ASTM D5830-95
(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
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 %.DichodifluoromethaneTetrahydrofuranTrichlorofluoromethaneAcetone1,1,2-Trichloro-1,2,2-Methyl Ethyl KetonetrifluoroethaneMIBKMethanolCyclohexanoneEthanol Ethyl AcetateIsopropanolPropyl Acetaten-PropanolButyl AcetateIsobutanolBenzenen-ButanolToluenetert-ButanolEthylbenzeneMethylene ChlorideXylenesChloroformStyreneCarbon TetrachlorideChlorobenzene1,1-DichloroethaneDichlorobenzenes1,2-DichloroethaneNitrobenzene1,2-DichloropropaneFluorobenzene1,1-Dichloroethylenen-Propyl Benzene>1,2-DichloroetheneIsopropyl Benzene1,1,1-TrichloroethaneIsobutyl BenzeneTetrachloroethylenen-Butyl BenzeneTrichloroethylene2-EthoxyethanolTetrachloroethane2-ButoxyethanolCyclopentane2-Ethoxyethanol AcetatePentane 2-MethoxyethanolHexane BromoformHeptane CarbitolCyclohexaneEthyl EtherIsooctane1,4-DioxaneNitropropaneDiacetone AlcoholEthanolamineAcetonitrileNitromethanePyridineEthylene ChlorideToluidineBenzyl ChlorideEthylene Glycol Propylene Glycol
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.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.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.
Designation: D 5830 – 95
Standard Test Method for
Solvents Analysis in Hazardous Waste Using Gas
Chromatography
This standard is issued under the fixed designation D 5830; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 1.2.1 Hydrocarbon mixtures such as kerosene and mineral
spirits.
1.1 This test method is used to determine qualitatively and
1.2.2 High-boiling organics, defined here as compounds
quantitatively the presence of the following compounds in
which boil above n-Hexadecane.
waste samples using gas chromatography. This test method is
1.2.3 Other organics that the analyst is able to identify,
designed for use as a screening method with a typical reporting
either through retention time data or gas chromatography/mass
level of 0.1 %.
spectrometric (GC/MS) analysis.
Dichodifluoromethane Tetrahydrofuran
1.3 Gas chromatographic methods are recommended for use
Trichlorofluoromethane Acetone
1,1,2-Trichloro-1,2,2- Methyl Ethyl Ketone
only by, or under close supervision of, an experienced analyst.
trifluoroethane MIBK
1.4 This standard does not purport to address all of the
Methanol Cyclohexanone
safety concerns, if any, associated with its use. It is the
Ethanol Ethyl Acetate
Isopropanol Propyl Acetate
responsibility of the user of this standard to establish appro-
n-Propanol Butyl Acetate
priate safety and health practices and determine the applica-
Isobutanol Benzene
bility of regulatory limitations prior to use.
n-Butanol Toluene
tert-Butanol Ethylbenzene
Methylene Chloride Xylenes
2. Referenced Documents
Chloroform Styrene
2.1 ASTM Standards:
Carbon Tetrachloride Chlorobenzene
1,1-Dichloroethane Dichlorobenzenes
D 1193 Specification for Reagent Water
1,2-Dichloroethane Nitrobenzene
2.2 EPA Document:
1,2-Dichloropropane Fluorobenzene
1,1-Dichloroethylene n-Propyl Benzene Gas Chromatography/Mass Spectrometry Method 8260,
1,2-Dichloroethene Isopropyl Benzene
Test Methods for Evaluating Solid Waste Physical/
1,1,1-Trichloroethane Isobutyl Benzene
Chemical Methods, SW-846, Third Edition, Final Update
Tetrachloroethylene n-Butyl Benzene
1, July 1992
Trichloroethylene 2-Ethoxyethanol
Tetrachloroethane 2-Butoxyethanol
Cyclopentane 2-Ethoxyethanol Acetate
3. Summary of Test Method
Pentane 2-Methoxyethanol
3.1 Waste samples are analyzed by direct injection, or by
Hexane Bromoform
Heptane Carbitol
carbon disulfide, M-Pyrol, or other suitable solvent extraction
Cyclohexane Ethyl Ether
and injection of the extract into a gas chromatograph. Detec-
Isooctane 1,4-Dioxane
tion is achieved using a detector which is specific for the
Nitropropane Diacetone Alcohol
Ethanolamine Acetonitrile
needed application, for example, flame ionization detector
Nitromethane Pyridine
(FID), electron capture detector (ECD), thermal conductivity
Ethylene Chloride Toluidine
Benzyl Chloride Ethylene Glycol detector (TCD), photoionization detector (PID), or mass selec-
Propylene Glycol
tive detector (MSD). This test method may be expanded to
utilize other detector types not previously mentioned.
1.1.1 This compound list is a compilation of hazardous
solvents and other constituents that are routinely seen in
4. Significance and Use
hazardous waste samples.
4.1 This test method is useful in identifying the major
1.2 The scope of this test method may be expanded to
solvent constituents in hazardous waste samples. This test
include other volatile and semivolatile organic constituents.
method is designed to support field or site assessments,
This test method is under the jurisdiction of ASTM Committee D-34 on Waste
Management and is the direct responsibility of Subcommittee D34.02 on Physical Annual Book of ASTM Standards, Vol 11.01.
and Chemical Characterization. Available from the Superintendent of Documents, U.S. Government Printing
Current edition approved Sept. 10, 1995. Published November 1995. Office, Washington, DC 20402.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5830
recycling operations, plant operations, or pollution control should be thoroughly rinsed with carbon disulfide, or M-Pyrol.
programs. Other solvents such as methanol may be used as rinse solvents
if sample types necessitate their use, but be aware that
5. Interferences
carryover and possible interferences may occur if the rinse
5.1 Interferences may be encountered from any number of
solvent is not completely cleaned from the syringe before
organic compounds that respond in the detector. Also, closely
reuse. Before each injection the syringe must be thoroughly
eluting components may complicate identification based solely
rinsed with the sample to be injected, where the first two
on retention time. When these types of interferences are
pumps are flushed into a separate waste receptacle.
encountered, the analyst must rely on other sources of infor-
5.3 When carbon disulfide (CS ) is used to extract solids or
mation for positive identification, such as:
sludges that contain significant amounts of water, low recovery
5.1.1 Gas chromatography/mass spectrometric (GC/MS)
of the water miscible solvents may result.
confirmation, see EPA Method 8260, direct injection tech-
5.4 Some grades of CS may contain trace amounts of
nique;
benzene.
5.1.2 Use of confirmation column, or confirmatory detector;
5.5 M-Pyrol seems to degrade slowly with time. The low-
5.1.3 Use of varying temperature programs or standard
level degradation products interfere with some late eluting
comparison, or both;
compounds on some columns (approximately five small
5.1.4 Sample history, for example, any information avail-
peaks).
able from the waste generator; and,
5.6 Interference from the CS solvent peak may occur if
5.1.5 Physical characteristics, for example, flammability, 2
using a TCD.
specific gravity, or miscibility with water.
5.2 Interferences may also be encountered from syringe 5.7 When using a TCD, be aware that water, as well as
carryover. Immediately following each injection, the syringe oxygenated compounds, for example, MEK, MIBK, may
FIG. 1 Daily QC Standard FID/DB-1701
D 5830
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 7.5 M-Pyrol, C H NO—Available through several chemi-
o o
when very low detection levels of halogenated compounds are cal suppliers and sources as 1-methyl-2-pyrrolidone.
expected and direct injection of the sample is possible. 7.6 Individual Standards for Each Component of Interest—
99 % purity available from many vendors.
6. Apparatus
8. Standard Preparation
6.1 Gas Chromatograph System—Equipped with capillary
8.1 Stock Standard Solutions—Stock standards are prepared
or packed column injection ports, or both, detector, and data
from pure standard materials. It is recommended that the
system.
standards be prepared so that each component is 5 to 10 % by
6.2 Recommended Chromatographic Columns:
weight. The stock standards must be prepared by directly
6.2.1 Capillary; Microbore or Megabore.
weighing each component. For extremely volatile components,
6.2.1.1 DB-1701, 30M 3 0.25-mm inside diameter,
such as ether and freons, it is recommended that a new stock
0.25-μm film thickness.
standard be prepared daily or as needed. If a dilution solvent is
6.2.1.2 DB-624, 30M 3 0.3-mm inside diameter, 1.8-μm
needed when preparing the stock standards, use the same
film thickness.
solvent used for sample extraction or dilution in Section 7.
6.2.2 Packed: Stainless Steel or Glass.
6.2.2.1 1 % SP-1000, 60/80 Carbopak B, 8-ft by ⁄8-in.
NOTE 2—Due to the incompatibility of some standard compounds, that
inside diameter. is, some compounds are not miscible with each other, and also because of
the number of compounds typically looked for in a single chromato-
6.2.2.2 10 % SP-2100, 100/120 Chromosorb WHP, 2M 3 2
graphic run, it is advisable to prepare 3 or 4 standard solutions each
mm ID.
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.
8.2 Secondary Working Standards—These are prepared
Equivalent or alternative columns, or both, may be used depending on
from stock standard solutions using the appropriate solvent.
application.
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
NOTE 3—Linear response and range must be established with all
inert material should be used for the cap liner.
detectors and chromatography systems used for quantitation. All calibra-
6.4 Microsyringes, 1.0, 10, and 100 μL.
tion and sample analysis must be done within the established linear range.
6.5 Analytical Balance, accurate to 0.0001 g.
8.3 Calibration Check Standard—A calibration check stan-
6.6 Pipettes, glass, disposable, or volumetric micropipettor
dard should be prepared. The standard mixture should provide
or equivalent.
a good overall check of the GC/detector system. The com-
6.7 Microdisk Filters, 0.45, 1.0, or 5.0 μm, optional.
pounds should cover the major compound types, for example,
6.8 Centrifuge, optional.
alcohols, aromatics, aliphatics, ketones, and halogenates. A
6.9 Vortex-Type Mixer.
typical calibration check standard flame ionization detector
7. Reagents and Materials
(FID) chromatogram is shown in Fig. 1.
7.1 Purity of Reagents—Reagent grade chemicals shall be
9. Sample Collection, Preservation, and Handling
used in all tests. Unless otherwise indicated, it is intended that
9.1 Sample collection should be in accordance with appro-
all reagents conform to the specifications of the Committee on
priate sampling protocols.
Analytical Reagents of the American Chemical Society where
9.2 Samples should be collected in glass containers, that
such specifications are available. Other grades may be used,
have tightly sealing caps. If very volatile organics are of
provided it is first ascertained that the reagent is of sufficiently
particular interest, the headspace in the container should be
high purity to permit its use without lessening the accuracy of
kept to a minimum.
the determination.
9.3 Sample Transfer Implements—Implements are required
7.2 Purity of Water— Unless otherwise indicated, refer-
to transfer portions of waste samples from the sample contain-
ences to water shall be understood to mean reagent water as
ers to the laboratory containers. Liquid samples may be
defined by Type II of Specification D 1193.
transferred using disposable pipets. Solids and semisolids may
7.3 Nitrogen or Helium (High Purity)—For carrier and
be transferred using a conventional laboratory spatula.
makeup gases. Air and hydrogen (high purity) for fuel gases.
9.4 Samples shall be handled maintaining safe laboratory
practices. Any samples with special hazards must be appropri-
ately labeled.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
9.5 Unused sample material, laboratory dilutions, and waste
listed by the American Chemical Society, see Analar Standards for Laboratory
from the samples may be regulated. Consult your specialist or
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
the regulations, or both, for guidance in the proper handling
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD. and disposal of laboratory wastes.
D 5830
10. Procedure hazardous waste samples. Depending on treatment or process
requirements, it may be necessary to analyze each phase or
10.1 Sample Preparation:
layer individually.
10.1.1 Analyze liquid matrices with relatively low viscosity
10.2 Recommended GC Operating Conditions:
using direct injection into the GC, either as received or after
10.2.1 For Capillary DB-1701 with FID
dilution with CS , M-Pyrol, or other suitable solvent.
10.1.2 Analyze solid or semisolid samples as follows: Column flow rate 1–1.5 mL/min
Make-up gas flow rate 30–60 mL/min
10.1.2.1 For carbon disulfide or M-Pyrol preparation, weigh
Split flow 60 cm /min
3 g of the waste sample in a 15-mL glass vial. Add3gof
Injector temperature 250°C
carbon disulfide or M-Pyrol to the vial and the mixture is Detector temperature 250°C
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.
Initial oven temperature 35°C
Initial time 6 min
10.1.2.2 Use alternate sample sizes and extraction solvent
Level 1 rate 6°C/min
weights if necessary. Actual sample size and solvent weight
Level 1 final value 180°C
must be recorded in the appropriate sample preparation log
Level 2 rate 10°C/min
book. It is essential for accurate waste sample analysis that Level 2 final value 230°C
Run time 40 min
sample size be sufficient to ensure a representative sample. If
Threshold 4 units
alternate sample size or extraction solvent volumes, or both,
Peak width 0.04 min
are used, this must be reflected in the calculations under the
NOTE 4—Typical chromatograms are shown in Figs. 2-5.
dilution factor in Section 11.
10.1.3 Multiple phases or layers are typically present in 10.2.2 For Capillary DB-624 with FID
FIG. 2 Solvent Standard #1 FID/DB-1701
D 5830
FIG. 3 Solvent Standard #2 FID/DB-1701
Column flow rate 3.5 mL/min Column flow rate 40 mL/min
Make-up gas flow 29 mL/min Air pressure (FID) 300 kPa
Airflow (FID) Approximately 300 mL/min Hydrogen pressure (FID) 130 kPa
Hydrogen flow (FID) Approximately 30 mL/min Injector temperature 250°C
Injector temperature 275°C Detector temperature 250°C
Detector temperature 275°C Initial oven temperature 90°C
Initial oven temperature 35°C Initial time 6 min
Initial time 5 min Level 1 rate 3°C/min
Level 1 rate 5°C/min Level 1 final value 120°C
Level 1 final value 150°C Level 2 rate 5°C/min
Level 1 hold time 4 min Level 2 final value 180°C
Lev
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.