ASTM C1234-98(2004)
(Test Method)Standard Practice for Preparation of Oils and Oily Waste Samples by High-Pressure, High-Temperature Digestion for Trace Element Determinations (Withdrawn 2009)
Standard Practice for Preparation of Oils and Oily Waste Samples by High-Pressure, High-Temperature Digestion for Trace Element Determinations (Withdrawn 2009)
SIGNIFICANCE AND USE
This practice is useful for preparation of difficult-to-digest, primarily oils and oily wastes, specimens for trace element determinations of up to 28 elements by atomic absorption or plasma emission techniques. Specimen preparation by high-pressure ashing is primarily applicable to specimens whose preparation by EPA SW-846 protocols is either not applicable or not defined. This sample preparation practice is applicable for the trace element characterization of mixed oily wastes for use by waste treatment facilities such as incinerators or waste stabilization facilities.
SCOPE
1.1 This test method describes a high-pressure, high-temperature digestion technique using the high-pressure asher (HPA) for preparation of oils and oily waste specimens for determination of up to 28 different elements by inductively coupled plasma-atomic emission plasma spectroscopy (ICP-AES), cold-vapor atomic absorption spectroscopy (CVAAS), and graphite furnace atomic absorption spectroscopy (GFAAS). Oily and high-percentage organic waste streams from nuclear and non-nuclear manufacturing processes can be successfully prepared for trace element determinations by ICP-AES, CVAAS, and GFAAS. This method is applicable to the determination of total trace elements in these mixed wastes. Specimens prepared by this method can be used to characterize organic mixed waste streams received by hazardous waste treatment incinerators and for total element characterization of the waste streams.
1.2 This test method is applicable only to organic waste streams that contain radioactivity levels that do not require special personnel or environmental protection from radioactivity or other acute hazards.
1.3 A list of elements determined in oily waste streams is found in Table 1.
1.4 This test method has been used successfully to completely digest a large variety of oils and oily mixed waste streams from nuclear processing facilities. While the method has been used to report data on up to 28 trace elements, its success should not be expected for all analytes in every specimen. The overall nature of these oily wastes tends to be heterogeneous that can affect the results. Homogeneity of the prepared sample is critical to the precision and quality of the results. Some elements, notably silver and antimony, may be recovered on a semiquantitative basis, while most results are highly quantitative.
1.5 This procedure is designed to be applicable to samples whose preparation methods are not defined, or not suitable, by other regulatory procedures or requirements, such as the U.S. Environmental Protection Agency (EPA) SW-846 and EPA-600 4-79-020 documents. This digestion method is designed to provide a high level of accuracy and precision, but does not replace or override any regulatory requirements for sample preparation.
1.6 This method uses hazardous materials, operations, and equipment at high pressure (90-110 bars, 89-108 atm, or 1305-1595 lb/in.2) and high temperatures, up to 320°C, and therefore poses significant hazards if not operated properly. This standard does not purport to address all of the safety problems, 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. Specific hazard statements are given in Sections 10 and 11.
WITHDRAWN RATIONALE
This practice describes a high-pressure, high-temperature digestion technique using the high-pressure asher (HPA) for preparation of oils and oily waste specimens for determination of up to 28 different elements by inductively coupled plasma-atomic emission plasma spectroscopy (ICP-AES), cold-vapor atomic absorption spectroscopy (CVAAS), and graphite furnace atomic absorption spectroscopy (GFAAS), inductively coupled plasma-mass spectrometry (ICPMS), and radiochemical methods.
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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:C1234–98(Reapproved 2004)
Standard Practice for
Preparation of Oils and Oily Waste Samples by High-
Pressure, High-Temperature Digestion for Trace Element
Determinations
This standard is issued under the fixed designation C 1234; 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 Environmental Protection Agency (EPA) SW-846 and EPA-
6004-79-020documents.Thisdigestionpracticeisdesignedto
1.1 This practice describes a high-pressure, high-
provide a high level of accuracy and precision, but does not
temperature digestion technique using the high-pressure asher
replace or override any regulatory requirements for sample
(HPA) for preparation of oils and oily waste specimens for
preparation.
determination of up to 28 different elements by inductively
1.6 This practice uses hazardous materials, operations, and
coupled plasma-atomic emission plasma spectroscopy (ICP-
equipment at high pressure (90–110 bars, 89–108 atm, or
AES), cold-vapor atomic absorption spectroscopy (CVAAS),
1305–1595 lb/in. ) and high temperatures, up to 320°C, and
and graphite furnace atomic absorption spectroscopy
therefore poses significant hazards if not operated properly.
(GFAAS), inductively coupled plasma-mass spectrometry
This standard does not purport to address all of the safety
(ICPMS), and radiochemical methods. Oily and high-
concerns, if any, associated with its use. It is the responsibility
percentage organic waste streams from nuclear and non-
of the user of this standard to establish appropriate safety and
nuclear manufacturing processes can be successfully prepared
health practices and determine the applicability of regulatory
for trace element determinations by ICP-AES, CVAAS, and
limitations prior to use. Specific hazard statements are given in
GFAAS. This practice is applicable to the determination of
Sections 10 and 11.
totaltraceelementsinthesemixedwastes.Specimensprepared
by this practice can be used to characterize organic mixed
2. Referenced Documents
waste streams received by hazardous waste treatment incinera-
2.1 ASTM Standards:
torsandfortotalelementcharacterizationofthewastestreams.
D 1193 Specification for Reagent Water
1.2 This practice is applicable only to organic waste streams
E 177 Practice for Use of the Terms Precision and Bias in
that contain radioactivity levels that do not require special
ASTM Test Methods
personnel or environmental protection from radioactivity or
2.2 US EPA Standards:
other acute hazards.
Methods for Chemical Analysis of Water and Wastes,
1.3 A list of elements determined in oily waste streams is
600/4-79-020, 1983
found in Table 1.
Test Methods for Evaluating Solid Waste, SW-846, 3rd Ed.,
1.4 This test practice has been used successfully to com-
pletely digest a large variety of oils and oily mixed waste
streams from nuclear processing facilities. While the practice
3. Terminology
has been used to report data on up to 28 trace elements, its
3.1 Definitions:
success should not be expected for all analytes in every
3.1.1 heating block—aluminum block used to hold samples
specimen. The overall nature of these oily wastes tends to be
inside the HPA autoclave/pressure chamber.
heterogeneous that can affect the results. Homogeneity of the
3.1.2 HPA-TC controller—computerinterfacebetweenHPA
prepared sample is critical to the precision and quality of the
autoclave and an IBM-compatible computer.
results.
3.1.3 pressure chamber—chamber within the HPA auto-
1.5 This practice is designed to be applicable to samples
clave where heating block filled with samples is placed. The
whose preparation practices are not defined, or not suitable, by
other regulatory procedures or requirements, such as the U.S.
For referenced ASTM Standards, visit the ASTM website, www.astm.org, or
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear contact ASTM Customer Service at service@astm.org. ForAnnual Book of ASTM
Fuel Cycle and is the direct responsibility of Subcommittee C26.02 on Fuel and Standardsvolume information, refer to the standard’s Document Summary page on
Fertile Material Specifications. the ASTM website.
Current edition approved July 10, 1998. Published October 1998. Originally Available from Superintendent of Documents, U.S. Government Printing
approved in 1993. Last previous edition approved in 1998 as C 1234–98 Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1234–98 (2004)
TABLE 1 List of Elements and Applicable Lower Concentration
element determinations of up to 28 elements by atomic
Ranges
absorption or plasma emission techniques. Specimen prepara-
Lower Reportable
tion by high-pressure ashing is primarily applicable to speci-
Element Analysis Method
A
Limit, µg/g
menswhosepreparationbyEPASW-846protocolsiseithernot
Aluminum 3.3 ICP-AES
applicable or not defined. This sample preparation practice is
Antimony 8.3 ICP-AES or GFAAS
applicable for the trace element characterization of mixed oily
Arsenic 8.3 ICP-AES or GFAAS
Barium 0.17 ICP-AES wastes for use by waste treatment facilities such as incinerators
Beryllium 0.05 ICP-AES
or waste stabilization facilities.
Boron 0.67 ICP-AES
Cadmium 0.50 ICP-AES or GFAAS
6. Interferences
Calcium 0.67 ICP-AES
Chromium 1.7 ICP-AES
6.1 Preparation of samples for trace element determinations
Cobalt 0.83 ICP-AES
is subject to matrix and chemical interferences. Although the
Copper 0.67 ICP-AES
Iron 0.67 ICP-AES
HPA practice is designed to totally digest most matrices, there
Lead 8.3 ICP-AES or GFAAS
are some matrix types that are not applicable to this practice,
Lithium 0.67 ICP-AES
for example, highly reactive substances (explosives), ex-
Magnesium 0.08 ICP-AES
Manganese 0.17 ICP-AES
tremely flammable materials, and some silicone-based lubri-
Mercury 0.03 CVAAS
cants.
Nickel 1.7 ICP-AES
Potassium 100 ICP-AES
Selenium 8.3 ICP-AES or GFAAS 7. Apparatus
Silver 1.0 ICP-AES
7.1 HPA High Pressure Asher —High-pressure, high-
Sodium 3.3 ICP-AES
Strontium 0.07 ICP-AES temperature autoclave under computer control allowing com-
Thallium 1.7 GFAAS
plete digestion of difficult specimens using mineral acids. The
Titanium 0.50 ICP-AES
system includes:
Vanadium 0.83 ICP-AES
Zinc 0.17 ICP-AES 7.1.1 Compatible computer with hard drive and with one
Zirconium 0.83 ICP-AES
open RS-232C serial interface.
A
Lower reportable limits are based on a 0.3-g sample diluted to a final volume
7.1.2 HPA-TC temperature controller—this device provides
of 50 mL. These limits should only be used as a guide. Actual values are
the interface between the HPA autoclave and the computer by
instrument and sample dependent.
means of RS-232C serial interface.
7.1.3 HPA autoclave unit.
TABLE 2 HPA Temperature Program for Oils and Oily Waste
7.1.4 HPAsample vessels, appropriate size and construction
Samples
for specimen type and mineral acid used.
Starting Ending
Phase Time, min
7.2 Ultrasonic Homogenizer—Specimen homogenizer us-
Temperature,°C Temperature,°C
ing ultrasonic disruption tip to homogenize specimens that
1 100 30 125
2 125 60 300
cannot be mixed by hand.
3 300 60 300
425 30 25
8. Reagents and Materials
50 0 0
8.1 Purity of Reagents—Chemicals used in the preparation
of spiking standards must be of ultra purity grade. Chemicals
chamber is designed to hold pressures up to 200 bar (197 atm
and reagents used in the preparation practice must conform to
or 2900 lb/in. ) and temperatures up to 320°C.
the specifications of the Committee on Analytical Reagents of
3.1.4 safety lid vent stack—top plate and cylinder that
the American Chemical Society, where such specifications are
covers the autoclave pressure chamber.
available. Other grades may be used, provided it is first
3.1.5 sample vessel—sample container, constructed of
ascertained that the reagent is of sufficient purity to permit its
quartz or glassy carbon, designed for use in the HPA.
use without lessening the accuracy of the determination.
3.1.6 temperature program—software program which con-
8.2 Reagent Water—References to water shall be under-
trols the temperature ramping of the HPA during the run. The
stood to mean reagent water as defined by Type 1 of Specifi-
program used for preparation of oil samples is shown in Table
cation D 1193.
2.
8.3 Nitric Acid (sp gr 1.42)—Ultra pure concentrated nitric
acid (HNO ).
4. Summary of the Practice
8.4 Hydrochloric Acid (sp gr 1.19)—Ultra pure concen-
4.1 Oil or oily waste specimens are digested in nitric and
trated hydrochloric acid (HCl).
hydrochloric acids using HPAhigh-pressure, high-temperature
equipment. Prepared specimens of 0.2 to 0.7 g will provide
enough solution for analysis by CVAAS, ICP-AES, and
High-pressure ashing equipment manufactured by Anton Paar K. G., Graz,
GFAAS for up to 28 elements. Austria has been found to be satisfactory for this procedure.
“Reagent Chemicals,American Chemical Society Specifications,”Am. Chemi-
cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
5. Significance and Use
theAmerican Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
5.1 This practice is useful for preparation of difficult-to-
Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
digest, primarily oils and oily wastes, specimens for trace Pharmacopeia.”
C1234–98 (2004)
8.5 Hydrofluoric Acid (sp gr 0.988)—Ultra pure concen- pressure may be generated. Due to the closed vessel HPA
trated hydrofluoric acid (HF). technique, the possibility of a specimen venting during the
8.6 Matrix Spiking Standards—Multielement standards HPA digestion is proportional to its mass.
used for matrix spiking shall be of sufficient purity and 10.2 Within a preparation batch, with the number of speci-
accuracy and, where possible, traceable to accepted nationally mens defined by the laboratory, the following quality control
known standards (that is, National Institute of Standards and samples should be included; a reagent blank con
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