ASTM D5830-95(2006)
(Test Method)Standard Test Method for Solvents Analysis in Hazardous Waste Using Gas Chromatography
Standard Test Method for Solvents Analysis in Hazardous Waste Using Gas Chromatography
SIGNIFICANCE AND USE
This test method is useful in identifying the major solvent constituents in hazardous waste samples. This test method is designed to support field or site assessments, recycling operations, plant operations, or pollution control programs.
SCOPE
1.1 This test method is used to determine qualitatively and quantitatively the presence of the following compounds in waste samples using gas chromatography. This test method is designed for use as a screening method with a typical reporting level of 0.1 %.
1.1.1 This compound list is a compilation of hazardous solvents and other constituents that are routinely seen in hazardous waste samples.
1.2 The scope of this test method may be expanded to include other volatile and semivolatile organic constituents.
1.2.1 Hydrocarbon mixtures such as kerosene and mineral spirits.
1.2.2 High-boiling organics, defined here as compounds which boil above n-Hexadecane.
1.2.3 Other organics that the analyst is able to identify, either through retention time data or gas chromatography/mass spectrometric (GC/MS) analysis.
1.3 Gas chromatographic methods are recommended for use only by, or under close supervision of, an experienced analyst.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D5830 − 95(Reapproved 2006)
Standard Test Method for
Solvents Analysis in Hazardous Waste Using Gas
Chromatography
This standard is issued under the fixed designation D5830; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.2 The scope of this test method may be expanded to
include other volatile and semivolatile organic constituents.
1.1 This test method is used to determine qualitatively and
1.2.1 Hydrocarbon mixtures such as kerosene and mineral
quantitatively the presence of the following compounds in
spirits.
waste samples using gas chromatography. This test method is
1.2.2 High-boiling organics, defined here as compounds
designedforuseasascreeningmethodwithatypicalreporting
which boil above n-Hexadecane.
level of 0.1%.
1.2.3 Other organics that the analyst is able to identify,
Dichodifluoromethane Tetrahydrofuran
either through retention time data or gas chromatography/mass
Trichlorofluoromethane Acetone
1,1,2-Trichloro-1,2,2- Methyl Ethyl Ketone spectrometric (GC/MS) analysis.
trifluoroethane MIBK
1.3 Gaschromatographicmethodsarerecommendedforuse
Methanol Cyclohexanone
Ethanol Ethyl Acetate
only by, or under close supervision of, an experienced analyst.
Isopropanol Propyl Acetate
1.4 This standard does not purport to address all of the
n-Propanol Butyl Acetate
Isobutanol Benzene
safety concerns, if any, associated with its use. It is the
n-Butanol Toluene
responsibility of the user of this standard to establish appro-
tert-Butanol Ethylbenzene
priate safety and health practices and determine the applica-
Methylene Chloride Xylenes
Chloroform Styrene
bility of regulatory limitations prior to use.
Carbon Tetrachloride Chlorobenzene
1,1-Dichloroethane Dichlorobenzenes
2. Referenced Documents
1,2-Dichloroethane Nitrobenzene
1,2-Dichloropropane Fluorobenzene
2.1 ASTM Standards:
1,1-Dichloroethylene n-Propyl Benzene
D1193Specification for Reagent Water
1,2-Dichloroethene Isopropyl Benzene
1,1,1-Trichloroethane Isobutyl Benzene 2.2 EPA Document:
Tetrachloroethylene n-Butyl Benzene
Gas Chromatography/Mass Spectrometry Method8260,
Trichloroethylene 2-Ethoxyethanol
Test Methods for Evaluating Solid Waste Physical/
Tetrachloroethane 2-Butoxyethanol
Chemical Methods, SW-846, Third Edition, Final Update
Cyclopentane 2-Ethoxyethanol Acetate
Pentane 2-Methoxyethanol
1, July 1992
Hexane Bromoform
Heptane Carbitol
3. Summary of Test Method
Cyclohexane Ethyl Ether
Isooctane 1,4-Dioxane
3.1 Waste samples are analyzed by direct injection, or by
Nitropropane Diacetone Alcohol
carbon disulfide, M-Pyrol, or other suitable solvent extraction
Ethanolamine Acetonitrile
Nitromethane Pyridine
and injection of the extract into a gas chromatograph. Detec-
Ethylene Chloride Toluidine
tion is achieved using a detector which is specific for the
Benzyl Chloride Ethylene Glycol
needed application, for example, flame ionization detector
Propylene Glycol
(FID), electron capture detector (ECD), thermal conductivity
1.1.1 This compound list is a compilation of hazardous
detector (TCD), photoionization detector (PID), or mass selec-
solvents and other constituents that are routinely seen in
tive detector (MSD). This test method may be expanded to
hazardous waste samples.
utilize other detector types not previously mentioned.
1 2
This test method is under the jurisdiction ofASTM Committee D34 on Waste For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Management and is the direct responsibility of Subcommittee D34.01.06 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Analytical Methods. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Feb. 1, 2006. Published March 2006. Originally the ASTM website.
approved in 1995. Last previous edition approved in 2001 as D5830–95(2001). Available from the Superintendent of Documents, U.S. Government Printing
DOI: 10.1520/D5830-95R06. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5830 − 95 (2006)
FIG. 1 Daily QC Standard FID/DB-1701
4. Significance and Use 5.1.4 Sample history, for example, any information avail-
able from the waste generator; and,
4.1 This test method is useful in identifying the major
5.1.5 Physical characteristics, for example, flammability,
solvent constituents in hazardous waste samples. This test
specific gravity, or miscibility with water.
method is designed to support field or site assessments,
recycling operations, plant operations, or pollution control
5.2 Interferences may also be encountered from syringe
programs.
carryover. Immediately following each injection, the syringe
should be thoroughly rinsed with carbon disulfide, or M-Pyrol.
5. Interferences
Other solvents such as methanol may be used as rinse solvents
5.1 Interferences may be encountered from any number of
if sample types necessitate their use, but be aware that
organic compounds that respond in the detector. Also, closely
carryover and possible interferences may occur if the rinse
elutingcomponentsmaycomplicateidentificationbasedsolely solvent is not completely cleaned from the syringe before
on retention time. When these types of interferences are
reuse. Before each injection the syringe must be thoroughly
encountered, the analyst must rely on other sources of infor- rinsed with the sample to be injected, where the first two
mation for positive identification, such as:
pumps are flushed into a separate waste receptacle.
5.1.1 Gas chromatography/mass spectrometric (GC/MS)
5.3 When carbon disulfide (CS ) is used to extract solids or
confirmation, see EPA Method8260, direct injection tech-
sludgesthatcontainsignificantamountsofwater,lowrecovery
nique;
of the water miscible solvents may result.
5.1.2 Useofconfirmationcolumn,orconfirmatorydetector;
5.1.3 Use of varying temperature programs or standard 5.4 Some grades of CS may contain trace amounts of
comparison, or both; benzene.
D5830 − 95 (2006)
5.5 M-Pyrol seems to degrade slowly with time. The low- such specifications are available. Other grades may be used,
level degradation products interfere with some late eluting provided it is first ascertained that the reagent is of sufficiently
compounds on some columns (approximately five small high purity to permit its use without lessening the accuracy of
peaks). the determination.
5.6 Interference from the CS solvent peak may occur if 7.2 Purity of Water—Unlessotherwiseindicated,references
to water shall be understood to mean reagent water as defined
using a TCD.
by Type II of Specification D1193.
5.7 When using a TCD, be aware that water, as well as
7.3 Nitrogen or Helium (High Purity)—For carrier and
oxygenated compounds, for example, MEK, MIBK, may
makeup gases. Air and hydrogen (high purity) for fuel gases.
suppress detector response.
Gases may be obtained from a gas generator if available,
5.8 If an electrolytic conductivity detector (ECD) must be
through purification of a lower grade, or from a high-purity
used, be aware that CS , M-Pyrol, and high concentrations of
tank supply.
halogenated compounds may overload and possibly damage
7.4 Carbon Disulfide, CS —Chromatography grade.
the detector. It is recommended that the ECD be used only 2
when very low detection levels of halogenated compounds are
7.5 M-Pyrol, C H NO—Available through several chemical
o o
expected and direct injection of the sample is possible.
suppliers and sources as 1-methyl-2-pyrrolidone.
7.6 Individual Standards for Each Component of Interest—
6. Apparatus
99% purity available from many vendors.
6.1 Gas Chromatograph System—Equipped with capillary
or packed column injection ports, or both, detector, and data
8. Standard Preparation
system.
8.1 Stock Standard Solutions—Stock standards are prepared
6.2 Recommended Chromatographic Columns:
from pure standard materials. It is recommended that the
6.2.1 Capillary; Microbore or Megabore.
standards be prepared so that each component is 5 to 10% by
weight. The stock standards must be prepared by directly
6.2.1.1 DB-1701,30M×0.25-mminsidediameter,0.25-µm
weighingeachcomponent.Forextremelyvolatilecomponents,
film thickness.
such as ether and freons, it is recommended that a new stock
6.2.1.2 DB-624, 30M×0.3-mm inside diameter, 1.8-µm
standard be prepared daily or as needed. If a dilution solvent is
film thickness.
needed when preparing the stock standards, use the same
6.2.2 Packed: Stainless Steel or Glass.
solvent used for sample extraction or dilution in Section 7.
6.2.2.1 1% SP-1000, 60/80 Carbopak B, 8-ft by ⁄8-in.
inside diameter. NOTE 2—Due to the incompatibility of some standard compounds, that
is, some compounds are not miscible with each other, and also because of
6.2.2.2 10% SP-2100, 100/120 Chromosorb WHP, 2M×2
the number of compounds typically looked for in a single chromato-
mm ID.
graphic run, it is advisable to prepare 3 or 4 standard solutions each
composed of 10 to 15 compounds. A set of standard chromatograms and
NOTE 1—These columns are recommended and have shown to give
a retention timetable should be available for reference.
good results. Operating conditions for each is listed in Section 10.
Equivalent or alternative columns, or both, may be used depending on 8.2 Secondary Working Standards—These are prepared
application.
from stock standard solutions using the appropriate solvent.
Secondary standards should encompass the linear range of the
6.3 Glass Screw-Cap Vials or Equivalent—To collect
GC system.
samples and store standards. Polytetrafluoroethylene or other
inert material should be used for the cap liner.
NOTE 3—Linear response and range must be established with all
detectors and chromatography systems used for quantitation. All calibra-
6.4 Microsyringes, 1.0, 10, and 100 µL.
tionandsampleanalysismustbedonewithintheestablishedlinearrange.
6.5 Analytical Balance, accurate to 0.0001 g.
8.3 Calibration Check Standard—A calibration check stan-
dard should be prepared. The standard mixture should provide
6.6 Pipettes, glass, disposable, or volumetric micropipettor
a good overall check of the GC/detector system. The com-
or equivalent.
pounds should cover the major compound types, for example,
6.7 Microdisk Filters, 0.45, 1.0, or 5.0 µm, optional.
alcohols, aromatics, aliphatics, ketones, and halogenates. A
typical calibration check standard flame ionization detector
6.8 Centrifuge, optional.
(FID) chromatogram is shown in Fig. 1.
6.9 Vortex-Type Mixer.
7. Reagents and Materials
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
7.1 Purity of Reagents—Reagent grade chemicals shall be
listed by the American Chemical Society, see Analar Standards for Laboratory
used in all tests. Unless otherwise indicated, it is intended that
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
all reagents conform to the specifications of the Committee on
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Analytical Reagents of theAmerican Chemical Society where MD.
D5830 − 95 (2006)
9. Sample Collection, Preservation, and Handling
Peak width 0.04 min
9.1 Sample collection should be in accordance with appro- NOTE 4—Typical chromatograms are shown in Figs. 2-5.
priate sampling protocols.
10.2.2 For Capillary DB-624 with FID
9.2 Samples should be collected in glass containers, that
Column flow rate 3.5 mL/min
Make-up gas flow 29 mL/min
have tightly sealing caps. If very volatile organics are of
Airflow (FID) Approximately 300 mL/min
particular interest, the headspace in the container should be
Hydrogen flow (FID) Approximately 30 mL/min
kept to a minimum.
Injector temperature 275°C
Detector temperature 275°C
9.3 Sample Transfer Implements—Implements are required
Initial oven temperature 35°C
to transfer portions of waste samples from the sample contain- Initial time 5 min
Level 1 rate 5°C/min
ers to the laboratory containers. Liquid samples may be
Level 1 final value 150°C
transferred using disposable pipets. Solids and semisolids may
Level 1 hold time 4 min
be transferred using a conventional laboratory spatula. Level 2 rate 20°C/min
Level 2 final value 225°C
9.4 Samples shall be handled maintaining safe laboratory
Run time 45 min
practices.Any samples with special hazards must be appropri-
10.2.3 For Packed SP-1000 with FID
ately labeled.
Column flow rate 40 mL/min
9.5 Unusedsamplematerial,laboratorydilutions,andwaste Air pressure (FID) 300 kPa
Hydrogen pressure (FID) 130 kPa
from the samples may be regulated. Consult your specialist or
Injector temperature 250°C
the regulations, or both, for guidance in the proper handling
Detector temperature 250°C
Initial oven temperature 90°C
and disposal of laboratory wastes.
Initial time 6 min
Level 1 rate 3°C/min
10. Procedure
Level 1 final value 120°C
10.1 Sample Preparation: Level 2 rate 5°C/min
Level 2 final value 180°C
10.1.1 Analyze liquid matrices with relatively low viscosity
Level 3 rate 10°C/min
using direct injection into the GC, either as received or after
Level 3 final value 230°C
dilution with CS , M-Pyrol, or other suitable solvent. Run time 46 min
10.1.2 Analyze solid or semisolid samples as follows:
10.2.4 For packed SP-2100 with FID
10.1.2.1 Forcarbondisulfideor M-Pyrolpreparation,weigh
Carrier gas flow 30 mL/min
3 g of the waste sample in a 15-mL glass vial. Add3gof
Injector temperatuare 250°C
Detector temperature 300°C
carbon disulfide or M-Pyrol to the vial and the mixture is
Airflow (FID) Approximately 300 mL/min
vortexed vigorously. After allowing the solids to settle, inject
Hydrogen flow (FID) Approximately 30 mL/min
the CS or M-Pyrol extract into the GC.
2 Initial oven temperature 45°C
Initial hold time 3 min
10.1.2.2 Use alternate sample sizes and extraction solvent
Level 1 rate 15°C/min
weights if necessary. Actual sample size and solvent weight
Level 1 final value 90°C
must be recorded in the appropriate sample preparation log
Level 2 rate 10°C/min
Level 2 final value 195°C
book. It is essential for accurate waste sample analysis that
Run time 16.5 min
sample size be sufficient to ensure a representative sample. If
10.3 Linear Range Determination—The linearity and linear
alternate sample size or extraction solvent volumes, or both,
range for each compound must be established on any GC
are used, this m
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