ASTM C1234-11(2016)

Standard Practice for Preparation of Oils and Oily Waste Samples by High-Pressure, High-Temperature Digestion for Trace Element Determinations

SIGNIFICANCE AND USE
5.1 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 practice covers 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. 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 practice is applicable to the determination of total trace elements in these mixed wastes. Specimens prepared by this practice 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 practice 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. (A) Lower reportable limits are based on a 0.3 g sample diluted to a final volume of 50 mL. These limits should only be used as a guide. Actual values are instrument and sample dependent.  
1.4 This practice has been used successfully to completely digest a large variety of oils and oily mixed waste streams from nuclear processing facilities. While the practice 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.  
1.5 This practice is designed to be applicable to samples whose preparation practices 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 practice 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 practice uses hazardous materials, operations, and equipment at high pressure (90 bars to 110 bars, 89 atm to 108 atm, or 1305 lb/in.2 to 1595 lb/in.2) and high temperatures, up to 320 °C, and therefore poses significant hazards if not operated properly.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7.1 Exception—Pressure measurements are given in lb/in. units.  
1.8 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. Specific warning statements are given in Sections 10.

General Information

• Status: Historical
• Publication Date: 31-Mar-2016
• ICS: 13.030.30 - Special wastes
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM C1234-11 - Standard Practice for Preparation of Oils and Oily Waste Samples by High-Pressure, High-Temperature Digestion for Trace Element Determinations
• Effective Date: 01-Apr-2016
• Replaced By: ASTM C1234-11(2019) - Standard Practice for Preparation of Oils and Oily Waste Samples by High-Pressure, High-Temperature Digestion for Trace Element Determinations
• Effective Date: 01-May-2019
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 01-Apr-2016
• Referred By: ASTM C1111-10(2020) - Standard Test Method for Determining Elements in Waste Streams by Inductively Coupled Plasma-Atomic Emission Spectroscopy
• Effective Date: 01-Apr-2016
• Referred By: ASTM D7876-13(2018) - Standard Practice for Practice for Sample Decomposition Using Microwave Heating (With or Without Prior Ashing) for Atomic Spectroscopic Elemental Determination in Petroleum Products and Lubricants
• Effective Date: 01-Apr-2016

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: C1234 − 11 (Reapproved 2016)
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 C1234; 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 other regulatory procedures or requirements, such as the U.S.
Environmental Protection Agency (EPA) SW-846 and EPA-
1.1 This practice covers a high-pressure, high-temperature
600/4-79-020documents.Thisdigestionpracticeisdesignedto
digestion technique using the high-pressure asher (HPA) for
provide a high level of accuracy and precision, but does not
preparation of oils and oily waste specimens for determination
replace or override any regulatory requirements for sample
of up to 28 different elements by inductively coupled plasma-
preparation.
atomic emission plasma spectroscopy (ICP-AES), cold-vapor
atomic absorption spectroscopy (CVAAS), and graphite fur- 1.6 This practice uses hazardous materials, operations, and
nace atomic absorption spectroscopy (GFAAS), inductively equipment at high pressure (90 bars to 110 bars, 89 atm to
2 2
coupled plasma-mass spectrometry (ICPMS), and radiochemi- 108 atm, or 1305 lb⁄in. to 1595 lb⁄in. ) and high
cal methods. Oily and high-percentage organic waste streams temperatures, up to 320 °C, and therefore poses significant
from nuclear and non-nuclear manufacturing processes can be hazards if not operated properly.
successfully prepared for trace element determinations by
1.7 The values stated in SI units are to be regarded as
ICP-AES, CVAAS, and GFAAS. This practice is applicable to
standard. No other units of measurement are included in this
thedeterminationoftotaltraceelementsinthesemixedwastes.
standard.
Specimenspreparedbythispracticecanbeusedtocharacterize
1.7.1 Exception—Pressure measurements are given in lb/in.
organic mixed waste streams received by hazardous waste
units.
treatment incinerators and for total element characterization of
1.8 This standard does not purport to address all of the
the waste streams.
safety concerns, if any, associated with its use. It is the
1.2 This practice is applicable only to organic waste streams
responsibility of the user of this standard to establish appro-
that contain radioactivity levels that do not require special
priate safety and health practices and determine the applica-
personnel or environmental protection from radioactivity or
bility of regulatory limitations prior to use. Specific warning
other acute hazards.
statements are given in Sections 10.
1.3 A list of elements determined in oily waste streams is
2. Referenced Documents
found in Table 1.
2.1 ASTM Standards:
1.4 This practice has been used successfully to completely
D1193 Specification for Reagent Water
digestalargevarietyofoilsandoilymixedwastestreamsfrom
E177 Practice for Use of the Terms Precision and Bias in
nuclear processing facilities. While the practice has been used
ASTM Test Methods
to report data on up to 28 trace elements, its success should not
2.2 US EPA Standards:
be expected for all analytes in every specimen. The overall
EPA-600/4-79-020 Methods for ChemicalAnalysis of Water
nature of these oily wastes tends to be heterogeneous that can
and Wastes
affect the results. Homogeneity of the prepared sample is
SW-846 Test Methods for Evaluating Solid Waste, Physical/
critical to the precision and quality of the results.
Chemical Methods
1.5 This practice is designed to be applicable to samples
whose preparation practices are not defined, or not suitable, by
For referenced ASTM Standards, visit the ASTM website, www.astm.org, or
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum contact ASTM Customer Service at [e-mail]. ForAnnual Book of ASTM
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom- Standards volume information, refer to the standard’s Document Summary page on
mittee D02.03 on Elemental Analysis. the ASTM website.
Current edition approved April 1, 2016. Published May 2016. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1993. Last previous edition approved in 2011 as C1234 – 11. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/C1234-11R16. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1234 − 11 (2016)
TABLE 1 List of Elements and Applicable Lower Concentration
4. Summary of the Practice
Ranges
4.1 Oil or oily waste specimens are digested in nitric and
Lower Reportable
Element Analysis Method
A hydrochloric acids using HPAhigh-pressure, high-temperature
Limit, µg/g
equipment. Prepared specimens of 0.2 g to 0.7 g will provide
Aluminum 3.3 ICP-AES
Antimony 8.3 ICP-AES or GFAAS enough solution for analysis by CVAAS, ICP-AES, and
Arsenic 8.3 ICP-AES or GFAAS
GFAAS for up to 28 elements.
Barium 0.17 ICP-AES
Beryllium 0.05 ICP-AES
Boron 0.67 ICP-AES 5. Significance and Use
Cadmium 0.50 ICP-AES or GFAAS
5.1 This practice is useful for preparation of difficult-to-
Calcium 0.67 ICP-AES
Chromium 1.7 ICP-AES digest, primarily oils and oily wastes, specimens for trace
Cobalt 0.83 ICP-AES
element determinations of up to 28 elements by atomic
Copper 0.67 ICP-AES
absorption or plasma emission techniques. Specimen prepara-
Iron 0.67 ICP-AES
Lead 8.3 ICP-AES or GFAAS
tion by high-pressure ashing is primarily applicable to speci-
Lithium 0.67 ICP-AES
menswhosepreparationbyEPASW-846protocolsiseithernot
Magnesium 0.08 ICP-AES
applicable or not defined. This sample preparation practice is
Manganese 0.17 ICP-AES
Mercury 0.03 CVAAS
applicable for the trace element characterization of mixed oily
Nickel 1.7 ICP-AES
wastes for use by waste treatment facilities such as incinerators
Potassium 100 ICP-AES
or waste stabilization facilities.
Selenium 8.3 ICP-AES or GFAAS
Silver 1.0 ICP-AES
Sodium 3.3 ICP-AES
6. Interferences
Strontium 0.07 ICP-AES
Thallium 1.7 GFAAS
6.1 Preparation of samples for trace element determinations
Titanium 0.50 ICP-AES
is subject to matrix and chemical interferences. Although the
Vanadium 0.83 ICP-AES
HPA practice is designed to totally digest most matrices, there
Zinc 0.17 ICP-AES
Zirconium 0.83 ICP-AES
are some matrix types that are not applicable to this practice,
A
Lower reportable limits are based on a 0.3 g sample diluted to a final volume of for example, highly reactive substances (explosives), ex-
50 mL. These limits should only be used as a guide.Actual values are instrument
tremely flammable materials, and some silicone-based lubri-
and sample dependent.
cants.
7. Apparatus
3. Terminology
7.1 HPA High Pressure Asher —High-pressure, high-
3.1 Definitions:
temperature autoclave under computer control allowing com-
3.1.1 heating block, n—aluminum block used to hold
plete digestion of difficult specimens using mineral acids. The
samples inside the HPA autoclave/pressure chamber.
system includes:
3.1.2 HPA-TC controller, n—computer interface between
7.1.1 Compatible computer with hard drive and with one
HPA autoclave and an IBM-compatible computer. open RS-232C serial interface.
7.1.2 HPA-TC temperature controller—this device provides
3.1.3 pressure chamber, n—chamber within the HPA auto-
the interface between the HPA autoclave and the computer by
clave where heating block filled with samples is placed. The
means of RS-232C serial interface.
chamber is designed to hold pressures up to 200 bar (197 atm
7.1.3 HPA autoclave unit.
or 2900 lb⁄in. ) and temperatures up to 320 °C.
7.1.4 HPAsample vessels, appropriate size and construction
3.1.4 safety lid vent stack, n—top plate and cylinder that
for specimen type and mineral acid used.
covers the autoclave pressure chamber.
7.2 Ultrasonic Homogenizer—Specimen homogenizer us-
3.1.5 sample vessel, n—sample container, constructed of
ing ultrasonic disruption tip to homogenize specimens that
quartz or glassy carbon, designed for use in the HPA.
cannot be mixed by hand.
3.1.6 temperature program, n—software program which
controls the temperature ramping of the HPA during the run.
8. Reagents and Materials
The program used for preparation of oil samples is shown in
8.1 Purity of Reagents—Chemicals used in the preparation
Table 2.
of spiking standards must be of ultra purity grade. Chemicals
and reagents used in the preparation practice must conform to
TABLE 2 HPA Temperature Program for Oils and Oily Waste
the specifications of the Committee on Analytical Reagents of
Samples
the American Chemical Society, where such specifications are
Starting Ending
Phase Time, min
Temperature,°C Temperature,°C
1 100 30 125
The sole source of supply of the apparatus known to the committee at this time
2 125 60 300
isAnton Paar K. G., Graz,Austria. If you are aware of alternative suppliers, please
3 300 60 300
provide this information toASTM International Headquarters. Your comments will
425 30 25
50 0 0 receive careful consideration at a meeting of the responsible technical committee,
which you may attend.
C1234 − 11 (2016)
available. Other grades may be used, provided it is first normally complete within 10 s to 60 s. If heat generation in the
ascertained that the reagent is of sufficient purity to permit its samplebecomesaproblem,determinedbythetemperaturerise
use without lessening the accuracy of the determination. in the specimen, then the homogenization should be judged
complete when the sample temperature rises to this level, as
8.2 Reagent Water—References to water shall be under-
determined on a specimen by specimen basis. Process and
stood to mean reagent water as defined by Type 1 of Specifi-
observe each sample individually to obtain the best, most
cation D1193.
representative results. Specimens with low flash points are not
8.3 Nitric Acid (sp gr 1.42)—Ultra pure concentrated nitric
recommended for homogenization by this method.
acid (HNO ).
9.3.2 Process the specimen immediately to maintain its
8.4 Hydrochloric Acid (sp gr 1.19)—Ultra pure concen-
homogeneity.
trated hydrochloric acid (HCl).
10. Procedure
8.5 Hydrofluoric Acid (sp gr 0.988)—Ultra pure concen-
trated hydrofluoric acid (HF).
10.1 Weigh 0.2 g to 0.7 g of homogeneous sample into a
clean HPA vessel. The sample mass necessary for the HPA is
8.6 Matrix Spiking Standards—Multielement standards
used for matrix spiking shall be of sufficient purity and matrix dependent, th
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: C1234 − 11 C1234 − 11 (Reapproved 2016)
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 C1234; 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
1.1 This practice covers 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. 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 practice is applicable to the determination of total trace
elements in these mixed wastes. Specimens prepared by this practice 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 practice 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 practice has been used successfully to completely digest a large variety of oils and oily mixed waste streams from
nuclear processing facilities. While the practice 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.
1.5 This practice is designed to be applicable to samples whose preparation practices 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 practice 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 practice uses hazardous materials, operations, and equipment at high pressure (90–110 bars, 89–108 atm, or
2 2
1305–1595(90 bars to 110 bars, 89 atm to 108 atm, or 1305 lb ⁄in. lb/in.to 1595 lb ⁄in. ) and high temperatures, up to
320°C,320 °C, and therefore poses significant hazards if not operated properly.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7.1 Exception—Pressure measurements are given in lb/in. units.
1.8 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. Specific warning statements are given in Sections 10.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved June 1, 2011April 1, 2016. Published July 2011May 2016. Originally approved in 1993. Last previous edition approved in 19982011 as
C 1234–98C1234 – 11. which was withdrawn June 2009 and reinstated in June 2011. DOI: 10.1520/C1234–11.DOI: 10.1520/C1234-11R16.
For referenced ASTM Standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. ForAnnual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1234 − 11 (2016)
TABLE 1 List of Elements and Applicable Lower Concentration
Ranges
Lower Reportable
Element Analysis Method
A
Limit, μg/g
Aluminum 3.3 ICP-AES
Antimony 8.3 ICP-AES or GFAAS
Arsenic 8.3 ICP-AES or GFAAS
Barium 0.17 ICP-AES
Beryllium 0.05 ICP-AES
Boron 0.67 ICP-AES
Cadmium 0.50 ICP-AES or GFAAS
Calcium 0.67 ICP-AES
Chromium 1.7 ICP-AES
Cobalt 0.83 ICP-AES
Copper 0.67 ICP-AES
Iron 0.67 ICP-AES
Lead 8.3 ICP-AES or GFAAS
Lithium 0.67 ICP-AES
Magnesium 0.08 ICP-AES
Manganese 0.17 ICP-AES
Mercury 0.03 CVAAS
Nickel 1.7 ICP-AES
Potassium 100 ICP-AES
Selenium 8.3 ICP-AES or GFAAS
Silver 1.0 ICP-AES
Sodium 3.3 ICP-AES
Strontium 0.07 ICP-AES
Thallium 1.7 GFAAS
Titanium 0.50 ICP-AES
Vanadium 0.83 ICP-AES
Zinc 0.17 ICP-AES
Zirconium 0.83 ICP-AES
A
Lower reportable limits are based on a 0.3-g0.3 g sample diluted to a final
volume of 50 mL. 50 mL. These limits should only be used as a guide. Actual
values are instrument and sample dependent.
2.2 US EPA Standards:
EPA-600/4-79-020 Methods for Chemical Analysis of Water and Wastes
SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
3. Terminology
3.1 Definitions:
3.1.1 heating block, n—aluminum block used to hold samples inside the HPA autoclave/pressure chamber.
3.1.2 HPA-TC controller, n—computer interface between HPA autoclave and an IBM-compatible computer.
3.1.3 pressure chamber, n—chamber within the HPA autoclave where heating block filled with samples is placed. The chamber
is designed to hold pressures up to 200 bar (197 atm or 2900 200 bar (197 atm or 2900 lb lb/in.⁄in. ) and temperatures up to
320°C.320 °C.
3.1.4 safety lid vent stack, n—top plate and cylinder that covers the autoclave pressure chamber.
3.1.5 sample vessel, n—sample container, constructed of quartz or glassy carbon, designed for use in the HPA.
3.1.6 temperature program, n—software program which controls the temperature ramping of the HPA during the run. The
program used for preparation of oil samples is shown in Table 2.
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
TABLE 2 HPA Temperature Program for Oils and Oily Waste
Samples
Starting Ending
Phase Time, min
Temperature,°C Temperature,°C
1 100 30 125
2 125 60 300
3 300 60 300
4 25 30 25
5 0 0 0
C1234 − 11 (2016)
4. Summary of the Practice
4.1 Oil or oily waste specimens are digested in nitric and hydrochloric acids using HPA high-pressure, high-temperature
equipment. Prepared specimens of 0.20.2 g to 0.7 g 0.7 g will provide enough solution for analysis by CVAAS, ICP-AES, and
GFAAS for up to 28 elements.
5. Significance and Use
5.1 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.
6. Interferences
6.1 Preparation of samples for trace element determinations is subject to matrix and chemical interferences. Although the HPA
practice is designed to totally digest most matrices, there are some matrix types that are not applicable to this practice, for example,
highly reactive substances (explosives), extremely flammable materials, and some silicone-based lubricants.
7. Apparatus
7.1 HPA High Pressure Asher —High-pressure, high-temperature autoclave under computer control allowing complete
digestion of difficult specimens using mineral acids. The system includes:
7.1.1 Compatible computer with hard drive and with one open RS-232C serial interface.
7.1.2 HPA-TC temperature controller—this device provides the interface between the HPA autoclave and the computer by
means of RS-232C serial interface.
7.1.3 HPA autoclave unit.
7.1.4 HPA sample vessels, appropriate size and construction for specimen type and mineral acid used.
7.2 Ultrasonic Homogenizer—Specimen homogenizer using ultrasonic disruption tip to homogenize specimens that cannot be
mixed by hand.
8. Reagents and Materials
8.1 Purity of Reagents—Chemicals used in the preparation of spiking standards must be of ultra purity grade. Chemicals and
reagents used in the preparation practice must conform to the specifications of the Committee on Analytical Reagents of the
American Chemical Society, where such specifications are available. Other grades may be used, provided it is first ascertained
that the reagent is of sufficient purity to permit its use without lessening the accuracy of the determination.
8.2 Reagent Water—References to water shall be understood to mean reagent water as defined by Type 1 of Specification
D1193.
8.3 Nitric Acid (sp gr 1.42)—Ultra pure concentrated nitric acid (HNO ).
8.4 Hydrochloric Acid (sp gr 1.19)—Ultra pure concentrated hydrochloric acid (HCl).
8.5 Hydrofluoric Acid (sp gr 0.988)—Ultra pure concentrated hydrofluoric acid (HF).
8.6 Matrix Spiking Standards—Multielement standards used for matrix spiking shall be of sufficient purity and accuracy and,
where possible, traceable to accepted nationally known standards (that is, National Institute of Standards and Technology (NIST)
or EPA). Spiking standards used should yield spiked specimens with concentrations between 0.50.5 mg ⁄L to 22 mg ⁄ mg/L L for
most elements.
9. Sample Preparation
9.1 Homogeneous specimens are a requirement if suitable analytical precision is expected. Most oils and oily wastes require
additional steps to provide homogeneous specimens for preparation. If the sample is visibly clear or can be shaken to provide a
homogeneous specimen, no further pretreatment is necessary.
9.2 Liquid or aqueous specimens that are cloudy or contain visible sediment or precipitates may require an ultrasonic bath to
resuspend settled material or maintain a homogeneous specimen for preparation. The process of ultrasonic mixing will generate
The sole source of supply of the apparatus known to the committee at this time is Anton Paar K. G., Graz, Austria. If you are aware of alternative suppliers, please provide
this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may
attend.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by
the American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
C1234 − 11 (2016)
heat, and warm the sample above ambient temperature. A consideration of the original sample must be made as to the effect of
ultrasonification on the sample. A sample with a low boiling point, such as freon, may not be applicable to ultrasonic mixing.
Ultrasonification between 11 min to 5 min 5 min is effective for liquid or aqueous samples.
9.3 It is difficult to obtain homogeneous specimens for preparation from multi-phase liquids, oils, oily wastes, or samples with
large amounts of solid matter. For these sample types, an ultrasonic sonifier is very useful in providing a homogeneous specimen.
The sonifier uses high-frequency electrical energy transmitted through a converter to vibrate a metal horn tip that is immersed in
the sample. The vibration of the horn tip causes cavitation of medium that causes the intense agitation of the medium leading to
very stable emulsions to be formed, even between polar and non-polar liquids.
9.3.1 The sonification process will generate heat, and the specimen should be checked during the process. Specimen
homogenization is determined by visual observation and is normally complete within 1010 s to 60 s. 60 s. If heat generation in
the sample becomes a problem, determined by the temperature rise in the specimen, then the homogenization should be judged
complete when the sample temperature rises to this level, as determined on a specimen by specimen basis. Process and observe
each sample individually to obtain the best, most representative results. Specimens with low flash points are not recommended for
homogenization by this method.
9.3.2 Process the specimen immediately to maintain its homogeneity.
10. Procedure
10.1 Weigh 0.20.2 g to 0.7 g 0.7 g of homogeneous sample into a clean HPA vessel. The sample mass necessary for the HPA
is matrix dependent, that is, organic or inorganic content, and samples up to 2 g 2 g can be prepared. Sample sizes of 0.20.2 g to
0.7 g 0.7 g are successful for highly organic specimens. The organic component of the specimen will have a direct effect on the
digestion in the HPA; the more organic a specimen the more internal pressure may be generated. Due to the closed vessel HPA
technique, the possibility of a specimen venting during the HPA digestion is proportional to its mass.
10.2 Within a preparation batch, with the number of specimens defined by the laboratory, the following quality control samples
should be included; a reagent blank containing all reagents used in the procedure, a matrix duplicate specimen for assessing
precision, and a matrix spiked specimen for assessing method accuracy. A batch size of ten specimens has been successful for HPA
digestion performed on oily waste samples.
10.3 Exercise extreme caution when handling specimens during the pressure decomposition process, as spont
...