat-labile and more
ents are of analytical interest. Their use must be avoided.
volatile solutes that may be of interest are stable and recover-
Extracted samples should be stored in glass bottles with
able by the method and the solvent of choice. Because
PTFE-fluorocarbon-lined caps. Extraction solvent volumes
low-boiling fractions are lost in solvent removal, reproducible
should be recorded and containers sealed to prevent solvent
results can only be obtained by strict adherence to method
evaporation or cross contamination. Extracts should be refrig-
details.
erated above the freezing point of the solvent.
8. Reagents and Materials
6.1.3 If required, rinse glassware and utensils with extrac-
tion solvent prior to use in order to remove interferences. The
8.1 Purity of Reagents—Reagent grade chemicals shall be
method blank should be less than 20 % of the minimum
used in all tests. Unless otherwise indicated, all reagents must
reportable concentration.
conform to the specifications of the Committee on Analytical
6.1.4 Impurities in the extracting solvent can be a source of
Reagents of the American Chemical Society where such
interferences or TSEC background. Solvent blanks should be
specifications are available. Other grades may be used, pro-
analyzed with each new bottle of solvent. Whenever a high
vided it is first determined that the reagent is of sufficiently
TSEC background, or interfering compounds are traced to the
high purity to permit its use without lessening the accuracy of
solvent, a new source of solvent should be obtained.
the determination.
Alternatively, impurities can often be removed by distillation
8.2 When low concentrations of TSEC are to be determined
in glass.
(that is, <100 µg/g in the waste) pesticide-grade solvents (that
6.2 Arelatively highTSEC background can also result from
inorganic drying agents (that is, Na SO , MgSO , CuSO ,
2 4 4 4
“Reagent Chemicals, American Chemical Society Specifications,” Am. Chem.
CaCl , CaSO,K CO , KOH, BaO, CaO, H SO,P O)inthe
2 4 2 3 2 4 2 5
Soc., Washington, DC. For suggestions on the testing of reagents not listed by the
extracting solvent.Arelatively high background of any drying
American Chemical Society, see “Analar Standards for Laboratory U.K. Chemical,”
agent used (>20 % of the minimum TSEC concentration of BDH Ltd., Poole, Dorset, and the “United States Pharmacopeia.”
D5368 − 93 (2006)
TABLE 1 Selected Applications of Soxhlet Extraction for Extraction of Organic Constituents from Solid Matrices
Compounds or Constituents Extraction Time,
Sample Matrix Solvent Reference
h (cycles)
A
1) Sediment 1,1,1-trichloro-1,2,2-trifluoroethane (freon) oil and grease 4 (80) (1) Plumb (1983)
2) Sludges and similar materials 1,1,1-trichloro-1,2,2-trifluoroethane (freon) oil and grease 4 (80) (2) Standard Methods
3) Sludges from sewage hexane then methanol total organic C oil, grease, 24 (3) Strachan (1983)
fats
4) Municipal wastewater suspended hexane/dichloromethane semi-volatile priority pollutants 24 (480) (4) Harrold (1982)
solids and activated carbon
5) Soil and housedust acetone/hexane (1:1) organochlorine insecticides 5 (60) (5) EPA (1980)
6) Sediment dichloromethane phenols 8 (6) Goldberg (1980)
7) Soil a) acetone/n-hexane (1:1) aldrin, dieldrin 12 (554) (7) Chiba (1968)
b) acetonitrile aldrin, dieldrin 14 (47)
c) 2-propanol/n-hexane (1:1) aldrin, dieldrin 18 (108)
8) Soil chloroform/methanol (1:1) (other solvents dieldrin 8 (160) (8) Saha (1969)
also studied)
9) Airborne particulates methanol (cyclohexane also studied) gross organics 2 (9) Hill (1977)
10) Airborne particulates benzene selected PAHs 4–6 (10) Pierce (1975)
11) Airborne particulates numerous solvents studied selected PAHs 6 (11) Stanley (1967)
12) Coke oven aerosol particulates benzene selected PAHs 2 (18–20) (12) Broddin (1977)
13) Artificial 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 nitrogen
aromatics
14) Activated carbon chloroform phenols 44 (440) (14) Pahl (1973)
chloroform/ethanol gross organics (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/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)
A
The boldface numbers in parentheses refer to the list of references at the end of this standard.
is, distilled in glass) are recommended. The solvent blank for adequate ventilation. Store bulk solvents in safety cabinets.
TSEC and the specific constituents of interest must be below Remove only a one-day supply and keep it in a hood.
20 % of the reportable lower limit for the analysis.
9.5 Avoid prolonged breathing of vapor or spray mist and
8.3 Acetone ((CH ) CO), technical grade. avoid prolonged or repeated skin contact for all organic
3 2
solvents. Consult Material Safety Data Sheets for recom-
8.4 Explosion-Proof Oven or Furnace.
mended handling procedures and precautions.
8.5 Heating Mantles.
9.6 Samples containing odorous, known or suspected vola-
tile materials, must be processed in a fume hood.
9. Precautions
9.7 Samples known or suspected of containing toxic or
9.1 Some solvents (for example, benzene, chloroform, and
hazardous materials must be handled in a fume hood. Safety
carbon tetrachloride) are suspected human carcinogens and
information relative to the handling of any known toxic
must be handled by approved methods.
materials must be obtained and implemented prior to any
9.2 Explosive peroxides tend to form in ether solvent. A
sample handling.
convenient means of testing for their presence is with E. M.
10. Sample and Sample Preparation
Quant test paper. This test should be performed before
evaporation of any ether-bearing extract.
10.1 Remove refrigerated solvent extract sample from stor-
age and allow it to reach room temperature. Keep sample
9.3 The use of fume hoods with volatile and toxic solvents
sealed to prevent evaporation.
is mandatory.
10.2 When sample has reached room temperature examine
9.4 Flammable solvents must be protected from heat,
to ensure that the sample is homogeneous and does not
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.