&EPA
United States
Environmental Protection
Agency
FINAL UPDATE 1MB
AND METHOD 9071B OF FINAL UPDATE MIA
Test Methods for Evaluating Solid Waste
Physical/Chemical Methods
SW-846
-------
Office of Solid Waste and
Emergency Response (5102G)
EPA-SW-846-03-03B
www.epa.gov
November 2004
-------
FINAL UPDATE 1MB
AND METHOD 9071B FROM FINAL UPDATE IIIA
TEST METHODS FOR EVALUATING SOLID WASTE
PHYSICAL/CHEMICAL METHODS
(SW-846) THIRD EDITION
THIS PACKET CONTAINS MATERIAL
FOR INCLUSION IN THE EPA PUBLICATION SW-846
Contents:
1. Cover sheet (What you are currently reading)
2. Instructions. This section explains how this package relates to the rest
of SW-846.
3. Status Tables. The "Status Tables" document includes two tables. One
table is a sequentially numbered listing of all SW-846 methods and their
current status. The other table lists the status of all other documents in
SW-846 (e.g., the Disclaimer, the chapters).
4. Table of Contents. The Table of Contents (dated November 2004) lists
all of the methods (as updated by Third Edition Final Updates I, II, IIA,
IIB, III, and IIIA and IIIB) in the order of appearance in the manual.
It does not reflect Draft Update FVA or IVB methods because those
methods are not yet finalized by the U.S. EPA.
5. Chapter Five and Methods 9010C. 9012B. 9060A. 9070A. and 9071B
(9071B is unchanged from Final Update IIIA).
6. Chapter Six and Methods 9045D and 9095B.
7. Chapter Seven
8. Chanter Eight and Methods 1010A. 1020B. 9040C. 1110A. and 1310B
-------
INSTRUCTIONS
SW-846, a methods manual, is a "living" document that changes when new data and advances in
analytical techniques are incorporated into the manual as new or revised methods. To date, the
Agency has formally issued Final Updates I, II, HA, IIB, III, and IIIA, and Draft Updates IVA and
FVB. (Currently, the methods and chapters of Draft Update IVB are not available from GPO, but
are available on-line at www.epa.gov/SW-846/ or on paper from NTIS, (800) 553-6847.) This
package contains Final Update IIIB methods and chapters with a footer date of November 2004. In
addition, Method 907 IB of Final Update IIIA with a footer date of April 1998 is included in this
package because it was not distributed by the GPO at the time of its promulgation. Previously, it
was only available through NTIS or at the SW-846 internet site.
These instructions describe how to get your basic manual up-to-date and what to do with your
update package. A number of SW-846 update packages have been released to the public since the
original Third Edition was released. In general, final updates should always be incorporated into
SW-846 in chronological order (e.g., Update I should be incorporated before Update II).
If you got your package from GPO, the following definitions are provided as they relate to
the text to follow regarding how to put together a GPO subscription to SW-846:
Previous subscribers are individuals that received copies of the Third Edition and other
SW-846 updates (including proposed updates) in the past and just received this Final
Update IIIB package in the mail.
New subscribers are individuals that recently (e.g., 6-8 weeks) placed an order with the
GPO and received new copies of the 4 (four) volume set of the Third Edition, a copy of
Final Update I, a copy of Final Update II/IIA, a copy of Final Update IIB, a copy of Final
Update HI, a copy of Draft Update IVA, and a copy of this package.
Instructions - 1 Final Update IIIB
-------
INCORPORATING FINAL UPDATE IIIB
AND METHOD 9071B (FROM FINAL UPDATE IIIA) IN YOUR MANUAL
This package is printed on white paper and all SW-846 chapters and methods finalized and
updated as part of Update IIIB have the date of "November 2004" in the lower right hand corner.
Method 907 IB was last finalized and updated as part of Update IIIA and thus has the date of April
1998 in its lower right hand corner. You may have gotten this package from the National
Technical Information Service (NTIS) or the Government Printing Office (GPO). Please visit the
EPA OSW Methods Team website at http://www.epa.gov/SW-846/ for information on other ways
to obtain SW-846 methods and updates.
Please note that, if you wish to keep all of the final, proposed, and draft updates together, you will
find that the binders provided to you as part of a GPO subscription are not large enough to contain
all of the material. In that case, you can add other binders of your choice. The instructions below
can be followed as appropriate if you get your SW-846 from other sources besides GPO.
NEW GPO SUBSCRIBERS - If you are a new subscriber, you should perform the following
tasks before addressing this package (those who obtained their manual from other sources, may
also find this information useful in putting together SW-846). You will need to use the detailed
instructions found in the Final Update III package.
Following the instructions found in your Final Update III package (starting at page
"Instructions - 2" of that update package), place the original Third Edition of SW-846
(September 1986) in the properly labeled four 3-ring notebooks, and then incorporate Final
Updates I (July 1992), II (September 1994), IIA (August 1993), IIB (January 1995), and III
(December 1996).
Either incorporate Draft Update FVA in the manual (without removing any white pages), or
keep the colored draft update in a separate binder of your choice. Draft Update IVB is
only available at the SW-846 internet site, at http://www.epa.gov/SW-846/. and may be
printed and added to the manual in the same manner.
Incorporate this package [Method 9071B of Final Update IIIA, dated April 1998, and Final
Update IIIB, dated November 2004)] into the manual and remove any previous versions of
its chapters and methods as appropriate.
PREVIOUS GPO SUBSCRIBERS - If you are a previous subscriber, it is important to establish
exactly what is currently contained in your manual before addressing this package. If your manual
is to be updated with only the latest final versions of the methods and chapters, the only white
pages in the document should be dated September 1986 (Third Edition), July 1992 (Final Update
I), August 1993 (Final Update IIA), September 1994 (Final Update II), January 1995 (Final Update
IIB), December 1996 (Final Update III), and April 1998 (if you have added Final Update IIIA
from NTIS or the EPA OSW Methods web site). Remove (and recycle or archive) any white
Instructions - 2 Final Update IIIB
-------
pages from your manual that have other dates unless you have printed, on white paper, other
methods (e.g., Draft Update IVB methods) from the EPA web site and would like to retain them in
your manual copy.
There may also be colored pages (e.g., pink pages for Proposed Update III) inserted in the manual.
Remove all yellow, blue, green, or pink pages from the manual. These colored pages represent
proposed versions of methods and chapters that have since been finalized. You may chose to keep
your copies of colored versions in separate binders.
Finally, incorporate this package into the manual, removing any previous versions of its methods
and chapters. (You may choose to keep the previous versions in a separate binder.)
Instructions - 3 Final Update IIIB
-------
UPDATE HISTORY OF SW-846
Package
Third Edition
Proposed Update I
Final Update I
Proposed Update II
Final Update I
Proposed Update II
Proposed Update IIA
Final Update IIA
(Method 4010, included
with Final Update II.)
Final Update II
Final Update IIB
Proposed Update III
Final Update III
Draft Update IVA
Final Update IIIA
Draft Update IVB
Proposed Update IIIB
Final Update IIIB
Date
September 1986
December 1987
November 1990
November 1990
July 1992
November 1992
October 1992
August 1993
September 1994
January 1995
January 1995
December 1996
January 1998
April 1998
Nov. 2000
August 2002
November
2004
Paper Color
White
Green
White
Blue
White
Yellow
White
White
White
White
Pink
White
Salmon
White
Get from
www.epa.gov/
SW-846
Buff
White
Status of Package
Finalized (Promulgated)
Obsolete
Obsolete
Obsolete
Finalized (Promulgated)
Obsolete
Obsolete
Finalized (Promulgated)
Finalized (Promulgated)
Finalized (Promulgated)
Obsolete
Finalized (Promulgated)
Draft
Finalized (Promulgated)
Draft
Obsolete
Finalized (Promulgated)
The GPO package also
includes Method 9071B
from Update IIIA
Instructions - 4
Final Update IIIB
-------
ASSISTANCE
After reading these instructions, if you need help due to difficulties understanding the status of the
package or have technical questions regarding the methods, you may telephone the Methods
Information Communication Exchange (MICE) at 703-676-4690 or send an E-mail to:
mice@saic.com.
If you have questions concerning your SW-846 U.S. Government Printing Office (GPO)
subscription, you should telephone the GPO at 202-512-1806. If you did not purchase your SW-
846 from the GPO, the GPO will not be able to help you.
Instructions - 5 Final Update IIIB
-------
STATUS TABLES FOR
SW-846, THIRD EDITION
ADDRESSES:
FINAL UPDATES I, II, MA, IIB, III, IIIA, AND 1MB
DRAFT UPDATES IVA AND IVB
OTHER METHODS AT THE OSW METHODS WEB SITE
NOVEMBER 2004
-------
HOW TO USE THIS DOCUMENT
This document provides historical information regarding EPA-published draft, proposed, and final SW-846 methods and chapters. It contains two
status tables, namely; the "SW-846 Method Status Table," which is a listing of SW-846 methods; and the "Status Table for SW-846 Chapter Text and Other
Documents," which lists all other documents in SW-846.
Use the "SW-846 Method Status Table" as a reference guide to identify the historical and latest versions of SW-846 methods. Methods in this status
table are listed sequentially by method number. The column showing "Other Methods" includes those methods that appear as new SW-846 methods at
EPA's Office of Solid Waste Methods Team internet site, http://www.epa.gov/SW-846/. An integrated version of the manual is also available at the Methods
Team internet site.
Use the "Status Table for SW-846 Chapter Text and Other Documents" as a reference guide to identify the historical and latest versions of chapters
and other SW-846 documents (e.g., the Disclaimer).
Previous versions of the "SW-846 Method Status Table" included a column for "Current Promulgated Method." The November 2004 version of that
table does not contain that column because, with the publication of the final Methods Innovation Rule, SW-846 and its methods are no longer required in
general by any RCRA regulation. See 40 CFR 260.11 (a)(11) for a listing of those SW-846 methods that may be still required by the RCRA regulations
for the analysis of method-defined parameters.
Do not use a status table as a guide for putting together a paper version of SW-846. Refer to the "Table of Contents" of the update for the order
in which chapters and methods should appear in SW-846.
-------
SW-846 METHOD STATUS TABLE
November 2004
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
0010
-
0020
-
-
0030
-
-
FINAL
UP. 1
(7/92)
-
-
-
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
-
-
-
-
-
-
FIN. UP.
Ill (12/96)
IIIA (4/98)
-
0011
(Up. Ill)
__
0023A
(Up. Ill)
Revision
of Method
23,40
CFR Part
60
-
-
0031
(Up. Ill)
0040
(Up. Ill)
FIN. UP.
IIIB
(11/04)
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
25D
Referral
25E
Referral
-
-
OTHER
METHODS
(e.g., at
web site)
-
-
-
-
-
-
METHOD TITLE
Modified Method 5
Sampling Train
Sampling for Selected Aldehyde and Ketone
Emissions from Stationary Sources
Source Assessment Sampling System (SASS)
Sampling Method for Polychlorinated Dibenzo-
p-Dioxins and Polychlorinated Dibenzofuran
Emissions from Stationary Sources
Determination of the Volatile Organic Content
of Waste Samples
Determination of Vapor Phase Organic
Concentration in Waste Samples
Volatile Organic Sampling Train
Sampling Method for Volatile Organic
Compounds (SMVOC)
Sampling of Principal Organic Hazardous
Constituents from Combustion Sources Using
Tedlarฎ Baqs
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
-
-
-
-
-
-
1010
1020
FINAL
UP. I
(7/92)
-
-
-
-
-
-
-
*
1020A
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
-
-
-
-
-
-
-
"
FIN. UP.
Ill (12/96)
IIIA (4/98)
0050
(Up. Ill)
0051
(Up. Ill)
0060
(Up. Ill)
0061
(Up. Ill)
0100
(Up. Ill)
-
-
~~
FIN. UP.
1MB
(11/04)
-
-
-
-
-
-
-
1010A
1020B
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
-
-
~~
~~
DRAFT
UP. IVB
(11/00)
-
-
-
-
-
207-1
Referral
207-2
Referral
OTHER
METHODS
(e.g., at
web site)
-
-
-
-
-
-
-
~
METHOD TITLE
Isokinetic HCI/CI2 Emission Sampling Train
Midget Impinger HCI/CI2 Emission Sampling
Train
Determination of Metals in Stack Emissions
Determination of Hexavalent Chromium
Emissions from Stationary Sources
Sampling for Formaldehyde and Other
Carbonyl Compounds in Indoor Air
Sampling Method for Isocyanates
Analysis for Isocyanates by High Performance
Liquid Chromatography (HPLC)
Test Methods for Flash Point by Pensky-
Martens Closed Cup Tester (Method text is a
referral to ASTM Standard D 93-79 or Standard
D 93-80)
Standard Test Methods for Flash Point by
Setaflash (Small Scale) Closed-cup Apparatus
(Method text is a referral to ASTM Standard D
3278-78)
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
~
-
1110
-
1310
-
1320
1330
3005
3010
FINAL
UP. I
(7/92)
-
~
-
__
-
1310A
1311
-
1330A
3005A
301 OA
FIN. UP.
II (9/94)
MA (8/93)
IIB (1/95)
-
-
-
-
-
1312
(Up. II)
-
-
FIN. UP.
Ill (12/96)
MIA (4/98)
1030
(Up. Ill)
~
-
1120
(Up. Ill)
~
-
-
-
FIN. UP.
1MB
(11/04)
~
-
-
1110A
-
1310B
__
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
-
_,
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
1040
1050
-
-
-
-
-
OTHER
METHODS
(e.g., at
web site)
-
-
-
-
-
-
-
'
METHOD TITLE
Ignitability of Solids
Test Method for Oxidizing Solids
Test Methods to Determine Substances Likely
to Spontaneously Combust
Corrosivity Toward Steel
Dermal Corrosion
Extraction Procedure (EP) Toxicity Test
Method and Structural Integrity Test
Toxicity Characteristic Leaching Procedure
Synthetic Precipitation Leaching Procedure
Multiple Extraction Procedure
Extraction Procedure for Oily Wastes
Acid Digestion of Waters for Total Recoverable
or Dissolved Metals for Analysis by FLAA or
ICP Spectroscopy
Acid Digestion of Aqueous Samples and
Extracts for Total Metals for Analysis by FLAA
or ICP Spectroscopv
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
--
3020
--
3040
3050
-
-
[3060, in
the
2nd Ed.]
3500
3510
FINAL
UP. 1
(7/92)
--
3020A
--
--
3050A
-
-
-
3500A
3510A
FIN. UP.
II (9/94)
HA (8/93)
IIB (1/95)
3015
(Up. II)
-
--
-
-
3051
(Up. II)
-
-
-
351 OB
(Up. II)
FIN. UP.
Ill (12/96)
IMA (4/98)
-
-
3031
(Up. Ill)
3040A
(Up. Ill)
3050B
(Up. Ill)
-
3052
(Up. Ill)
3060A
(Up. Ill)
3500B
(Up. Ill)
3510C
(Up. Ill)
FIN. UP.
1MB
(11/04)
--
--
-
-
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
301 5A
-
--
-
--
3051A
--
-
--
-
DRAFT
UP. IVB
(11/00)
-
-
--
--
-
-
--
-
3500C
--
OTHER
METHODS
(e.g., at
web site)
--
-
--
-
-
--
-
--
--
-
METHOD TITLE
Microwave Assisted Acid Digestion of Aqueous
Samples and Extracts
Acid Digestion of Aqueous Samples and
Extracts for Total Metals for Analysis by GFAA
Spectroscopy
Acid Digestion of Oils for Metals Analysis by
Atomic Absorption or ICP Spectrometry
Dissolution Procedure for Oils, Greases, or
Waxes
Acid Digestion of Sediments, Sludges, and
Soils
Microwave Assisted Acid Digestion of
Sediments, Sludges, Soils, and Oils
Microwave Assisted Acid Digestion of
Siliceous and Organically Based Matrices
Alkaline Digestion for Hexavalent Chromium
Organic Extraction and Sample Preparation
Separatory Funnel Liquid-Liquid Extraction
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
3520
3540
-
-
3550
FINAL
UP. I
(7/92)
-
3520A
3540A
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
-
3520B
(Up. II)
3540B
(Up. II)
3541
(Up. II)
-
3550A
(Up. II)
FIN. UP.
Ill (12/96)
IDA (4/98)
-
3520C
(Up. Ill)
3535
(Up. Ill)
3540C
(Up. Ill)
-
3542
(Up. Ill)
3545
(Up. Ill)
_
3550B
(Up. Ill)
FIN. UP.
IIIB
(11/04)
-
-
~"
-
-
-
~
-
DRAFT
UP. IVA
(1/98)
--
-
3535A
-
-
-
3545A
-
DRAFT
UP. IVB
(11/00)
-
-
3535A
(Replaces
IVA
version)
-
-
-
3545A
(Replaces
IVA
version)
3546
3550C
OTHER
METHODS
(e.g., at
web site)
3511
(11/02)
-
~
-
-
-
~
-
METHOD TITLE
Organic Compounds in Water by
Microextraction
Continuous Liquid-Liquid Extraction
Solid-Phase Extraction (SPE)
Soxhlet Extraction
Automated Soxhlet Extraction
Extraction of Semivolatile Analytes Collected
Using Method 0010 (Modified Method 5
Sampling Train)
Pressurized Fluid Extraction (PFE)
Microwave Extraction
Ultrasonic Extraction
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
-
-
-
3580
-
3600
3610
3611
3620
3630
FINAL
UP. 1
(7/92)
-
-
-
-
3580A
-
3600A
3610A
361 1A
3620A
3630A
FIN. UP.
II (9/94)
IIA (8/93)
(IB (1/95)
-
-
-
-
-
3600B
(Up. II)
-
-
-
3630B
(Up. II)
FIN. UP.
Ill (12/96)
MIA (4/98)
3560
(Up. Ill)
3561
(Up. Ill)
-
-
3585
(Up. Ill)
3600C
(Up. Ill)
361 OB
(Up. Ill)
361 1B
(Up. Ill)
3620B
(Up. Ill)
3630C
(Up. Ill)
FIN. UP.
1MB
(11/04)
-
-
-
-
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
3562
-
-
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
-
--
-
-
--
3620C
-
OTHER
METHODS
(e.g., at
web site)
-
-
-
3570
(11/02)
-
-
-
-
--
-
METHOD TITLE
Supercritical Fluid Extraction of Total
Recoverable Petroleum Hydrocarbons
Supercritical Fluid Extraction of Polynuclear
Aromatic Hydrocarbons
Supercritical Fluid Extraction of
Poiychlorinated Biphenyls (PCBs) and
Organochlorine Pesticides
Microscale Solvent Extraction (MSE)
Waste Dilution
Waste Dilution for Volatile Organics
Cleanup
Alumina Cleanup
Alumina Column Cleanup and Separation of
Petroleum Wastes
Florisil Cleanup
Silica Gel Cleanup
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
3640
3650
3660
-
3810
__
3820
--
-
-
FINAL
UP. 1
(7/92)
-
3650A
3660A
-
-
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
3640A
(Up. II)
-
-
3665
(Up. II)
-
-
4010
(Up. IIA)
-
FIN. UP.
Ill (12/96)
IIIA (4/98)
-
3650B
(Up. Ill)
3660B
(Up. Ill)
3665A
(Up. Ill)
-
4000
(Up. Ill)
4010A
(Up. Ill)
4015
(Up. Ill)
FIN. UP.
IIIB
(11/04)
-
-
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
-
-
Noticed
for
removal
from
SW-846
-
--
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
-
3815
-
-
-
-
OTHER
METHODS
(e.g., at
web site)
-
--
-
-
-
-
--
-
METHOD TITLE
Gel-Permeation Cleanup
Acid-Base Partition Cleanup
Sulfur Cleanup
Sulfuric Acid/Permanganate Cleanup
Headspace
Screening Solid Samples for Volatile Organics
Hexadecane Extraction and Screening of
Purgeable Organics
Immunoassay
Screening for Pentachlorophenol by
Immunoassay
Screening for
2,4-Dichlorophenoxyacetic Acid by
Immunoassay
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
--
-
-
-
-
-
-
-
-
-
FINAL
UP. I
(7/92)
-
-
-
-
-
-
-
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
-
-
-
-
-
-
-
-
-
-
FIN. UP.
Ill (12/96)
IIIA (4/98)
4020
(Up. Ill)
-
4030
(Up. Ill)
4035
(Up. Ill)
4040
(Up. Ill)
4041
(Up. Ill)
4042
(Up. Ill)
-
4050
(Up. Ill)
4051
(Up. Ill)
FIN. UP.
1MB
(11/04)
-
-
-
-
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
~
-
-
-
-
-
~
-
-
-
OTHER
METHODS
(e.g., at
web site)
-
4025
(10/02)
~
-
-
-
-
4025
(10/02)
~
-
METHOD TITLE
Screening for Polychlorinated Biphenyls by
Immunoassay
Screening for Polychlorinated Dibenzodioxins
and Polychlorinated Dibenzofurans (PCDD/Fs)
by Immunoassay
Soil Screening for Petroleum Hydrocarbons by
Immunoassay
Soil Screening for Polynuclear Aromatic
Hydrocarbons by Immunoassay
Soil Screening for Toxaphene by Immunoassay
Soil Screening for Chlordane by Immunoassay
Soil Screening for DDT by Immunoassay
Screening for Polychorinated Dibenzodioxins
and Polychlorinated Dibenzofurans (PCDD/Fs)
by Immunoassay
TNT Explosives in Soil by Immunoassay
Hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in
Soil by Immunoassav
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
__
-
-
-
5030
-
-
-
FINAL
UP. I
(7/92)
-
-
-
5030A
-
-
~
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
-
-
-
-
-
-
FIN. UP.
Ill (12/96)
IMA (4/98)
-
5000
(Up. Ill)
5021
(Up. Ill)
5030B
(Up. Ill)
5031
(Up. Ill)
5032
(Up. Ill)
5035
(Up. Ill)
FIN. UP.
1MB
(11/04)
-
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
4500
4670
-
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
4425
-
-
-
-
-
-
-
OTHER
METHODS
(e.g., at
web site)
-
-
5021A
(6/03)
5030C
(5/03)
-
-
5035A
(7/02)
METHOD TITLE
Screening Extracts of Environmental Samples
for Planar Organic Compounds (PAHs, PCBs,
PCDDs/PCDFs) by a Reporter Gene on a
Human Cell Line
Mercury in Soil by Immunoassay
Triazine Herbicides as Atrazine in Water by
Quantitative Immunoassay
Sample Preparation for Volatile Organic
Compounds
5021 A: Volatile Organic Compounds in
Various Sample Matrices Using Equilibrium
Headspace Analysis
Purge-and-Trap for Aqueous Samples
Volatile, Nonpurgeable, Water-Soluble
Compounds by Azeotropic Distillation
Volatile Organic Compounds by Vacuum
Distillation
Closed-System Purge-and-Trap and Extraction
for Volatile Organics in Soil and Waste
Samples
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
5040
-
-
6010
-
-
-
-
7000
-
FINAL
UP. I
(7/92)
-
-
601 OA
-
-
-
-
7000A
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
5040A
(Up. II)
5041
(Up. II)
5050
(Up. II)
-
6020
(Up. II)
-
-
-
-
-
FIN. UP.
Ill (12/96)
IIIA (4/98)
Deleted
from
SW-846
(Up. Ill)
5041A
(Up. Ill)
-
6010B
(Up. Ill)
-
-
-
-
-
-
FIN. UP.
1MB
(11/04)
-
-
-
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
-
6020A
6200
6500
6800
7000B
7010
DRAFT
UP. IVB
(11/00)
-
-
601 OC
-
-
-
-
-
-
OTHER
METHODS
(e.g., at
web site)
-
--
-
-
-
-
-
-
--
METHOD TITLE
Analysis of Sorbent Cartridges from Volatile
Organic Sampling Train (VOST): Gas
Chromatography/Mass Spectrometry
Technique
Analysis for Desorption of Sorbent Cartridges
from Volatile Organic Sampling Train (VOST)
Bomb Preparation Method for Solid Waste
Inductively Coupled Plasma-Atomic Emission
Spectrometry
Inductively Coupled Plasma - Mass
Spectrometry
Field Portable X-Ray Fluorescence
Spectrometry for the Determination of
Elemental Concentrations in Soil and Sediment
Dissolved Inorganic Anions in Aqueous
Matrices by Capillary Ion Electrophoresis
Elemental and Speciated Isotope Dilution Mass
Spectrometry
7000B (Draft Up. IVA): Flame Atomic
Absorption Spectrophotometry
Graphite Furnace Atomic Absorption
Spectrophotometrv
10
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Ndte: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
7020
7040
7041
7060
7061
FINAL
UP. I
(7/92)
_
_
_
7061A
-.
_
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
7060A
(Up. II)
7062
(Up. II)
FIN. UP.
Ill (12/96)
IIIA(4/98)
_
7063
(Up. Ill)
FIN. UP.
NIB
(11/04)
__
_
__
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
__
__
DRAFT
UP. IVB
(11/00)
_
_
OTHER
METHODS
(e.g., at
web site)
_
METHOD TITLE
Aluminum (Atomic Absorption, Direct
Aspiration)
Antimony (Atomic Absorption, Direct
Aspiration)
Antimony (Atomic Absorption, Furnace
Technique)
Arsenic (Atomic Absorption, Furnace
Technique)
Arsenic (Atomic Absorption, Gaseous Hydride)
Antimony and Arsenic (Atomic Absorption,
Borohydride Reduction)
Arsenic in Aqueous Samples and Extracts by
Anodic Stripping Voltammetrv (ASV)
11
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
7080
7090
7091
7130
FINAL
UP. 1
(7/92)
7081
FIN. UP.
II (9/94)
HA (8/93)
IIB (1/95)
7080A
(Up. II)
FIN. UP.
Ill (12/96)
IIIA (4/98)
FIN. UP.
IIIB
(11/04)
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
DRAFT
UP. IVB
(11/00)
OTHER
METHODS
(e.g., at
web site)
METHOD TITLE
Barium (Atomic Absorption, Direct Aspiration)
Barium (Atomic Absorption, Furnace
Technique)
Beryllium (Atomic Absorption, Direct
Aspiration)
Beryllium (Atomic Absorption, Furnace
Technique)
Cadmium (Atomic Absorption, Direct
Aspiration)
12
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
7131
7140
7190
7191
7195
7196
7197
7198
FINAL
UP. 1
(7/92)
.
7196A
-
FIN. UP.
II (9/94)
MA (8/93)
IIB (1/95)
7131A
(Up. II)
-
FIN. UP.
Ill (12/96)
IIIA (4/98)
_
-
FIN. UP.
NIB
(11/04)
-
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
-
DRAFT
UP. IVB
(11/00)
-
OTHER
METHODS
(e.g., at
web site)
-
METHOD TITLE
Cadmium (Atomic Absorption, Furnace
Technique)
Calcium (Atomic Absorption, Direct Aspiration)
Chromium (Atomic Absorption, Direct
Aspiration)
Chromium (Atomic Absorption, Furnace
Technique)
Chromium, Hexavalent (Coprecipitation)
Chromium, Hexavalent (Colorimetric)
Chromium, Hexavalent (Chelation/Extraction)
Chromium, Hexavalent (Differential Pulse
Polaroqraphv)
13
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
7200
7201
7210
FINAL
UP. 1
(7/92)
-
7211
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
FIN. UP.
Ill (12/96)
IMA (4/98)
7199
(Up. Ill)
FIN. UP.
1MB
(11/04)
-
DRAFT
UP. IVA
(1/98)
-
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
DRAFT
UP. IVB
(11/00)
-
OTHER
METHODS
(e.g., at
web site)
-
METHOD TITLE
Determination of Hexavalent Chromium in
Drinking Water, Groundwater and Industrial
Wastewater Effluents by Ion Chromatography
Cobalt (Atomic Absorption, Direct Aspiration)
Cobalt (Atomic Absorption, Furnace
Technique)
Copper (Atomic Absorption, Direct Aspiration)
Copper (Atomic Absorption, Furnace
Technique)
14
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
j
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
7380
7420
7421
FINAL
UP. 1
(7/92)
7381
7430
FIN. UP.
II (9/94)
MA (8/93)
IIB (1/95)
FIN. UP.
Ill (12/96)
IMA (4/98)
FIN. UP.
1KB
(11/04)
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
DRAFT
UP. IVB
(11/00)
OTHER
METHODS
(e.g., at
web site)
METHOD TITLE
Iron (Atomic Absorption, Direct Aspiration)
Iron (Atomic Absorption, Furnace Technique)
Lead (Atomic Absorption, Direct Aspiration)
Lead (Atomic Absorption, Furnace Technique)
Lithium (Atomic Absorption, Direct Aspiration)
15
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
7450
7460
7470
7471
-
-
FINAL
UP. I
(7/92)
7461
-
-
-
-
FIN. UP.
II (9/94)
HA (8/93)
(IB (1/95)
7470A
(Up. II)
7471 A
(Up. II)
-
-
FIN. UP.
Ill (12/96)
IIIA (4/98)
-
-
7472
(Up. Ill)
-
FIN. UP.
NIB
(11/04)
-
-
-
-
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
-
7471 B
-
7473
DRAFT
UP. IVB
(11/00)
-
-
-
-
OTHER
METHODS
(e.g., at
web site)
-
-
-
-
METHOD TITLE
Magnesium (Atomic Absorption, Direct
Aspiration)
Manganese (Atomic Absorption, Direct
Aspiration)
Manganese (Atomic Absorption, Furnace
Technique)
Mercury in Liquid Waste (Manual Cold-Vapor
Technique)
Mercury in Solid or Semisolid Waste (Manual
Cold-Vapor Technique)
Mercury in Aqueous Samples and Extracts by
Anodic Stripping Voltammetry (ASV)
Mercury in Solids and Solutions by Thermal
Decomposition, Amalgamation, and Atomic
Absorption Spectrophotometrv
16
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
7480
7481
7520
FINAL
UP. 1
(7/92)
~
FIN. UP.
II (9/94)
HA (8/93)
IIB (1/95)
~
FIN. UP.
Ill (12/96)
MIA (4/98)
-
7521
(Up. Ill)
FIN. UP.
IIIB
(11/04)
--
DRAFT
UP. IVA
(1/98)
7474
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
DRAFT
UP. IVB
(11/00)
-
OTHER
METHODS
(e.g., at
web site)
-
METHOD TITLE
Mercury in Sediment and Tissue Samples by
Atomic Fluorescence Spectrometry
Molybdenum (Atomic Absorption, Direct
Aspiration)
Molybdenum (Atomic Absorption, Furnace
Technique)
Nickel (Atomic Absorption, Direct Aspiration)
Nickel (Atomic Absorption, Furnace Method)
17
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
7550
-
7610
7740
7741
-
FINAL
UP. 1
(7/92)
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
7741A
(Up. II)
7742
(Uo. ID
FIN. UP.
Ill (12/96)
IIIA (4/98)
7580
(Up. Ill)
-
-
FIN. UP.
IIIB
(11/04)
-
-
-
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
-
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
OTHER
METHODS
(e.g., at
web site)
-
-
-
METHOD TITLE
Osmium (Atomic Absorption, Direct Aspiration)
White Phosphorus (PA) by Solvent Extraction
and Gas Chromatography
Potassium (Atomic Absorption, Direct
Aspiration)
Selenium (Atomic Absorption, Furnace
Technique)
Selenium (Atomic Absorption, Gaseous
Hydride)
Selenium (Atomic Absorption, Borohydride
Reduction)
18
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
7760
7770
7840
FINAL
UP. 1
(7/92)
7760A
7761
7780
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
FIN. UP.
Ill (12/96)
MIA (4/98)
FIN. UP.
IIIB
(11/04)
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
DRAFT
UP. IVB
(11/00)
OTHER
METHODS
(e.g., at
web site)
METHOD TITLE
Silver (Atomic Absorption, Direct Aspiration)
Silver (Atomic Absorption, Furnace Technique)
Sodium (Atomic Absorption, Direct Aspiration)
Strontium (Atomic Absorption, Direct
Aspiration)
Thallium (Atomic Absorption, Direct Aspiration)
19
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
7841
7870
7910
7911
7950
FINAL
UP. 1
(7/92)
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
FIN. UP.
Ill (12/96)
MIA (4/98)
FIN. UP.
IIIB
(11/04)
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
DRAFT
UP. IVB
(11/00)
OTHER
METHODS
(e.g., at
web site)
METHOD TITLE
Thallium (Atomic Absorption, Furnace
Technique)
Tin (Atomic Absorption, Direct Aspiration)
Vanadium (Atomic Absorption, Direct
Aspiration)
Vanadium (Atomic Absorption, Furnace
Technique)
Zinc (Atomic Absorption, Direct Aspiration)
20
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
8000
8010
-
8015
8020
-
FINAL
UP. 1
(7/92)
7951
8000A
801 OA
8011
801 5A
8021
FIN. UP.
II (9/94)
MA (8/93)
MB (1/95)
-
8010B
(Up. II)
-
-
8020A
(Up. II)
8021A
(Up. II)
FIN. UP.
Ill (12/96)
MIA (4/98)
8000B
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
-
8015B
Deleted
from
SW-846
(Up. Ill)
8021 B
(Up. Ill)
FIN. UP.
1MB
(11/04)
-
~~
-
-
-
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
-
~
-
-
-
DRAFT
UP. IVB
(11/00)
-
~~
-
8015C
-
OTHER
METHODS
(e.g., at
web site)
8000C
(3/03)
-
8015D
(6/03)
-
METHOD TITLE
Zinc (Atomic Absorption, Furnace Technique)
Determinative Chromatographic Separations
Halogenated Volatile Organics by Gas
Chromatography
1,2-Dibromoethane and 1 ,2-Dibromo-3-
chloropropane by Microextraction and Gas
Chromatography
Nonhalogenated Organics Using GC/FID
Aromatic Volatile Organics by Gas
Chromatography
Aromatic and Halogenated Volatiles by Gas
Chromatography Using Photoionization and/or
Electrolytic Conductivity Detectors
21
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
8030
-
-
-
8040
~
8060
-
-
FINAL
UP. I
(7/92)
8030A
-
-
-
8040A
-
-
8070
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
8031
(Up. II)
8032
(Up. II)
-
-
8061
(Up. II)
-
FIN. UP.
Ill (12/96)
IMA (4/98)
Deleted
from
SW-846
(Up. Ill)
-
8032A
(Up. Ill)
8033
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
8041
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
8061A
(Up. Ill)
8070A
(Up. Ill)
FIN. UP.
IIIB
(11/04)
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
8041A
-
-
OTHER
METHODS
(e.g., at
web site)
-
-
-
-
-
-
METHOD TITLE
Acrolein and Acrylonitrile by Gas
Chromatography
Acrylonitrile by Gas Chromatography
Acrylamide by Gas Chromatography
Acetonitrile by Gas Chromatography with
Nitrogen-Phosphorus Detection
Phenols by Gas Chromatography
Phenols by Gas Chromatography
Phthalate Esters
Phthalate Esters by Gas Chromatography with
Electron Capture Detection (GC/ECD)
Nitrosamines by Gas Chromatography
22
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
8080
~
8090
-
_
8100
FINAL
UP. 1
(7/92)
~
~
~~
~~
-
_
FIN. UP.
II (9/94)
1IA (8/93)
IIB (1/95)
8080A
(Up. II)
8081
(Up. II)
""
-
__
_
FIN. UP.
Ill (12/96)
IMA (4/98)
Deleted
from
SW-846
(Up. Ill)
8081A
(Up. Ill)
8082
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
8091
(Up. Ill)
__
FIN. UP.
1MB
(11/04)
~~
-
-
_
DRAFT
UP. IVA
(1/98)
8081 B
8082A
~
-
__
DRAFT
UP. IVB
(11/00)
--
8081 B
(Replaces
IVA
version)
8082A
(Replaces
IVA
version)
8085
-
8095
_
OTHER
METHODS
(e.g., at
web site)
~
_
-
_
_
METHOD TITLE
Organochlorine Pesticides and Polychlorinated
Biphenyls by Gas Chromatography
Organochlorine Pesticides by Gas
Chromatography
Polychlorinated Biphenyls (PCBs) by Gas
Chromatography
Compound-independent Elemental Quantitation
of Pesticides by Gas Chromatography with
Atomic Emission Detection (GC/AED)
Nitroaromatics and Cyclic Ketones
Nitroaromatics and Cyclic Ketones by Gas
Chromatography
Explosives by Gas Chromatography
Polynuclear Aromatic Hydrocarbons
23
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
8120
-
-
8140
~
FINAL
UP. I
(7/92)
8110
-
-
-
"
8141
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
~~
-
8120A
(Up. II)
8121
(Up. II)
-
~~
8141A
(Up. II)
FIN. UP.
Ill (12/96)
IIIA (4/98)
Deleted
from
SW-846
(Up. Ill)
8111
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
-
8131
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
"~
FIN. UP.
1MB
(11/04)
-
-
-
~~
DRAFT
UP. IVA
(1/98)
-
-
-
8141B
DRAFT
UP. IVB
(11/00)
-
-
-
8141B
(Replaces
IVA
version)
OTHER
METHODS
(e.g., at
web site)
-
-
-
METHOD TITLE
Haloethers by Gas Chromatography
Haloethers by Gas Chromatography
Chlorinated Hydrocarbons by Gas
Chromatography
Chlorinated Hydrocarbons by Gas
Chromatography: Capillary Column Technique
Aniline and Selected Derivatives by Gas
Chromatography
Organophosphorus Pesticides
8141 B: Organophosphorus Compounds by
Gas Chromatography
24
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
8150
-
8240
8250
-
-
FINAL
UP. I
(7/92)
8150A
-
8240A
8260
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
8150B
(Up. II)
8151
(Up. II)
8240B
(Up. II)
8250A
(Up. II)
8260A
(Up. II)
' -
FIN. UP.
Ill (12/96)
MIA (4/98)
Deleted
from
SW-846
(Up. Ill)
8151A
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
8260B
(Up. Ill)
-
FIN. UP.
IIIB
(11/04)
.
-
-
DRAFT
UP. IVA
(1/98)
~
_
-
-
DRAFT
UP. IVB
(11/00)
-
8261
-
OTHER
METHODS
(e.g., at
web site)
-
-
8265
(3/02)
METHOD TITLE
Chlorinated Herbicides by Gas
Chromatography
Chlorinated Herbicides by GC Using
Methylation or Pentafluorobenzylation
Derivatization
Volatile Organic Compounds by Gas
Chromatography/Mass Spectrometry (GC/MS)
Semivolatile Organic Compounds by Gas
Chromatography/Mass Spectrometry (GC/MS)
Volatile Organic Compounds by Gas
Chromatography/Mass Spectrometry (GC/MS)
Volatile Organic Compounds by Vacuum
Distillation in Combination with Gas
Chromatography/Mass Spectrometry
(VD/GC/MS)
Volatile Organic Compounds in Water, Soil,
Soil Gas and Air by Direct Sampling Ion Trap
Mass Spectrometrv (DSITMS)
25
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
8270
8280
8310
-
-
-
FINAL
UP. I
(7/92)
8270A
-
-
-
FIN. UP.
II (9/94)
HA (8/93)
IIB (1/95)
8270B
(Up. II)
8275
(Up. II)
8290
(Up. II)
8315
(Up. II)
8316
(Up. II)
8318
(Up. II)
FIN. UP.
Ill (12/96)
IIIA (4/98)
8270C
(Up. Ill)
8275A
(Up. Ill)
8280A
(Up. Ill)
_
831 5A
(Up. Ill)
-
-
FIN. UP.
IIIB
(11/04)
-
-
-
-
DRAFT
UP. IVA
(1/98)
8270D
8280B
8290A
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
831 8A
OTHER
METHODS
(e.g., at
web site)
-
-
-
-
METHOD TITLE
Semivolatile Organic Compounds by Gas
Chromatography/Mass Spectrometry (GC/MS)
Semivolatile Organic Compounds (PAHs and
PCBs) in Soils/Sludges and Solid Wastes
Using Thermal Extraction/Gas
Chromatography/Mass Spectrometry
(TE/GC/MS)
8280B: Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans by High
Resolution Gas Chromatography/Low
Resolution Mass Spectrometry (HRGC/LRMS)
Polychlorinated Dibenzodioxins (PCDDs) and
Polychlorinated Dibenzofurans (PCDFs) by
High-Resolution Gas Chromatography/
High-Resolution Mass Spectrometry
(HRGC/HRMS)
Polynuclear Aromatic Hydrocarbons
Determination of Carbonyl Compounds by High
Performance Liquid Chromatography (HPLC)
Acrylamide, Acrylonitrile and Acrolein by High
Performance Liquid Chromatography (HPLC)
/V-Methylcarbamates by High Performance
Liquid Chromatoqraphv (HPLC)
26
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
~
-
-
-
-
-
-
FINAL
UP. I
(7/92)
~~
-
-
-
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
8321
(Up. II)
-
8330
(Up. II)
8331
(Up. II)
-
8410
(Up. II)
-
FIN. UP.
Ill (12/96)
IMA (4/98)
8321A
(Up. Ill)
-
8325
(Up. Ill)
-
-
8332
(Up. Ill)
-
8430
(Up. Ill)
FIN. UP.
1MB
(11/04)
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
8321 B
-
8330A
-
-
-
-
DRAFT
UP. IVB
(11/00)
8321 B
(Replaces
IVA
version)
-
-
-
-
-
-
OTHER
METHODS
(e.g., at
web site)
~~
8323
(1/03)
-
-
-
-
-
METHOD TITLE
Solvent-Extractable Nonvolatile Compounds by
High Performance Liquid Chromatography/
Thermospray/Mass Spectrometry
(HPLC/TS/MS) or Ultraviolet (UV) Detection
Determination of Organotins by Micro-liquid
Chromatography-electrospray Ion Trap Mass
Spectrometry
Solvent Extractable Nonvolatile Compounds by
High Performance Liquid
Chromatography/Particle Beam/Mass
Spectrometry (HPLC/PB/MS)
Nitroaromatics and Nitramines by High
Performance Liquid Chromatography (HPLC)
Tetrazene by Reverse Phase High
Performance Liquid Chromatography (HPLC)
Nitroglycerine by High Performance Liquid
Chromatography
Gas Chromatography/Fourier Transform
Infrared (GC/FT-IR) Spectrometry for
Semivolatile Organics: Capillary Column
Analysis of Bis(2-chloroethyl) Ether and
Hydrolysis Products by Direct Aqueous
Injection GC/FT-IR
27
-------
SW-846 METHOD STATUS TABLE (11/04). CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
-
-
-
-
-
9010
9012
-
FINAL
UP. 1
(7/92)
-
-
-
-
-
-
901 OA
-
9013
FIN. UP.
II (9/94)
HA (8/93)
IIB (1/95)
' -
-
-
-
-
-
-
-
-
FIN. UP.
Ill (12/96)
IMA (4/98)
8440
(Up. Ill)
8515
(Up. Ill)
8520
(Up. Ill)
-
-
-
9010B
(Up. Ill)
9012A
(Up. Ill)
-
FIN. UP.
IIIB
(11/04)
-
-
-
-
-
-
-
9010C
9012B
-
DRAFT
UP. IVA
(1/98)
-
-
-
-
9000
9001
-
-
-
DRAFT
UP. IVB
(11/00)
-
8510
-
-
8535
8540
-
-
-
-
-
OTHER
METHODS
(e.g., at
web site)
-
-
-
-
-
-
-
-
-
-
METHOD TITLE
Total Recoverable Petroleum Hydrocarbons by
Infrared Spectrophotometry
Colorimetric Screening Procedure for RDX and
HMX in Soil
Colorimetric Screening Method for
Trinitrotoluene (TNT) in Soil
Continuous Measurement of Formaldehyde in
Ambient Air
Screening Procedure for Total Volatile Organic
Halides in Water
Pentachlorophenol by UV-induced Colorimetry
Determination of Water in Waste Materials by
Karl "Fischer Titration
Determination of Water in Waste Materials by
Quantitative Calcium Hydride Reaction
Total and Amenable Cyanide: Distillation
Total and Amenable Cyanide (Automated
Colorimetric, with Off-line Distillation)
Cyanide Extraction Procedure for Solids and
Oils
28
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
-
9020
9022
-
9030
ป
-
9035
9036
9038
FINAL
UP. I
(7/92)
-
-
9020A
9021
~
-
9030A
9031
-
-
_
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
-
9020B
(Up. II)
-
-
-
-
-
_
FIN. UP.
Ill (12/96)
MIA (4/98)
9014
(Up. Ill)
-
-
-
9023
(Up. Ill)
9030B
(Up. Ill)
_
9034
(Up. Ill)
-
_
FIN. UP.
NIB
(11/04)
-
-
-
~
-
-
-
-
_
DRAFT
UP. IVA
(1/98)
-
~
~
_
-
-
-
,,
-
-
_
DRAFT
UP. IVB
(11/00)
-
-
-
-
-
-
-
-
_
OTHER
METHODS
(e.g., at
web site)
-
9015
(9/04)
-
__
-
-
-
-
_
-
_
METHOD TITLE
Titrimetric and Manual Spectrophotometric
Determinative Methods for Cyanide
Metal Cyanide Complexes by Anion Exchange
Chromatography and UV Detection
Total Organic Halides (TOX)
Purgeable Organic Halides (POX)
Total Organic Halides (TOX) by Neutron
Activation Analysis
Extractable Organic Halides (EOX) in Solids
Acid-Soluble and Acid-Insoluble Sulfides:
Distillation
Extractable Sulfides
Titrimetric Procedure for Acid-Soluble and
Acid-Insoluble Sulfides
Sulfate (Colorimetric, Automated, Chloranilate)
Sulfate (Colorimetric, Automated,
Methylthymol Blue, AA II)
Sulfate (Turbidimetric)
29
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
9040
9041
9045
9050
-
-
9060
9065
FINAL
UP. 1
(7/92)
9041A
9045A
-
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
9040A
(Up. II)
9040B
(Up. IIB)
__
9045B
(Up. II)
9045C
(Up. IIB)
-
9056
(Up. II)
-
-
FIN. UP.
Ill (12/96)
MIA (4/98)
_
9050A
(Up. Ill)
-
9057
(Up. Ill)
-
FIN. UP.
IIIB
(11/04)
9040C
_
9045D
-
-
-
-
9060A
-
DRAFT
UP. IVA
(1/98)
~
-
-
-
DRAFT
UP. IVB
(11/00)
__
-
9056A
-
9058
-
OTHER
METHODS
(e.g., at
website)
-
-
-
-
-
METHOD TITLE
pH Electrometric Measurement
pH Paper Method
Soil and Waste pH
Specific Conductance
Determination of
Inorganic Anions by Ion Chromatography
Determination of Chloride from HCI/CI2
Emission Sampling Train (Methods 0050 and
0051) by Anion Chromatography
Determination of Perchlorate Using Ion
Chromatography with Chemical Suppression
Conductivity Detection
Total Organic Carbon
Phenolics (Spectrophotometric, Manual 4-AAP
with Distillation)
30
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
9066
9067
9070
9071
-
-
-
FINAL
UP. 1
(7/92)
-
-
-
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
-
9071A
(Up. II)
-
9075
(Up. II)
9076
(Up. II)
FIN. UP.
Ill (12/96)
IIIA (4/98)
-
-
9070
Title and
text
replaced
with
referral to
Method
1664
(Up. IIIA)
9071 B
(Up. IIIA)
-
-
-
FIN. UP.
IIIB
(11/04)
-
-
9070A
(Suffix and
title added)
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
~
-
9074
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
-
-
-
OTHER
METHODS
(e.g., at
web site)
-
-
-
-
-
-
METHOD TITLE
Phenolics (Colorimetric, Automated 4-AAP with
Distillation)
Phenolics (Spectrophotometric, MBTH with
Distillation)
n-Hexane Extractable Material (HEM) for
Aqueous Samples
(Method text is a referral to Method 1664: n-
Hexane Extractable Material (HEM; Oil and
Grease) and Silica Gel Treated n-Hexane
Extractable Material (SGT-HEM; Non-polar
Material) by Extraction and Gravimetry)
n-Hexane Extractable Material (HEM) for
Sludge, Sediment, and Solid Samples
Turbidimetric Screening Method for Total
Recoverable Petroleum Hydrocarbons in Soil
Test Method for Total Chlorine in New and
Used Petroleum Products by X-Ray
Fluorescence Spectrometry (XRF)
Test Method for Total Chlorine in New and
Used Petroleum Products by Oxidative
Combustion and Microcoulometry
31
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
-
-
-
9080
9081
9090
9095
-
9100
9131
9132
FINAL
UP. 1
(7/92)
-
-
-
-
-
9090A
-
-
-
-
_
FIN. UP.
II (9/94)
HA (8/93)
IIB (1/95)
9077
(Up. II)
-
-
-
-
-
-
9096
(Up. II)
-
-
_
FIN. UP.
Ill (12/96)
IIIA (4/98)
-
9078
(Up. Ill)
9079
(Up. Ill)
-
-
-
9095A
(Up. Ill)
-
-
-
_
FIN. UP.
1MB
(11/04)
-
- '
-
-
-
-
9095B
-
-
-
_
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
-
-
-
-
-
_
DRAFT
UP. IVB
(11/00)
-
-
-
-
-
~
-
-
-
-
_
OTHER
METHODS
(e.g., at
web site)
-
-
-
-
-
-
-
-
-
-
_
METHOD TITLE
Test Methods for Total Chlorine in New and
Used Petroleum Products (Field Test Kit
Methods)
Screening Test Method for Polychlorinated
Biphenyls in Soil
Screening Test Method for Polychlorinated
Biphenyls in Transformer Oil
Cation-Exchange Capacity of Soils
(Ammonium Acetate)
Cation-Exchange Capacity of Soils (Sodium
Acetate)
Compatibility Test for Wastes and Membrane
Liners
Paint Filter Liquids Test
Liquid Release Test (LRT) Procedure
Saturated Hydraulic Conductivity, Saturated
Leachate Conductivity, and Intrinsic
Permeability
Total Coliform: Multiple Tube Fermentation
Technique
Total Coliform: Membrane-Filter Technique
32
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
9200
-
-
-
-
-
-
-
9250
FINAL
UP. I
(7/92)
~~
-
-
-
-
-
-
-
-
FIN. UP.
II (9/94)
MA (8/93)
IIB (1/95)
"
-
-
-
-
-
-
-
-
FIN. UP.
Ill (12/96)
IIIA (4/98)
Deleted
from
SW-846
(Up. Ill)
9210
(Up. Ill)
9211
(Up. Ill)
9212
(Up. Ill)
9213
(Up. Ill)
9214
(Up. Ill)
9215
(Up. Ill)
-
-
FIN. UP.
1MB
(11/04)
-
-
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
"~
-
-
-
-
-
-
9216
-
DRAFT
UP. IVB
(11/00)
"
921 OA
-
-
~
-
-
-
-
OTHER
METHODS
(e.g., at
web site)
~~
-
-
-
-
-
-
-
-
METHOD TITLE
Nitrate
Potentiometric Determination of Nitrate in
Aqueous Samples with Ion-Selective Electrode
Potentiometric Determination of Bromide in
Aqueous Samples with Ion-Selective Electrode
Potentiometric Determination of Chloride in
Aqueous Samples with Ion-Selective Electrode
Potentiometric Determination of Cyanide in
Aqueous Samples and Distillates with Ion-
Selective Electrode
Potentiometric Determination of Fluoride in
Aqueous Samples with Ion-Selective Electrode
Potentiometric Determination of Sulfide in
Aqueous Samples and Distillates with Ion-
Selective Electrode
Potentiometric Determination of Nitrite in
Aqueous Samples with Ion-Selective Electrode
Chloride (Colorimetric, Automated Ferricyanide
AAI)
33
-------
SW-846 METHOD STATUS TABLE (11/04), CONTINUED
Note: The date in parenthesis is the date found at the bottom right-hand corner of the method.
METHOD NUMBER
THIRD
ED
(9/86)
9251
9252
-
9310
9315
9320
HCN
Test
Meth.
H2S Test
Meth.
FINAL
UP. 1
(7/92)
-
-
_.
__
HCN Test
Meth.
H2S Test
Meth.
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
9252A
(Up. II)
9253
(Up. II)
__
HCN Test
Method
(Up. II)
H2S Test
Method
(Up. II)
FIN. UP.
Ill (12/96)
IIIA (4/98)
-
Deleted
from
SW-846
(Up. Ill)
-
__
HCN Test
Method
(Up. Ill)
H2S Test
Method
(Up. Ill)
FIN. UP.
IIIB
(11/04)
-
-
__
Proposed
Removal
from
SW-846
Proposed
Removal
from
SW-846
DRAFT
UP. IVA
(1/98)
-
-
__
DRAFT
UP. IVB
(11/00)
-
-
_
~~
OTHER
METHODS
(e.g., at
web site)
-
-
,
METHOD TITLE
Chloride (Colorimetric, Automated Ferricyanide
AAII)
Chloride (Titrimetric, Mercuric Nitrate)
Chloride (Titrimetric, Silver Nitrate)
Gross Alpha and Gross Beta
Alpha-Emitting Radium Isotopes
Radium-228
Test Method to Determine Hydrogen Cyanide
Released from Wastes
Test Method to Determine Hydrogen Sulfide
Released from Wastes
34
-------
STATUS TABLE FOR SW-846 CHAPTER TEXT AND OTHER DOCUMENTS
Note: The date in parenthesis is the date found at the bottom right hand corner of the document.
TITLE
Disclaimer
Abstract
Table of Contents
Method Index and Conversion Table
Preface and Overview
Acknowledgments
Chapter One - Quality Control
Chapter Two - Choosing the Correct
Procedure
Chapter Three - Inorganic Analytes
THIRD ED.
(9/86)
-
/
/
/
/
/
/
/
/
FINAL
UP. 1
(7/92)
/
/
/
-
-
-
/
/
/
FIN. UP.
II (9/94)
MA (8/93)
IIB (1/95)
-
/ (Up. II)
/
(Up. II & IIB)
-
-
-
-
/ (Up. II)
/ (Up. II)
FINAL UP.
Ill (12/96)
IMA 4/98)
/ (Up. Ill)
-
/
(Up. Ill & MIA)
-
/ (Up. Ill)
-
-
/ (Up. Ill)
/ (Up. Ill)
DRAFT
UP. IVA
-
~
/
-
-
-
-
/
/
DRAFT
UP. IVB
-
-
/
(Replaces
IVA version)
-
-
-
/
(Replaces
IVA version)
/
(Replaces
IVA version)
FINAL
UP. 1MB
-
-
/
-
-
-
-
-
-
CURRENT
FINAL
VERSION
Rev1
(12/96)
Rev 2
(9/94)
Rev 6
(11/04)
RevO
(9/86)
Rev1
(12/96)
RevO
(9/86)
Rev1
(7/92)
Rev 3
(12/96)
Rev 3
(12/96)
35
-------
TITLE
Chapter Four Organic Analytes
Chapter Five Miscellaneous Test
Methods
Chapter Six Properties
Chapter Seven Characteristics
Introduction and Regulatory
Definitions
Chapter Eight -Methods for
Determining Characteristics
Chapter Nine - Sampling Plan
Chapter Ten Sampling Methods
Chapter Eleven Ground Water
Monitoring
Chapter Twelve - Land Treatment
Monitoring
Chapter Thirteen - Incineration
THIRD ED.
(9/86)
/
/
/
/
/
/
/
/
/
/
FINAL
UP. 1
(7/92)
-
-
-
/
-
-
-
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
/ (Up. II)
/ (Up. II)
/
(Up. II & IIB)
/ (Up. II)
/ (Up. II)
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Rev 3
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Rev 4
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Rev 4
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Rev 3
(11/04)
RevO
(9/86)
Rev 2
(12/96)
RevO
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TITLE
Appendix - Company References
THIRD ED.
(9/86)
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FINAL
UP. 1
(7/92)
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FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
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FINAL UP.
Ill (12/96)
MIA 4/98)
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UP. IVA
DRAFT
UP. IVB
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UP. 1MB
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CURRENT
FINAL
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RevO
(9/86)
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TABLE OF CONTENTS
VOLUME ONE
SECTION A
DISCLAIMER
ABSTRACT
TABLE OF CONTENTS
METHOD INDEX AND CONVERSION TABLE
PREFACE
ACKNOWLEDGEMENTS
PART I METHODS FOR ANALYTES AND PROPERTIES
CHAPTER ONE - QUALITY CONTROL
1.0 Introduction
2.0 QA Project Plan
3.0 Field Operations
4.0 Laboratory Operations
5.0 Definitions
6.0 References
CHAPTER TWO - CHOOSING THE CORRECT PROCEDURE
2.1 Purpose
2.2 Required Information
2.3 Implementing the Guidance
2.4 Characteristics
2.5 Ground Water
2.6 References
CHAPTER THREE - INORGANIC ANALYTES
3.1 Sampling Considerations
3.2 Sample Preparation Methods
Method 3005A: Acid Digestion of Waters for Total Recoverable or Dissolved Metals
for Analysis by FLAA or ICP Spectroscopy
Method 301OA: Acid Digestion of Aqueous Samples and Extracts for Total Metals
for Analysis by FLAA or ICP Spectroscopy
Method 3015: Microwave Assisted Acid Digestion of Aqueous Samples and
Extracts
Method 3020A: Acid Digestion of Aqueous Samples and Extracts for Total Metals
for Analysis by GFAA Spectroscopy
Method 3031: Acid Digestion of Oils for Metals Analysis by Atomic Absorption or
ICP Spectrometry
CONTENTS - 1 Revision 6
November 2004
-------
Method 3040A:
Method 3050B:
Method 3051:
Method 3052:
Method 3060A:
Dissolution Procedure for Oils, Greases, or Waxes
Acid Digestion of Sediments, Sludges, and Soils
Microwave Assisted Acid Digestion of Sediments, Sludges, Soils,
and Oils
Microwave Assisted Acid Digestion of Siliceous and Organically
Based Matrices
Alkaline Digestion for Hexavalent Chromium
3.3 Methods for Determination of Inorganic Analytes
Method 601 OB: Inductively Coupled Plasma-Atomic Emission Spectrometry
Method 6020: Inductively Coupled Plasma-Mass Spectrometry
Method 7000A: Atomic Absorption Methods
Method 7020: Aluminum (Atomic Absorption, Direct Aspiration)
Method 7040: Antimony (Atomic Absorption, Direct Aspiration)
Method 7041: Antimony (Atomic Absorption, Furnace Technique)
Method 7060A: Arsenic (Atomic Absorption, Furnace Technique)
Method 7061A: Arsenic (Atomic Absorption, Gaseous Hydride)
Method 7062: Antimony and Arsenic (Atomic Absorption, Borohydride Reduction)
Method 7063: Arsenic in Aqueous Samples and Extracts by Anodic Stripping
Voltammetry (ASV)
Method 7080A: Barium (Atomic Absorption, Direct Aspiration)
Method 7081: Barium (Atomic Absorption, Furnace Technique)
Method 7090: Beryllium (Atomic Absorption, Direct Aspiration)
Method 7091: Beryllium (Atomic Absorption, Furnace Technique)
Method 7130: Cadmium (Atomic Absorption, Direct Aspiration)
Method 7131 A: Cadmium (Atomic Absorption, Furnace Technique)
Method 7140: Calcium (Atomic Absorption, Direct Aspiration)
Method 7190: Chromium (Atomic Absorption, Direct Aspiration)
Method 7191: Chromium (Atomic Absorption, Furnace Technique)
Method 7195: Chromium, Hexavalent (Coprecipitation)
Method 7196A: Chromium, Hexavalent (Colorimetric)
Method 7197: Chromium, Hexavalent (Chelation/Extraction)
Method 7198: Chromium, Hexavalent (Differential Pulse Polarography)
Method 7199: Determination of Hexavalent Chromium in Drinking Water,
Groundwater and Industrial Wastewater Effluents by Ion
Chromatography
Method 7200: Cobalt (Atomic Absorption, Direct Aspiration)
Method 7201: Cobalt (Atomic Absorption, Furnace Technique)
Method 7210: Copper (Atomic Absorption, Direct Aspiration)
Method 7211: Copper (Atomic Absorption, Furnace Technique)
Method 7380: Iron (Atomic Absorption, Direct Aspiration)
Method 7381: Iron (Atomic Absorption, Furnace Technique)
Method 7420: Lead (Atomic Absorption, Direct Aspiration)
Method 7421: Lead (Atomic Absorption, Furnace Technique)
Method 7430: Lithium (Atomic Absorption, Direct Aspiration)
Method 7450: Magnesium (Atomic Absorption, Direct Aspiration)
Method 7460: Manganese (Atomic Absorption, Direct Aspiration)
CONTENTS - 2
Revision 6
November 2004
-------
Method 7461:
Method 7470A:
Method 7471 A:
Method 7472:
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
7480:
7481:
7520:
7521:
7550:
7580:
7610:
7740:
7741 A:
7742:
7760A:
7761:
7770:
7780:
7840:
7841:
7870:
7910:
7911:
7950:
7951:
Manganese (Atomic Absorption, Furnace Technique)
Mercury in Liquid Waste (Manual Cold-Vapor Technique)
Mercury in Solid or Semisolid Waste (Manual Cold-Vapor
Technique)
Mercury in Aqueous Samples and Extracts by Anodic Stripping
Voltammetry (ASV)
Molybdenum (Atomic Absorption, Direct Aspiration)
Molybdenum (Atomic Absorption, Furnace Technique)
Nickel (Atomic Absorption, Direct Aspiration)
Nickel (Atomic Absorption, Furnace Method)
Osmium (Atomic Absorption, Direct Aspiration)
White Phosphorus (P4) by Solvent Extraction and Gas
Chromatography
Potassium (Atomic Absorption, Direct Aspiration)
Selenium (Atomic Absorption, Furnace Technique)
Selenium (Atomic Absorption, Gaseous Hydride)
Selenium (Atomic Absorption, Borohydride Reduction)
Silver (Atomic Absorption, Direct Aspiration)
Silver (Atomic Absorption, Furnace Technique)
Sodium (Atomic Absorption, Direct Aspiration)
Strontium (Atomic Absorption, Direct Aspiration)
Thallium (Atomic Absorption, Direct Aspiration)
Thallium (Atomic Absorption, Furnace Technique)
Tin (Atomic Absorption, Direct Aspiration)
Vanadium (Atomic Absorption, Direct Aspiration)
Vanadium (Atomic Absorption, Furnace Technique)
Zinc (Atomic Absorption, Direct Aspiration)
Zinc (Atomic Absorption, Furnace Technique)
APPENDIX - COMPANY REFERENCES
NOTE: A suffix of "A" in the method number indicates revision one (the method has
been revised once). A suffix of "B" in the method number indicates revision two (the
method has been revised twice). A suffix of "C" in the method number indicates
revision three (the method has been revised three times), etc. In order to properly
document the method used for analysis, the entire method number including
the suffix letter designation (e.g., A, B, C or D) must be identified by the
analyst. A method reference found within the RCRA regulations and the text of SW-
846 methods and chapters refers to the latest final revision of the method, even if the
method number does not include the appropriate letter suffix.
CONTENTS - 3
Revision 6
November 2004
-------
VOLUME ONE
SECTION B
DISCLAIMER
ABSTRACT
TABLE OF CONTENTS
METHOD INDEX AND CONVERSION TABLE
PREFACE
ACKNOWLEDGEMENTS
CHAPTER ONE. REPRINTED - QUALITY CONTROL
1.0 Introduction
2.0 QA Project Plan
3.0 Field Operations
4.0 Laboratory Operations
5.0 Definitions
6.0 References
CHAPTER FOUR - ORGANIC ANALYTES
4.1 Sampling Considerations
4.2 Sample Preparation Methods
4.2.1 Extractions and Preparations
Method 3500B: Organic Extraction and Sample Preparation
Method 351OC: Separatory Funnel Liquid-Liquid Extraction
Method 3520C: Continuous Liquid-Liquid Extraction
Method 3535: Solid-Phase Extraction (SPE)
Method 3540C: Soxhlet Extraction
Method 3541: Automated Soxhlet Extraction
Method 3542: Extraction of Semivolatile Analytes Collected Using Method 0010
(Modified Method 5 Sampling Train)
Method 3545: Pressurized Fluid Extraction (PFE)
Method 3550B: Ultrasonic Extraction
Method 3560: Supercritical Fluid Extraction of Total Recoverable Petroleum
Hydrocarbons
Method 3561: Supercritical Fluid Extraction of Polynuclear Aromatic Hydrocarbons
Method 3580A: Waste Dilution
Method 3585: Waste Dilution for Volatile Organics
Method 5000: Sample Preparation for Volatile Organic Compounds
CONTENTS - 4 Revision 6
November 2004
-------
Method 5021:
Method 5030B:
Method 5031:
Method 5032:
Method 5035:
Method 5041A:
4.2.2 Cleanup
Method 3600C:
Method 361 OB:
Method 3611B:
Method 3620B:
Method 3630C:
Method 3640A:
Method 3650B:
Method 3660B:
Method 3665A:
Volatile Organic Compounds in Soils and Other Solid Matrices
Using Equilibrium Headspace Analysis
Purge-and-Trap for Aqueous Samples
Volatile, Nonpurgeable, Water-Soluble Compounds by Azeotropic
Distillation
Volatile Organic Compounds by Vacuum Distillation
Closed-System Purge-and-Trap and Extraction for Volatile Organics
in Soil and Waste Samples
Analysis for Desorption of Sorbent Cartridges from Volatile Organic
Sampling Train (VOST)
Cleanup
Alumina Cleanup
Alumina Column Cleanup and Separation of Petroleum Wastes
Florisil Cleanup
Silica Gel Cleanup
Gel-Permeation Cleanup
Acid-Base Partition Cleanup
Sulfur Cleanup
Sulfuric Acid/Permanganate Cleanup
4.3 Determination of Organic Analytes
4.3.1 Gas Chromatographic Methods
Method 8000B:
Method 8011:
Method 8015B:
Method 8021B:
Method 8031:
Method 8032A:
Method 8033:
Method 8041:
Method 8061A:
Method
Method
Method
Method
Method
Method
Method
8070A:
8081A:
8082:
8091:
8100:
8111:
8121:
Determinative Chromatographic Separations
1,2-Dibromoethane and 1,2-Dibromo-3-chloropropane by
Microextraction and Gas Chromatography
Nonhalogenated Organics Using GC/FID
Aromatic and Halogenated Volatiles by Gas Chromatography Using
Photoionization and/or Electrolytic Conductivity Detectors
Acrylonitrile by Gas Chromatography
Acrylamide by Gas Chromatography
Acetonitrile by Gas Chromatography with Nitrogen-Phosphorus
Detection
Phenols by Gas Chromatography
Phthalate Esters by Gas Chromatography with Electron Capture
Detection (GC/ECD)
Nitrosamines by Gas Chromatography
Organochlorine Pesticides by Gas Chromatography
Polychlorinated Biphenyls (PCBs) by Gas Chromatography
Nitroaromatics and Cyclic Ketones by Gas Chromatography
Polynuclear Aromatic Hydrocarbons
Haloethers by Gas Chromatography
Chlorinated Hydrocarbons by Gas Chromatography: Capillary
Column Technique
CONTENTS - 5
Revision 6
November 2004
-------
Method 8131: Aniline and Selected Derivatives by Gas Chromatography
Method 8141A: Organophosphorus Compounds by Gas Chromatography: Capillary
Column Technique
Method 8151A: Chlorinated Herbicides by GC Using Methylation or
Pentafluorobenzylation Derivatization
4.3.2 Gas Chromatographic/Mass Spectroscopic Methods
Method 8260B: Volatile Organic Compounds by Gas Chromatography/Mass
Spectrometry (GC/MS)
Method 8270C: Semivolatile Organic Compounds by Gas Chromatography/Mass
Spectrometry (GC/MS)
Method 8275A: Semivolatile Organic Compounds (PAHs and PCBs) in
Soils/Sludges and Solid Wastes Using Thermal Extraction/Gas
Chromatography/Mass Spectrometry (TE/GC/MS)
Method 8280A: The Analysis of Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans by High Resolution Gas
Chromatography/Low Resolution Mass Spectrometry
(HRGC/LRMS)
Method 8290: Polychlorinated Dibenzodioxins (PCDDs) and Polychlorinated
Dibenzofurans (PCDFs) by High-Resolution Gas
Chromatography/High-Resolution Mass Spectrometry
(HRGC/HRMS)
Attachment A: Procedures for the Collection, Handling, Analysis, and
Reporting of Wipe Tests Performed within the Laboratory
4.3.3 High Performance Liquid Chromatographic Methods
Method 8310: Polynuclear Aromatic Hydrocarbons
Method 8315A: Determination of Carbonyl Compounds by High Performance Liquid
Chromatography (HPLC)
Appendix A: Recrystallization of 2,4-Dinitrophenylhydrazine (DNPH)
Method 8316: Acrylamide, Acrylonitrile and Acrblein by High Performance Liquid
Chromatography (HPLC)
Method 8318: N-Methylcarbamates by High Performance Liquid Chromatography
(HPLC)
Method 8321 A: Solvent Extractable Nonvolatile Compounds by High Performance
Liquid Chromatography/Thermospray/Mass Spectrometry
(HPLCn~S/MS) or Ultraviolet (UV) Detection
Method 8325: Solvent Extractable Nonvolatile Compounds by High Performance
Liquid Chromatography/Particle Beam/Mass Spectrometry
(HPLC/PB/MS)
Method 8330: Nitroaromatics and Nitramines by High Performance Liquid
Chromatography (HPLC)
Method 8331: Tetrazene by Reverse Phase High Performance Liquid
Chromatography (HPLC)
Method 8332: Nitroglycerine by High Performance Liquid Chromatography
CONTENTS - 6 Revision 6
November 2004
-------
4.3.4 Infrared Methods
Method 8410: Gas Chromatography/Fourier Transform Infrared (GC/FT-IR)
Spectrometry for Semivolatile Organics: Capillary Column
Method 8430: Analysis of Bis(2-chloroethyl) Ether and Hydrolysis Products by
Direct Aqueous Injection GC/FT-IR
Method 8440: Total Recoverable Petroleum Hydrocarbons by Infrared
Spectrophotometry
4.3.5 Miscellaneous Spectrometric Methods
Method 8520: Continuous Measurement of Formaldehyde in Ambient Air
4.4 Immunoassay Methods
Method 4000: Immunoassay
Method 401OA: Screening for Pentachlorophenol by Immunoassay
Method 4015: Screening for 2,4-Dichlorophenoxyacetic Acid by Immunoassay
Method 4020: Screening for Polychlorinated Biphenyls by Immunoassay
Method 4030: Soil Screening for Petroleum Hydrocarbons by Immunoassay
Method 4035: Soil Screening for Polynuclear Aromatic Hydrocarbons by
Immunoassay
Method 4040: Soil Screening for Toxaphene by Immunoassay
Method 4041: Soil Screening for Chlordane by Immunoassay
Method 4042: Soil Screening for DDT by Immunoassay
Method 4050: TNT Explosives in Soil by Immunoassay
Method 4051: Hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in Soil by
Immunoassay
4.5 Miscellaneous Screening Methods
Method 3810: Headspace
Method 3820: Hexadecane Extraction and Screening of Purgeable Organics
Method 8515: Colorimetric Screening Method for Trinitrotoluene (TNT) in Soil
Method 9078: Screening Test Method for Polychlorinated Biphenyls in Soil
Method 9079: Screening Test Method for Polychlorinated Biphenyls in
Transformer Oil
APPENDIX - COMPANY REFERENCES
CONTENTS - 7 Revision 6
November 2004
-------
NOTE: A suffix of "A" in the method number indicates revision one (the method has
been revised once). A suffix of "B" in the method number indicates revision two (the
method has been revised twice). A suffix of "C" in the method number indicates
revision three (the method has been revised three times), etc. In order to properly
document the method used for analysis, the entire method number including
the suffix letter designation (e.g., A, B, C or D) must be identified by the
analyst. A method reference found within the RCRA regulations and the text of SW-
846 methods and chapters refers to the latest final revision of the method, even if the
method number does not include the appropriate letter suffix.
CONTENTS - 8 Revision 6
November 2004
-------
VOLUME ONE
SECTION C
DISCLAIMER
ABSTRACT
TABLE OF CONTENTS
METHOD INDEX AND CONVERSION TABLE
PREFACE
CHAPTER ONE. REPRINTED - QUALITY CONTROL
1.0 Introduction
2.0 QA Project Plan
3.0 Field Operations
4.0 Laboratory Operations
5.0 Definitions
6.0 References
CHAPTER FIVE - MISCELLANEOUS TEST METHODS
Method 5050:
Method 901OC:
Method 9012B:
Method 9013:
Method 9014:
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
9020B:
9021:
9022:
9023:
9030B:
9031:
9034:
9035:
9036:
9038:
9056:
9057:
Method 9060A:
Method 9065:
Method 9066:
Method 9067:
Method 9070A:
Bomb Preparation Method for Solid Waste
Total and Amenable Cyanide: Distillation
Total and Amenable Cyanide (Automated Colorimetric, with Off-Line
Distillation)
Cyanide Extraction Procedure for Solids and Oils
Titrimetric and Manual Spectrophotometric Determinative Methods
for Cyanide
Total Organic Halides (TOX)
Purgeable Organic Halides (POX)
Total Organic Halides (TOX) by Neutron Activation Analysis
Extractable Organic Halides (EOX) in Solids
Acid-Soluble and Acid-Insoluble Sulfides: Distillation
Extractable Sulfides
Titrimetric Procedure for Acid-Soluble and Acid-Insoluble Sulfides
Sulfate (Colorimetric, Automated, Chloranilate)
Sulfate (Colorimetric, Automated, Methylthymol Blue, AAII)
Sulfate (Turbidimetric)
Determination of Inorganic Anions by Ion Chromatography
Determination of Chloride from HCI/CI2 Emission Sampling Train
(Methods 0050 and 0051) by Anion Chromatography
Total Organic Carbon
Phenolics (Spectrophotometric, Manual 4-AAP with Distillation)
Phenolics (Colorimetric, Automated 4-AAP with Distillation)
Phenolics (Spectrophotometric, MBTH with Distillation)
n-Hexane Extractable Material (HEM) for Aqueous Samples
CONTENTS - 9
Revision 6
November 2004
-------
Method 9071B:
Method 9075:
Method 9076:
Method 9077:
Method A:
Method B:
Method C:
Method 9131:
Method 9132:
Method 9210:
Method 9211:
Method 9212:
Method 9213:
Method 9214:
Method 9215:
Method 9250:
Method 9251:
Method 9253:
Method 9320:
n-Hexane Extractable Material (HEM) for Sludge, Sediment, and
Solid Samples
Test Method for Total Chlorine in New and Used Petroleum
Products by X-Ray Fluorescence Spectrometry (XRF)
Test Method for Total Chlorine in New and Used Petroleum
Products by Oxidative Combustion and Microcoulometry
Test Methods for Total Chlorine in New and Used Petroleum
Products (Field Test Kit Methods)
Fixed End Point Test Kit Method
Reverse Titration Quantitative End Point Test Kit Method
Direct Titration Quantitative End Point Test Kit Method
Total Coliform: Multiple Tube Fermentation Technique
Total Coliform: Membrane-Filter Technique
Potentiometric Determination of Nitrate in Aqueous Samples with
Ion-Selective Electrode
Potentiometric Determination of Bromide in Aqueous Samples with
Ion-Selective Electrode
Potentiometric Determination of Chloride in Aqueous Samples with
Ion-Selective Electrode
Potentiometric Determination of Cyanide in Aqueous Samples and
Distillates with Ion-Selective Electrode
Potentiometric Determination of Fluoride in Aqueous Samples with
Ion-Selective Electrode
Potentiometric Determination of Sulfide in Aqueous Samples and
Distillates with Ion-Selective Electrode
Chloride (Colorimetric, Automated Ferricyanide AAI)
Chloride (Colorimetric, Automated Ferricyanide AAII)
Chloride (Titrimetric, Silver Nitrate)
Radium-228
CHAPTER SIX - PROPERTIES
Method 1030:
Method 1120:
Method 1312:
Method 1320:
Method 1330A:
Method 9041A:
Method 9045D:
Method 9050A:
Method 9080:
Method 9081:
Method 9090A:
Method 9095B:
Method 9096:
Appendix A:
Ignitability of Solids
Dermal Corrosion
Synthetic Precipitation Leaching Procedure
Multiple Extraction Procedure
Extraction Procedure for Oily Wastes
pH Paper Method
Soil and Waste pH
Specific Conductance
Cation-Exchange Capacity of Soils (Ammonium Acetate)
Cation-Exchange Capacity of Soils (Sodium Acetate)
Compatibility Test for Wastes and Membrane Liners
Paint Filter Liquids Test
Liquid Release Test (LRT) Procedure
Liquid Release Test Pre-Test
CONTENTS-10
Revision 6
November 2004
-------
Method 9100:
Method 9310:
Method 9315:
Saturated Hydraulic Conductivity, Saturated Leachate Conductivity,
and Intrinsic Permeability
Gross Alpha and Gross Beta
Alpha-Emitting Radium Isotopes
PART II CHARACTERISTICS
CHAPTER SEVEN - CHARACTERISTICS INTRODUCTION AND REGULATORY DEFINITIONS
7.1 Ignitability
7.2 Corrosivity
7.3 Reactivity
7.4 Toxicity Characteristic Leaching Procedure
CHAPTER EIGHT - METHODS FOR DETERMINING CHARACTERISTICS
8.1 Ignitability
Method 101OA:
Method 1020B:
Test Methods for Flash Point by Pensky-Martens Closed Cup
Tester
Standard Test Methods for Flash Point by Setaflash (Small Scale)
Closed-cup Apparatus
8.2 Corrosivity
Method 9040C:
Method 1110A:
8.3 Toxicity
Method 131 OB:
Method 1311:
pH Electrometric Measurement
Corrosivity Toward Steel
Extraction Procedure (EP) Toxicity Test Method and Structural
Integrity Test
Toxicity Characteristic Leaching Procedure
APPENDIX - COMPANY REFERENCES
CONTENTS-11
Revision 6
November 2004
-------
NOTE: A suffix of "A" in the method number indicates revision one (the method has
been revised once). A suffix of "B" in the method number indicates revision two (the
method has been revised twice). A suffix of "C" in the method number indicates
revision three (the method has been revised three times), etc. In order to properly
document the method used for analysis, the entire method number including
the suffix letter designation (e.g., A, B, C or D) must be identified by the
analyst. A method reference found within the RCRA regulations and the text of SW-
846 methods and chapters refers to the latest final revision of the method, even if the
method number does not include the appropriate letter suffix.
CONTENTS -12 Revision 6
November 2004
-------
VOLUME TWO
DISCLAIMER
ABSTRACT
TABLE OF CONTENTS
METHOD INDEX AND CONVERSION TABLE
PREFACE
CHAPTER ONE, REPRINTED - QUALITY CONTROL
1.0 Introduction
2.0 QA Project Plan
3.0 Field Operations
4.0 Laboratory Operations
5.0 Definitions
6.0 References
PART III SAMPLING
CHAPTER NINE - SAMPLING PLAN
9.1 Design and Development
9.2 Implementation
CHAPTER TEN - SAMPLING METHODS
Method 0010: Modified Method 5 Sampling Train
Appendix A: Preparation of XAD-2 Sorbent Resin
Appendix B: Total Chromatographable Organic Material Analysis
Method 0011: Sampling for Selected Aldehyde and Ketone Emissions from
Stationary Sources
Method 0020: Source Assessment Sampling System (SASS)
Method 0023A: Sampling Method for Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofuran Emissions from Stationary Sources
Method 0030: Volatile Organic Sampling Train
Method 0031: Sampling Method for Volatile Organic Compounds (SMVOC)
Method 0040: Sampling of Principal Organic Hazardous Constituents from
Combustion Sources Using Tedlarฎ Bags
Method 0050: Isokinetic HCI/CI2 Emission Sampling Train
Method 0051: Midget Impinger HCI/CI2 Emission Sampling Train
Method 0060: Determination of Metals in Stack Emissions
Method 0061: Determination of Hexavalent Chromium Emissions from Stationary
Sources
CONTENTS - 13 Revision 6
November 2004
-------
Method 0100: Sampling for Formaldehyde and Other Carbonyl Compounds in
Indoor Air
CONTENTS -14 Revision 6
November 2004
-------
PART IV MONITORING
CHAPTER ELEVEN - GROUND WATER MONITORING
11.1 Background and Objectives
11.2 Relationship to the Regulations and to Other Documents
11.3 Revisions and Additions
11.4 Acceptable Designs and Practices
11.5 Unacceptable Designs and Practices
CHAPTER TWELVE - LAND TREATMENT MONITORING
12.1 Background
12.2 Treatment Zone
12.3 Regulatory Definition
12.4 Monitoring and Sampling Strategy
12.5 Analysis
12.6 References and Bibliography
CHAPTER THIRTEEN - INCINERATION
13.1 Introduction
13.2 Regulatory Definition
13.3 Waste Characterization Strategy
13.4 Stack-Gas Effluent Characterization Strategy
13.5 Additional Effluent Characterization Strategy
13.6 Selection of Specific Sampling and Analysis Methods
13.7 References
APPENDIX - COMPANY REFERENCES
NOTE: A suffix of "A" in the method number indicates revision one (the method has
been revised once). A suffix of "B" in the method number indicates revision two (the
method has been revised twice). A suffix of "C" in the method number indicates
revision three (the method has been revised three times), etc. In order to properly
document the method used for analysis, the entire method number including
the suffix letter designation (e.g., A, B, C or D) must be identified by the
analyst. A method reference found within the RCRA regulations and the text of SW-
846 methods and chapters refers to the latest final revision of the method, even
though the method number does not include the appropriate letter suffix.
CONTENTS - 15 Revision 6
November 2004
-------
CHAPTER FIVE
MISCELLANEOUS TEST METHODS
Prior to employing the methods in this chapter, analysts are advised to consult the
disclaimer statement at the front of this manual and the information in Chapter Two for guidance
on the allowed flexibility in the choice of apparatus, reagents, and supplies. Procedures for
required method-defined parameters are not subject to the same flexibility afforded in other SW-
846 methods. In addition, unless specified in a regulation, the use of SW-846 methods is not
mandatory in response to Federal testing requirements. The information contained in each
procedure is provided by EPA as guidance to be used by the analyst and the regulated community
in making judgements necessary to meet the data quality objectives or needs for the intended use
of the data.
The following methods are found in Chapter Five:
Method 5050:
Method 901OC:
Method 9012B:
Method 9013:
Method 9014:
Method
Method
Method
Method
Method
Method
Method
9020B:
9021:
9022:
9023:
9030B:
9031:
9034:
Method 9035:
Method 9036:
Method 9038:
Method 9056:
Method 9057:
Method 9060A:
Method 9065:
Method 9066:
Method 9067:
Method 9070A:
Method 9071B:
Bomb Preparation Method for Solid Waste
Total and Amenable Cyanide: Distillation
Total and Amenable Cyanide (Automated Colorimetric, with
Off-Line Distillation)
Cyanide Extraction Procedure for Solids and Oils
Titrimetric and Manual Spectrophotometric Determinative
Methods for Cyanide
Total Organic Halides (TOX)
Purgeable Organic Halides (POX)
Total Organic Halides (TOX) by Neutron Activation Analysis
Extractable Organic Halides (EOX) in Solids
Acid-Soluble and Acid-Insoluble Sulfides: Distillation
Extractable Sulfides
Titrimetric Procedure for Acid-Soluble and Acid-Insoluble
Sulfides
Sulfate (Colorimetric, Automated, Chloranilate)
Sulfate (Colorimetric, Automated, Methylthymol Blue, AAII)
Sulfate (Turbidimetric)
Determination of Inorganic Anions by Ion Chromatography
Determination of Chloride from HCI/CI2 Emission Sampling
Train (Methods 0050 and 0051) by Anion Chromatography
Total Organic Carbon
Phenolics (Spectrophotometric, Manual 4-AAP with
Distillation)
Phenolics (Colorimetric, Automated 4-AAP with Distillation)
Phenolics (Spectrophotometric, MBTH with Distillation)
n-Hexane Extractable Material (HEM) for Aqueous Samples
n-Hexane Extractable Material (HEM) for Sludge, Sediment,
and Solid Samples
FIVE -1
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Method 9075:
Method 9076:
Method 9077:
Method A:
Method B:
Method C:
Method 9131:
Method 9132:
Method 9210:
Method 9211:
Method 9212:
Method 9213:
Method 9214:
Method 9215:
Method 9250:
Method 9251:
Method 9253:
Method 9320:
Test Method for Total Chlorine in New and Used Petroleum
Products by X-Ray Fluorescence Spectrometry (XRF)
Test Method for Total Chlorine in New and Used Petroleum
Products by Oxidative Combustion and Microcoulometry
Test Methods for Total Chlorine in New and Used
Petroleum Products (Field Test Kit Methods)
Fixed End Point Test Kit Method
Reverse Titration Quantitative End Point Test Kit Method
Direct Titration Quantitative End Point Test Kit Method
Total Coliform: Multiple Tube Fermentation Technique
Total Coliform: Membrane-Filter Technique
Potentiometric Determination of Nitrate in Aqueous Samples
with Ion-Selective Electrode
Potentiometric Determination of Bromide in Aqueous
Samples with Ion-Selective Electrode
Potentiometric Determination of Chloride in Aqueous
Samples with Ion-Selective Electrode
Potentiometric Determination of Cyanide in Aqueous
Samples and Distillates with Ion-Selective Electrode
Potentiometric Determination of Fluoride in Aqueous
Samples with Ion-Selective Electrode
Potentiometric Determination of Sulfide in Aqueous Samples
and Distillates with Ion-Selective Electrode
Chloride (Colorimetric, Automated Ferricyanide AAI)
Chloride (Colorimetric, Automated Ferricyanide AAII)
Chloride (Titrimetric, Silver Nitrate)
Radium-228
FIVE - 2
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METHOD 901OC
TOTAL AND AMENABLE CYANIDE: DISTILLATION
1.0 SCOPE AND APPLICATION
1.1 This method is a reflux-distillation procedure used to extract soluble cyanide salts
and many insoluble cyanide complexes from wastes and leachates. It is based on the
decomposition of nearly all cyanides by a reflux distillation procedure using a strong acid and a
magnesium catalyst. Cyanide, in the form of hydrocyanic acid (HCN) is purged from the
sample and captured into an alkaline scrubber solution. The concentration of cyanide in the
scrubber solution is then determined by Method 9014 or Method 9213. This method may be
used as a reflux-distillation procedure for both total cyanide and cyanide amenable to
chlorination. The "reactive" cyanide content of a waste is not determined by this method. Refer
to 40 CFR 261.23 for information on the characteristic of reactivity.
1.2 This method was designed to address the problem of "trace" analyses (<1000
ppm). The method may also be used for "minor" (1000 ppm -10,000 ppm) and "major"
(>10,000 ppm) analyses by adapting the appropriate sample dilution. However, the amount of
sodium hydroxide in the standards and the sample analyzed must be the same.
2.0 SUMMARY OF METHOD
2.1 The cyanide, as hydrocyanic acid (HCN), is released from samples containing
cyanide by means of a reflux-distillation operation under acidic conditions and absorbed in a
scrubber containing sodium hydroxide solution. The cyanide concentration in the absorbing
solution is then determined colorimetrically or titrametrically by Method 9014 or by ion-selective
electrode by Method 9213.
3.0 INTERFERENCES
3.1 Interferences are eliminated or reduced by using the distillation procedure.
Chlorine and sulfide are interferences in Method 9010.
3.2 Oxidizing agents such as chlorine decompose most cyanides. Chlorine
interferences can be removed by adding an excess of sodium arsenite to the waste prior to
preservation and storage of the sample to reduce the chlorine to chloride which does not
interfere.
3.3 Sulfide interference can be removed by adding an excess of bismuth nitrate to the
waste (to precipitate the sulfide) before distillation. Samples that contain hydrogen sulfide,
metal sulfides, or other compounds that may produce hydrogen sulfide during the distillation
should be treated by the addition of bismuth nitrate.
3.4 High results may be obtained for samples that contain nitrate and/or nitrite. During
the distillation, nitrate and nitrite will form nitrous acid, which will react with some organic
compounds to form oximes. These compounds once formed will decompose under test
conditions to generate HCN. The possibility of interference of nitrate and nitrite is eliminated by
pretreatment with sulfamic acid just before distillation. Nitrate and nitrite are interferences when
present at levels higher than 10 mg/L and in conjunction with certain organic compounds.
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3.5 Thiocyanate is reported to be an interference when present at very high levels.
Levels of 10 mg/L were not found to interfere.
3.6 Fatty acids, detergents, surfactants, and other compounds may cause foaming
during the distillation when they are present in high concentrations and may make the endpoint
for the titrimetric determination difficult to detect. Refer to Sec. 6.7 for an extraction procedure
to eliminate this interference.
4.0 APPARATUS AND MATERIALS
4.1 Reflux distillation apparatus such as shown in Figure 1 or Figure 2. The boiling
flask should be of one liter size with inlet tube and provision for condenser. The gas scrubber
may be a 270-mL Fisher-Milligan scrubber (Fisher, Part No. 07-513) or equivalent. The reflux
apparatus may be a Wheaton 377160 distillation unit or equivalent.
4.2 Hot plate stirrer/heating mantle.
4.3 pH meter.
4.4 Amber light.
4.5 Vacuum source.
4.6 Refrigerator.
4.7 Erlenmeyer flask - 500 mL.
4.8 Kl starch paper.
4.9 Class A volumetric flasks -1000, 250, and 100 mL.
5.0 REAGENTS
5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is
intended that all reagents shall 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 sufficiently high purity
to permit its use without lessening the accuracy of the determination.
5.2 Reagent water. All references to water in this method refer to reagent water, as
defined in Chapter One.
5.3 Reagents for sample collection, preservation, and handling
5.3.1 Sodium arsenite (0.1N), NaAsO2. Dissolve 3.2 g of NaAsO2 in 250 mL
water.
5.3.2 Ascorbic acid, C6H8O6.
5.3.3 Sodium hydroxide solution (50%), NaOH. Commercially available.
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5.3.4 Acetic acid (1.6M) CH3COOH. Dilute one part of concentrated acetic acid
with 9 parts of water.
5.3.5 2,2,4-Trimethylpentane, C8H18.
5.3.6 Hexane, C6H14.
5.3.7 Chloroform, CHCI3.
5.4 Reagents for cyanides amenable to chlorination
5.4.1 Calcium hypochlorite solution (0.35M), Ca(OCI)2. Combine 5 g of calcium
hypochlorite and 100 ml of water. Shake before using.
5.4.2 Sodium hydroxide solution (1.25N), NaOH. Dissolve 50 g of NaOH in 1
liter of water.
5.4.3 Sodium arsenite (O.1N). See Sec. 5.3.1.
5.4.4 Potassium iodide starch paper.
5.5 Reagents for distillation
5.5.1 Sodium hydroxide (1.25N). See Sec. 5.4.2.
5.5.2 Bismuth nitrate (0.062M), Bi(NO)3 5H2O. Dissolve 30 g of Bi(NO)3
5H2O in 100 mL of water. While stirring, add 250 ml of glacial acetic acid, CH3COOH.
Stir until dissolved and dilute to 1 liter with water.
5.5.3 Sulfamic acid (0.4N), H2NSO3H. Dissolve 40 g of H2NSO3H in 1 liter of
water.
5.5.4 Sulfuric acid (18N), H2SO4. Slowly and carefully add 500 ml of
concentrated H2SO4 to 500 mL of water.
5.5.5 Magnesium chloride solution (2.5M), MgCI2ป 6H2O. Dissolve 510 g of
MgCI2 6H2O in 1 liter of water.
5.5.6 Lead acetate paper.
5.5.7 Stock potassium cyanide solutions -- Refer to Method 9014 for the
preparation of stock cyanide solutions and calibration standards.
6.0 SAMPLE COLLECTION, PRESERVATION AND HANDLING
6.1 Samples should be collected in plastic or glass containers. All containers must be
thoroughly cleaned and rinsed.
6.2 Oxidizing agents such as chlorine decompose most cyanides. To determine
whether oxidizing agents are present, test a drop of the sample with potassium iodide-starch
test paper. A blue color indicates the need for treatment. Add 0.1N sodium arsenite solution a
few mL at a time until a drop of sample produces no color on the indicator paper. Add an
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additional 5 mL of sodium arsenite solution for each liter of sample. Ascorbic acid can be used
as an alternative although it is not as effective as arsenite. Add a few crystals of ascorbic acid
at a time until a drop of sample produces no color on the indicator paper. Then add an
additional 0.6 g of ascorbic acid for each liter of sample volume.
6.3 Aqueous samples must be preserved by adding 50% sodium hydroxide until the pH
is greater than or equal to 12 at the time of collection.
6.4 Samples should be chilled to 4 ฐC.
6.5 When properly preserved, cyanide samples can be stored for up to 14 days prior to
sample preparation steps.
6.6 Solid and oily wastes may be extracted prior to analysis by Method 9013. It uses a
dilute NaOH solution (pH = 12) as the extractant. This yields extractable cyanide.
6.7 If fatty acids, detergents, and surfactants are a problem, they may be extracted
using the following procedure. Acidify the sample with acetic acid (1.6M) to pH 6.0 to 7.0.
CAUTION: This procedure can produce lethal HCN gas.
Extract with isooctane, hexane, or chloroform (preference in order named) with solvent volume
equal to 20% of the sample volume. One extraction is usually adequate to reduce the
compounds below the interference level. Avoid multiple extractions or a long contact time at
low pH in order to keep the loss of HCN at a minimum. When the extraction is completed,
immediately raise the pH of the sample to above 12 with 50% NaOH solution.
7.0 PROCEDURE
7.1 Pretreatment for cyanides amenable to chlorination
7.1.1 This test must be performed under amber light. K3[Fe-(CN)6] may
decompose under UV light and hence will test positive for cyanide amenable to
chlorination if exposed to fluorescent lighting or sunlight. Two identical sample aliquots
are required to determine cyanides amenable to chlorination.
7.1.2 To one 500 mL sample or to a sample diluted to 500 ml, add calcium
hypochlorite solution dropwise while agitating and maintaining the pH between 11 and 12
with 1.25N sodium hydroxide until an excess of chlorine is present as indicated by Kl-
starch paper turning blue. The sample will be subjected to alkaline chlorination by this
step.
CAUTION: The initial reaction product of alkaline chlorination is the very toxic gas
cyanogen chloride; therefore, it is necessary that this reaction be
performed in a hood.
7.1.3 Test for excess chlorine with Kl-starch paper and maintain this excess for
one hour with continuous agitation. A distinct blue color on the test paper indicates a
sufficient chlorine level. If necessary, add additional calcium hypochlorite solution.
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7.1.4 After one hour, add 1 ml_ portions of 0.1 N sodium arsenite until Kl-starch
paper shows no residual chlorine. Add 5 mL of excess sodium arsenite to ensure the
presence of excess reducing agent.
7.1.5 Analyze the total cyanide concentration of both the chlorinated and the
unchlorinated samples by Method 9014 or 9213. The difference between the total
cyanide concentration in the chlorinated and unchlorinated samples is equal to the
cyanide amenable to chlorination.
7.2 Distillation procedure
7.2.1 Place 500 mL of sample, or sample diluted to 500 ml in the one liter
boiling flask. Pipet 50 mL of 1.25N sodium hydroxide into the gas scrubber. If the
apparatus in Figure 1 is used, add water until the spiral is covered. Connect the boiling
flask, condenser, gas scrubber and vacuum trap.
7.2.2 Start a slow stream of air entering the boiling flask by adjusting the
vacuum source. Adjust the vacuum so that approximately two bubbles of air per second
enter the boiling flask through the air inlet tube.
7.2.3 If samples are known or suspected to contain sulfide, add 50 mL of
0.062M bismuth nitrate solution through the air inlet tube. Mix for three minutes. Use lead
acetate paper to check the sample for the presence of sulfide. A positive test is indicated
by a black color on the paper.
7.2.4 If samples are known or suspected to contain nitrate or nitrite, or if
bismuth nitrate was added to the sample, add 50 mL of 0.4N sulfamic acid solution
through the air inlet tube. Mix for three minutes.
NOTE: Excessive use of sulfamic acid could create method bias.
7.2.5 Slowly add 50 mL of 18N sulfuric acid through the air inlet tube. Rinse the
tube with water and allow the airflow to mix the flask contents for three minutes. Add 20
mL of 2.5M magnesium chloride through the air inlet and wash the inlet tube with a stream
of water.
7.2.6 Heat the solution to boiling. Reflux for one hour. Turn off heat and
continue the airflow for at least 15 minutes. After cooling the boiling flask, and closing the
vacuum source, disconnect the gas scrubber.
7.2.7 Transfer the solution from the scrubber into a 250-mL volumetric flask.
Rinse the scrubber into the volumetric flask. Dilute to volume with water.
7.2.8 Proceed to the cyanide determinative methods given in Methods 9014 or
9213. If the distillates are not analyzed immediately, they should be stored at 4 ฐC in
tightly sealed flasks.
8.0 QUALITY CONTROL
8.1 All quality control data should be maintained and available for easy reference or
inspection,
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8.2 Employ a minimum of one reagent blank per analytical batch or one in every 20
samples to determine if contamination or any memory effects are occurring.
8.3 Analyze check standards with every analytical batch of samples. If the standards
are not within 15% of the expected value, then the samples must be reanalyzed.
8.4 Run one replicate sample for every 20 samples. A replicate sample is a sample
brought through the entire sample preparation and analytical process. The CV of the replicates
should be 20% or less. If this criterion is not met, the samples should be reanalyzed.
8.5 Run one matrix spiked sample every 20 samples to check the efficiency of sample
distillation by adding cyanide from the working standard or intermediate standard to 500 ml of
sample to ensure a concentration of approximately 40 ug/L. The matrix spiked sample is
brought through the entire sample preparation and analytical process.
8.6 It is recommended that at least two standards (a high and a low) be distilled and
compared to similar values on the curve to ensure that the distillation technique is reliable. If
distilled standards do not agree within + 10% of the undistilled standards, the analyst should
find the cause of the apparent error before proceeding.
8.7 The method of standard additions shall be used for the analysis of all samples that
suffer from matrix interferences such as samples which contain sulfides.
9.0 METHOD PERFORMANCE
9.1 The titration procedure using silver nitrate is used for measuring concentrations of
cyanide exceeding 0.1 mg/L The colorimetric procedure is used for concentrations below 1
mg/L of cyanide and is sensitive to about 0.02 mg/L.
9.2 EPA Method 335.2 (sample distillation with titration) reports that in a single
laboratory using mixed industrial and domestic waste samples at concentrations of 0.06 to 0.62
mg/L CNT, the standard deviations for precision were ฑ 0.005 to ฑ 0.094, respectively. In a
single laboratory using mixed industrial and domestic waste samples at concentrations of 0.28
and 0.62 mg/L CN', recoveries (accuracy) were 85% and 102%, respectively.
9.3 In two additional studies using surface water, ground water, and landfill leachate
samples, the titration procedure was further evaluated. The concentration range used in these
studies was 0.5 to 10 mg/L cyanide. The detection limit was found to be 0.2 mg/L for both total
and amenable cyanide determinations. The precision (CV) was 6.9 and 2.6 for total cyanide
determinations and 18.6 and 9.1 for amenable cyanide determinations. The mean recoveries
were 94% and 98.9% for total cyanide, and 86.7% and 97.4% for amenable cyanide.
10.0 REFERENCES
1. 1985 Annual Book of ASTM Standards. Vol. 11.01; "Standard Specification for Reagent
Water"; ATSM: Philadelphia, PA, 1985,; D1193-77.
2. 1982 Annual Book ASTM Standards. Part 19; "Standard Test Methods for Cyanide in
Water"; ASTM: Philadelphia, PA, 1982; 2036-82.
3. Bark, L.S.; Higson, H.G. Talanta 1964, 2, 471-479.
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4. Britton, P.; Winter, J.; Kroner, R.C. "EPA Method Study 12, Cyanide in Water"; final report
to the U.S. Environmental Protection Agency. National Technical Information Service:
Springfield, VA, 1984; PB80-196674.
5. Casey, J.P.; Bright, J.W.; Helms, B.D. "Nitrosation Interference in Distillation Tests for
Cyanide"; Gulf Coast Waste Disposal Authority: Houston, Texas.
6. Egekeze, J.O.; Oehne, F.W. J. Anal. Toxicology 1979. 3, 119.
7. Elly, C.T. vL Water Pollution Control Federation 1968, 40, 848-856.
8. Fuller, W. Cyanide in the Environment: Van Zyl, D., Ed.; Proceedings of Symposium;
December, 1984.
9. Gottfried, G.J. "Precision, Accuracy, and MDL Statements for EPA Methods 9010, 9030,
9060, 7520, 7521,7550, 7551, 7910, and 7911"; final report to the U.S. Environmental
Protection Agency. Environmental Monitoring and Support Laboratory. Biospheric: Cincinnati,
OH, 1984.
10. Methods for Chemical Analysis of Water and Wastes: U.S. Environmental Protection
Agency. Office of Research and Development. Environmental Monitoring and Support
Laboratory. ORD Publication Offices of Center for Environmental Research Information:
Cincinnati, OH, 1983; EPA-600/4-79-020.
11. Rohrbouqh. W.G.: et al. Reagent Chemicals. American Chemical Society Specifications.
7th ed.; American Chemical Society: Washington, DC, 1986.
12. Standard Methods for the Examination of Water and Wastewater. 18th ed.; Greenberg,
A.E.; Clesceri, L.S.; Eaton, A.D.; Eds.; American Waterworks Association, Water Pollution
Control Federation, American Public Health Association: Washington, DC, 1992.
13. Umana, M.; Beach, J.; Sheldon, L. "Revisions to Method 9010"; final report to the U.S.
Environmental Protection Agency. Office of Solid Waste. Research Triangle Institute:
Research Triangle Park, NC, 1986.
14. Umana, M.; Sheldon, L. "Interim Report: Literature Review"; interim report to the U.S.
Environmental Protection Agency. Office of Solid Waste. Research Triangle Institute:
Research Triangle Park, NC, 1986.
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FIGURE 1.
APPARATUS FOR CYANIDE DISTILLATION
Cooling Water
'nlet Tube
Heater
Screw Clamp
To Low Vacuum Source
Gas Scrubber
Distilling Flask
O
9010C-8
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FIGURE 2.
APPARATUS FOR CYANIDE DISTILLATION
Connecting Tubing
Allihn Condenser
Air Inlet Tube
One-Liter
Boiling Flask
n
I I Gas Scrubber
Suction
9010C-9
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METHOD 901OC
TOTAL AND AMENABLE CYANIDE: DISTILLATION
7.1 Pretreat sample
to determine
cyanides amenable
to chlorination.
7.2.1 Place sample
in round bottom
flask; transfer
NaOH solution into
scrubber; construct
distillation
assembly.
7.2.2 Turn vacuum
on and adjust
bubble rate.
7.2.3 Do
samples contain
sulfide?
7.2.3 Add bismuth
nitrate solution to
boiling flask.
7.2.4 Add sulfamic
acid solution to
boiling flask.
7.2.4 Nitrate
or nitrite in
samples?
7.2.5 Add sulfuric
acid; rinse inlet
tube with water;
add magnesium
chloride; rinse
inlet tube with
water.
7.2.6 Boil
solution; reflux;
cool; close vacuum
source.
7.2.7 Transfer
solution to a
volumetric
flask.
7.2.8 Proceed to
appropriate
determinative
method.
9010C-10
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METHOD 9012B
TOTAL AND AMENABLE CYANIDE (AUTOMATED COLORIMETRIC.
WITH OFF-LINE DISTILLATION)
1.0 SCOPE AND APPLICAT'ON
1.1 This method is used to determine the concentration of inorganic cyanide (CAS
Registry Number 57-12-5) in wastes or leachate. This method detects inorganic cyanides that
are present as either soluble salts or complexes. It is used to determine values for both total
cyanide and cyanide amenable to chlorination. The "reactive" cyanide content of a waste is not
determined by this method. Refer to 40 CFR 261.23 for information on the characteristic of
reactivity.
2.0 SUMMARY OF METHOD
2.1 The cyanide, as hydrocyanic acid (HCN), is released from samples containing
cyanide by means of a reflux-distillation operation under acidic conditions and absorbed in a
scrubber containing sodium hydroxide solution. The cyanide ion in the absorbing solution is
then determined by automated UV colorimetry.
2.2 In the automated colorimetric measurement, the cyanide is converted to cyanogen
chloride (CNCI) by reaction with Chloramine-T at a pH less than 8 without hydrolyzing to the
cyanate. After the reaction is complete, color is formed on the addition of pyridine-barbituric
acid reagent. The concentration of NaOH must be the same in the standards, the scrubber
solutions, and any dilution of the original scrubber solution to obtain colors of comparable
intensity.
3.0 INTERFERENCES
3.1 Interferences are eliminated or reduced by using the distillation procedure.
Chlorine and sulfide are interferences in this method.
3.2 Oxidizing agents such as chlorine decompose most cyanides. Chlorine
interferences.can be removed by adding an excess of sodium arsenite to the waste prior to
preservation and storage of the sample to reduce the chlorine to chloride which does not
interfere.
3.3 Sulfide interference can be removed by adding an excess of bismuth nitrate to the
waste (to precipitate the sulfide) before distillation. Samples that contain hydrogen sulfide,
metal sulfides, or other compounds that may produce hydrogen sulfide during the distillation
should be treated by the addition of bismuth nitrate.
3.4 High results may be obtained for samples that contain nitrate and/or nitrite. During
the distillation, nitrate and nitrite will form nitrous acid, which will react with some organic
compounds to form oximes. These compounds once formed will decompose under test
conditions to generate HCN. The possibility of interference of nitrate and nitrite is eliminated by
pretreatment with sulfamic acid just before distillation. Nitrate and nitrite are interferences when
present at levels higher than 10 mg/L and in conjunction with certain organic compounds.
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3.5 Thiocyanate is reported to be an interference when present at very high levels.
Levels of 10 mg/L were not found to interfere in Method 9010.
3.6 Fatty acids, detergents, surfactants, and other compounds may cause foaming
during the distillation when they are present in large concentrations and will make the endpoint
of the titration difficult to detect. They may be extracted at pH 6-7.
4.0 APPARATUS AND MATERIALS
4.1 Reflux distillation apparatus such as shown in Figure 1 or Figure 2. The boiling
flask should be of one liter size with inlet tube and provision for condenser. The gas scrubber
may be a 270-mL Fisher-Milligan scrubber (Fisher, Part No. 07-513 or equivalent). The reflux
apparatus may be a Wheaton 377160 distillation unit or equivalent.
4.2 Automated continuous-flow analytical instrument with:
4.2.1 Sampler.
4.2.2 Manifold.
4.2.3 Proportioning pump.
4.2.4 Heating bath with distillation coil.
4.2.5 Distillation head.
4.2.6 Colorimeter equipped with a 15-mm flowcell and 570 nm filter.
4.2.7 Recorder.
4.3 Hot plate stirrer/heating mantle.
4.4 pH meter.
4.5 Amber light.
4.6 Vacuum source.
4.7 Refrigerator.
4.8 5 mL microburette.
4.9 7 Class A volumetric flasks - 100 and 250 mL.
4.10 Erlenmeyer flask - 500 mL.
5.0 REAGENTS
5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it
is intended that all reagents shall conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such specifications are available. Other
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grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
5.2 Reagent water. All references to water in this method refer to reagent water, as
defined in Chapter One.
5.3 Reagents for sample collection, preservation, and handling
5.3.1 Sodium arsenite (0.1N), NaAsO2. Dissolve 3.2 g of NaAsO2 in 250 mL
water.
5.3.2 Ascorbic acid, C6H8O6.
5.3.3 Sodium hydroxide solution (50%), NaOH. Commercially available.
5.3.4 Acetic acid (1.6M) CH3COOH. Dilute one part of concentrated acetic acid
with 9 parts of water.
5.3.5 2,2,4-Trimethylpentane, C8H18.
5.3.6 Hexane, C6H14.
5.3.7 Chloroform, CHCI3.
5.4 Reagents for cyanides amenable to chlorination
5.4.1 Calcium hypochlorite solution (0.35M), Ca(OCI)2. Combine 5 g of calcium
hypochlorite and 100 mL of water. Shake before using.
5.4.2 Sodium hydroxide solution (1.25N), NaOH. Dissolve 50 g of NaOH in 1
liter of water.
5.4.3 Sodium arsenite (O.1N). See Sec. 5.3.1.
5.4.4 Potassium iodide starch paper.
5.5 Reagents for distillation
5.5.1 Sodium hydroxide (1.25N). See Sec. 5.4.2.
5.5.2 Bismuth nitrate (0.062M), Bi(NO)3 5H2O. Dissolve 30 g of Bi(NO)3
5H2O in 100 ml of water. While stirring, add 250 ml of glacial acetic acid, CH3COOH.
Stir until dissolved and dilute to 1 liter with water.
5.5.3 Sulfamic acid (0.4N), H2NSO3H. Dissolve 40 g H2NSO3H in 1 liter of
water.
5.5.4 Sulfuric acid (18N), H2SO4. Slowly and carefully add 500 mL of
concentrated H2SO4 to 500 mL of water.
5.5.5 Magnesium chloride solution (2.5M), MgCI2ป 6H2O. Dissolve 510 g of
MgCI2 6H2O in 1 liter of water.
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5.5.6 Lead acetate paper.
5.6 Reagents for automated colorimetric determination
5.6.1 Pyridine-barbituric acid reagent Place 15 g of barbituric acid in a 250-
ml_ volumetric flask, add just enough reagent water to wash the sides of the flask, and wet
the barbituric acid. Add 75 ml_ of pyridine and mix. Add 15 mL of concentrated HCI, mix,
and cool to room temperature. Dilute to 250 mL with reagent water and mix. This reagent
is stable for approximately six months if stored in a cool, dark place.
5.6.2 Chloramine-T solution - Dissolve 2.0 g of white, water soluble
chloramine-T in 500 mL of reagent water and refrigerate until ready to use.
5.6.3 Sodium hydroxide, 1 N - Dissolve 40 g of NaOH in reagent water, and
dilute to 1 liter.
5.6.4 All working standards should contain 2 mL of 1 N NaOH (Sec. 5.6.3) per
100 mL
5.6.5 Dilution water and receptacle wash water (NaOH, 0.25 N) Dissolve
10.0 g of NaOH in 500 mL of reagent water. Dilute to 1 liter.
6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6.1 Samples should be collected in plastic or glass containers. All containers must be
thoroughly cleaned and rinsed.
6.2 Oxidizing agents such as chlorine decompose most cyanides. To determine
whether oxidizing agents are present, test a drop of the sample with potassium iodide-starch
test paper. A blue color indicates the need for treatment. Add 0.1N sodium arsenite solution a
few mL at a time until a drop of sample produces no color on the indicator paper. Add an
additional 5 mL of sodium arsenite solution for each liter of sample. Ascorbic acid can be used
as an alternative although it is not as effective as arsenite. Add a few crystals of ascorbic acid
at a time until a drop of sample produces no color on the indicator paper. Then add an
additional 0.6 g of ascorbic acid for each liter of sample volume.
6.3 Aqueous samples must be preserved by adding 50% sodium hydroxide until the
pH is greater than or equal to 12 at the time of collection.
6.4 Samples should be chilled to 4 ฐC.
6.5 When properly preserved, cyanide samples can be stored for up to 14 days prior
to sample preparation steps.
6.6 Solid and oily wastes may be extracted prior to analysis by Method 9013 (Cyanide
Extraction Procedure for Solids and Oils). It uses a dilute NaOH solution (pH = 12) as the
extractant. This yields extractable cyanide.
6.7 If fatty acids, detergents, and surfactants are a problem, they may be extracted
using the following procedure. Acidify the sample with acetic acid (1.6M) to pH 6.0 to 7.0.
CAUTION: This procedure can produce lethal HCN gas.
9012B-4 Revision 2
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Extract with isooctane, hexane, or chloroform (preference in order named) with solvent volume
equal to 20% of the sample volume. One extraction is usually adequate to reduce the
compounds below the interference level. Avoid multiple extractions or a long contact time at
low pH in order to keep the loss of HCN at a minimum. When the extraction is completed,
immediately raise the pH of the sample to above 12 with 50% NaOH solution.
7.0 PROCEDURE
7.1 Pretreatment for cyanides amenable to chlorination
7.1.1 This test must be performed under amber light. K3[Fe-(CN)6] may
decompose under UV light and hence will test positive for cyanide amenable to
chlorination if exposed to fluorescent lighting or sunlight. Two identical sample aliquots are
required to determine cyanides amenable to chlorination.
7.1.2 To one 500 mL sample or to a sample diluted to 500 ml, add calcium
hypochlorite solution dropwise while agitating and maintaining the pH between 11 and 12
with 1.25N sodium hydroxide until an excess of chlorine is present as indicated by Kl-
starch paper turning blue. The sample will be subjected to alkaline chlorination by this
step.
CAUTION: The initial reaction product of alkaline chlorination is the very toxic gas
cyanogen chloride; therefore, it is necessary that this reaction be
performed in a hood.
7.1.3 Test for excess chlorine with Kl-starch paper and maintain this excess for
one hour with continuous agitation. A distinct blue color on the test paper indicates a
sufficient chlorine level. If necessary, add additional calcium hypochlorite solution.
7.1.4 After one hour, add 1 ml portions of 0.1 N sodium arsenite until Kl-starch
paper shows no residual chlorine. Add 5 mL of excess sodium arsenite to ensure the
presence of excess reducing agent.
7.1.5 Test for total cyanide as described below in both the chlorinated and the
unchlorinated samples. The difference of total cyanide in the chlorinated and
unchlorinated samples is the cyanide amenable to chlorination.
7.1.6 If samples are known or suspected to contain sulfide, add 50 mL of
0.062M bismuth nitrate solution through the air inlet tube. Mix for three minutes. Use lead
acetate paper to check the sample for the presence of sulfide. A positive test is indicated
by a black color on the paper.
7.2 Distillation procedure
7.2.1 Place 500 mL of sample, or sample diluted to 500 mL in the one liter
boiling flask. Pipet 50 mL of 1.25N sodium hydroxide into the gas scrubber. If the
apparatus in Figure 1 is used, add water until the spiral is covered. Connect the boiling
flask, condenser, gas scrubber and vacuum trap.
7.2.2 Start a slow stream of air entering the boiling flask by adjusting the
vacuum source. Adjust the vacuum so that approximately two bubbles of air per second
enter the boiling flask through the air inlet tube.
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7.2.3 If samples are known or suspected to contain nitrate or nitrite, or if
bismuth nitrate was added to the sample, add 50 mL of 0.4N sulfamic acid solution
through the air inlet tube. Mix for three minutes.
NOTE: Excessive use of sulfamic acid could create method bias.
7.2.4 Slowly add 50 mL of 18N sulfuric acid through the air inlet tube. Rinse
the tube with water and allow the airflow to mix the flask contents for three minutes. Add
20 mL of 2.5M magnesium chloride through the air inlet and wash the inlet tube with a
stream of water.
7.2.5 Heat the solution to boiling. Reflux for one hour. Turn off heat and
continue the airflow for at least 15 min. After cooling the boiling flask, and closing the
vacuum source, disconnect the gas scrubber.
7.2.6 Transfer the solution from the scrubber into a 250-mL volumetric flask.
Rinse the scrubber into the volumetric flask. Dilute to volume with water.
7.3 Automated colorimetric determination
7.3.1 Set up the manifold in a hood or a well-ventilated area as shown in Figure
3.
7.3.2 Allow colorimeter and recorder to warm up for 30 min. Run a baseline
with all reagents, feeding reagent water through the sample line.
7.3.3 Place appropriate standards in the sampler in order of increasing
concentration. Complete loading of the sampler tray with unknown samples.
7.3.4 When the baseline becomes steady, begin the analysis.
7.4 Standard curve for samples without sulfide
7.4.1 Prepare a series of standards by pipetting suitable volumes of working
standard potassium cyanide solution into 250-mL volumetric flasks. To each flask, add 50
mL of 1.25N sodium hydroxide and dilute to 250 mL with water. Prepare using the
following table. The sodium hydroxide concentration will be 0.25N.
mL of Working Standard Solution Concentration
(1 mL=10ugCN-) (|jg CNVL)
0.0 Blank
1.0 40
2.0 80
5.0 200
10.0 400
15.0 600
20.0 800
7.4.2 After the standard solutions have been prepared according to the table
above, pipet 50 mL of each standard solution into a 100-mL volumetric flask and proceed
9012B-6 Revision 2
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to Sees. 7.3.2 and 7.3.3 to obtain absorbance values for the standard curve. The final
concentrations for the standard curve will be one half of the amounts in the above table
(final concentrations ranging from 20 to 400 ug/L).
7.4.3 It is recommended that at least two standards (a high and a low) be
distilled and compared to similar values on the curve to ensure that the distillation
technique is reliable. If distilled standards do not agree within ฑ 10% of the undistilled
standards, the analyst should find the cause of the apparent error before proceeding.
7.4.4 Prepare a standard curve ranging from 20 to 400 ug/L by plotting
absorbance of standard versus the cyanide concentration
7.5 Standard curve for samples with sulfide
7.5.1 It is imperative that all standards be distilled in the same manner as the
samples using the method of standard additions (for example, bismuth nitrate must also
be added to the standards). Standards distilled by this method will give a linear curve, at
low concentrations, but as the concentration increases, the recovery decreases. It is
recommended that at least five standards be distilled.
7.5.2 Prepare a series of standards similar in concentration to those mentioned
in Sec. 7.4.1 and analyze as in Sec. 7.3. Prepare a standard curve by plotting
absorbance of standard versus the cyanide concentration.
7.6 Calculation - Prepare a standard curve by plotting peak heights of standards
against their concentration values. Compute concentrations of samples by comparing sample
peak heights with the standard curve.
8.0 QUALITY CONTROL
8.1 Refer to Chapter One for specific quality control procedures.
8.2 Verify the calibration curve with an independent calibration check standard. If the
standards are not within 15% of the expected value, a new recalibration curve is required.
Verify the calibration curve with every sample batch by analyzing a mid-range standard.
8.3 Run one matrix spike sample for every 10 samples to check the efficiency of
sample distillation. A matrix spike should be prepared by adding cyanide from the working
standard or intermediate standard to 500 mL of sample to ensure a concentration of
approximately 40 ug/L. Both the matrix duplicate and matrix spike duplicate are brought
through the entire sample preparation and analytical process.
8.4 The method of standard additions shall be used for the analysis of all samples that
suffer from matrix interferences such as samples which contain sulfides.
9.0 METHOD PERFORMANCE
9.1 Precision and accuracy data are not available at this time.
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10.0 REFERENCES
1. Annual Book of ASTM Standards, Part 31, "Water," Standard D2036-75, Method B, p. 505
(1976).
2. Goulden, P.O., B.K. Afghan, and P. Brooksbank, Determination of Nanogram Quantities
of Simple and Complex Cyanides in Water, Anal. Chem., 44(11). pp. 1845-49 (1972).
3. Standard Methods for the Examination of Water and Wastewater, 14th ed., pp. 376 and
370, Method 413F and D (1975).
4. Technicon AutoAnalyzer II Methodology, Industrial Method No. 315-74 WCUV Digestion
and Distillation, Technicon Industrial Systems, Tarrytown, New York, 10591 (1974).
9012B-8 Revision 2
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FIGURE 1
APPARATUS FOR CYANIDE DISTILLATION
Connecting Tubing
Allihn Condenser
Air Inlet Tube
One-Liter
Boiling Flask
Suction
9012B-9
Revision 2
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FIGURE 2
CYANIDE DISTILLATION APPARATUS
Cooling Water
fnlet Tube
Heater -ป
Screw Clamp
4
a.
'X
To Low Vacuum Source
Gas Scrubber
Condenser
Distilling Flask
O
9012B-10
Revision 2
November 2004
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-------
METHOD 9012B
TOTAL AND AMENABLE CYANIDE (AUTOMATED COLORIMETRIC
WITH OFF-LINE DISTILLATION )
7.1 Pretreat to
determine
cyanides amenable
to chlorination.
7.1.6 Treat
sampla by
adding bismuth
nitrate solution.
7.2.1 Place sample
in flask; pipot
sodium hydroxide
into absorbing
tube.
7.2.2 Introduce
air stream into
boiling flask.
7.2.3 Add
sulfamic
acid solution
through air
inlet tube.
7.2.4 Add
rinse tube with
Type II water
add magnesium
chloride.
7.2.5 Boil
solution;
reflux; cool;
close off
vacuum source.
7.2.6 Drain
solution
from absorber
into flask.
7.3 Perform
baseline
colorimetric
analysis.
9012B-12
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METHOD 9012B (continued)
7.5.1 Distill
standards in
same manner
as sample.
7.4
Does
sample
contain
sulfide?
7.5.2 Prepare
standard curve
of absorbance.
7.4.1 Prepare a
series of
CN standards.
7.4.2 Pipet
50 mL of each
standard into
flasks and obtain
absorbances.
7.4.4 Distill at
least two
standards to check
distillation
techniques.
7.6 Compute
concentrations.
9012B-13
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METHOD 9060A
TOTAL ORGANIC CARBON
1.0 SCOPE AND APPLICATION
1.1 This method is used to determine the concentration of organic carbon in ground
water, surface and saline waters, and domestic and industrial wastes. Some restrictions are
noted in Sees. 2.0 and 3.0.
1.2 This method is most applicable to measurement of organic carbon above 1 mg/L.
2.0 SUMMARY OF METHOD
2.1 Organic carbon is measured using a carbonaceous analyzer. This instrument
converts the organic carbon in a sample to carbon dioxide (CO2) by either catalytic combustion
or wet chemical oxidation. The CO2 formed is then either measured directly by an infrared
detector or converted to methane (CH4) and measured by a flame ionization detector. The
amount of CO2 or CH4 in a sample is directly proportional to the concentration of carbonaceous
material in the sample.
2.2 Carbonaceous analyzers are capable of measuring all forms of carbon in a
sample. However, because of various properties of carbon-containing compounds in liquid
samples, the manner of preliminary sample treatment as well as the instrument settings will
determine which forms of carbon are actually measured. The forms of carbon that can be
measured by this method are:
1. Soluble, nonvolatile organic carbon: e.g., natural sugars.
2. Soluble, volatile organic carbon: e.g., mercaptans, alkanes, low molecular weight
alcohols.
3. Insoluble, partially volatile carbon: e.g., low molecular weight oils.
4. Insoluble, particulate carbonaceous materials: e.g., cellulose fibers.
5. Soluble or insoluble carbonaceous materials adsorbed or entrapped on insoluble
inorganic suspended matter: e.g., oily matter adsorbed on silt particles.
2.3 Carbonate and bicarbonate are inorganic forms of carbon and must be separated
from the total organic carbon value. Depending on the instrument manufacturer's instructions,
this separation can be accomplished by either a simple mathematical subtraction, or by
removing the carbonate and bicarbonate by converting them to CO2 with degassing prior to
analysis.
3.0 INTERFERENCES
3.1 Carbonate and bicarbonate carbon represent an interference under the terms of
this test and must be removed or accounted for in the final calculation.
9060A -1 Revision 1
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3.2 This procedure is applicable only to homogeneous samples which can be injected
into the apparatus reproducibly by means of a microliter-type syringe or pipet. The openings of
the syringe or pipet limit the maximum size of particle which may be included in the sample.
3.3 Removal of carbonate and bicarbonate by acidification and purging with nitrogen,
or other inert gas, can result in the loss of volatile organic substances.
4,0 APPARATUS AND MATERIALS
4.1 Apparatus for blending or homogenizing samples - Generally, a Waring-type
blender is satisfactory.
4.2 Apparatus for total and dissolved organic carbon
4.2.1 Several companies manufacture analyzers for measuring carbonaceous
material in liquid samples. The most appropriate system should be selected based on
consideration of the types of samples to be analyzed, the expected concentration range,
and the forms of carbon to be measured.
4.2.2 No specific analyzer is recommended as superior. If the technique of
chemical oxidation is used, the laboratory must be certain that the instrument is capable of
achieving good carbon recoveries in samples containing particulates.
5.0 REAGENTS
5.1 ASTM Type II water (ASTM D1193) - Water should be monitored for impurities,
and should be boiled and cooled to remove CO2.
5.2 Potassium hydrogen phthalate. stock solution. 1,000 mg/L carbon Dissolve
0.2128 g of potassium hydrogen phthalate (primary standard grade) in Type II water and dilute
to 100.0 ml.
NOTE: Sodium oxalate and acetic acid are not recommended as stock solutions.
5.3 Potassium hydrogen phthalate, standard solutions Prepare standard solutions
from the stock solution by dilution with Type II water.
5.4 Carbonate-bicarbonate, stock solution. 1,000 mg/L carbon - Weigh 0.3500 g of
sodium bicarbonate and 0.4418 g of sodium carbonate and transfer both to the same 100-mL
volumetric flask. Dissolve with Type II water.
5.5 Carbonate-bicarbonate, standard solution Prepare a series of standards similar
to Step 5.3.
NOTE: This standard is not required by some instruments.
5.6 Blank solution - Use the same Type II water as was used to prepare the standard
solutions.
9060A - 2 Revision 1
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6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6.1 Sampling and storage of samples in glass bottles is preferable. Sampling and
storage in plastic bottles such as conventional polyethylene and cubitainers is permissible if it is
established that the containers do not contribute contaminating organics to the samples.
NOTE: A brief study performed in the EPA Laboratory indicated that Type II water stored in
new, 1-qt cubitainers did not show any increase in organic carbon after 2 weeks'
exposure.
6.2 Because of the possibility of oxidation or bacterial decomposition of some
components of aqueous samples, the time between sample collection and the start of analysis
should be minimized. Also, samples should be kept cool (4 ฐC) and protected from sunlight
and atmospheric oxygen.
6.3 In instances where analysis cannot be performed within 2 hr from time of sampling,
the sample is acidified (pH z 2) with HCI or H2SO4.
7.0 PROCEDURE
7.1 Homogenize the sample in a blender.
NOTE: To avoid erroneously high results, inorganic carbon must be accounted for. The
preferred method is to measure total carbon and inorganic carbon and to obtain the
organic carbon by subtraction. If this is not possible, follow Steps 7.2 and 7.3 prior to
analysis; however, volatile organic carbon may be lost.
7.2 Lower the pH of the sample to 2.
7.3 Purge the sample with nitrogen for 10 min.
7.4 Follow instrument manufacturer's instructions for calibration, procedure, and
calculations.
7.5 For calibration of the instrument, a series of standards should be used that
encompasses the expected concentration range of the samples.
7.6 Quadruplicate analysis is required. Report both the average and the range.
8.0 QUALITY CONTROL
8.1 All quality control data should be maintained and available for easy reference or
inspection.
8.2 Employ a minimum of one blank per sample batch to determine if contamination or
any memory effects are occurring.
8.3 Verify calibration with an independently prepared check standard every 15 samples.
8.4 Run one spike duplicate sample for every 10 samples. A duplicate sample is a
sample brought through the whole sample preparation and analytical process.
9060A - 3 Revision 1
November 2004
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9.0 METHOD PERFORMANCE
9.1 Precision and accuracy data are available in Method 415.1 of Methods for Chemical
Analysis of Water and Wastes.
10.0 REFERENCES
1. Annual Book of ASTM Standards, Part 31, "Water," Standard D 2574-79, p. 469 (1976).
2. Standard Methods for the Examination of Water and Wastewater, 14th ed., p. 532,
Method 505 (1975).
9060A - 4 Revision 1
November 2004
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Method 9060A
TOTAL ORGANIC CARBON
7.1 Homogenize
the sample in
a blender.
7.2 Lower the
sample pH.
7.4 Follow
manufacturer's
instructions for
calibration procedure,
and calculations
using carbonaceous
analyzer.
7.5 Use series of
standards for
calibration.
7.3 Purge the
sample with
nitrogen.
7.6 Quadruplicate
analysis.
9060A - 5
Revision 1
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METHOD 9070A
n-HEXANE EXTRACTABLE MATERIAL (HEM) FOR AQUEOUS SAMPLES
See Method 1664, Revision A, Publication No. EPA-821-R-98-002, for this method
procedure.
The full text of EPA Method 1664, Revision A, may be viewed or downloaded from the
Internet at: http://www.epa.qov/ost/methods/1664fQ51 .html.
You may also obtain copies of Method 1664, Revision A, through the U.S. EPA National
Service Center for Environmental Publications (NSCEP), 11029 Kenwood Road, Cincinnati, OH
45242.
Revision 1
9070A - 1 November 2004
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METHOD 9071B
n-HEXANE EXTRACTABLE MATERIAL (HEM) FOR SLUDGE. SEDIMENT. AND SOLID SAMPLES
1.0 SCOPE AND APPLICATION
1.1 Method 9071 may be used to quantify low concentrations of oil and grease in soil,
sediments, sludges, and other solid materials amenable to chemical drying and solvent extraction
with n-hexane. "Oil and grease" is a conventional pollutant under 40 CFR 401.16 and generally
refers to substances, including biological lipids and mineral hydrocarbons, that have similar physical
characteristics and common solubility in an organic extracting solvent. As such, oil and grease is
an operationally defined parameter, and the results will depend entirely on the extracting solvent and
method of extraction. Method 9071 employs n-hexane as the extraction solvent with Soxhlet
extraction and the results of this method are appropriately termed "n-hexane extractable material
(HEM)." Section 1.2 lists the type of materials that may be extracted by this method. In the context
of this method, "HEM" is used throughout this method and for operational purposes, may be
considered synonymous with "oil and grease" within the limitations discussed below.
1.2 Specifically, Method 9071 is suitable for extracting relatively non-volatile hydrocarbons,
vegetable oils, animal fats, waxes, soaps, greases, biological lipids, and related materials.
1.3 Method 9071 is not recommended for measuring materials that volatilize at
temperatures below 85ฐC. Petroleum fuels from gasoline through #2 fuel oil may be partially lost
during the solvent removal process.
1.4 Some crude oils and heavy fuel oils may contain materials that are not soluble in
n-hexane, and recovery of these materials may be low.
2.0 SUMMARY OF METHOD
2.1 A representative portion of wet (as received) waste is acidified with concentrated HCI
and chemically dried with magnesium sulfate or sodium sulfate. Magnesium sulfate monohydrate
is used to dry acidified sludges as it will combine with 75% of its own weight in water in forming
MgSO4 7H2O. Anhydrous sodium sulfate is used to dry soil and sediment samples.
2.2 After drying, the HEM is extracted with n-hexane using a Soxhlet apparatus. The
n-hexane extract is then distilled from the extract and the HEM is desiccated and weighed.
2.3 When necessary, a separate sample portion is evaluated for percent solids, and the
dry weight fraction may be used to calculate the dry-weight HEM concentration of the soil, sediment,
or waste.
3.0 DEFINITIONS
3.1 n-Hexane extractable material (HEM, oil and grease): Material that is extracted from
a sample using n-hexane and determined by this method. This material includes relatively non-
volatile hydrocarbons, vegetable oils, animal fats, waxes, soaps, greases, and related matter.
3.2 Refer to Chapter One for additional definitions.
9071B-1 Revision 2
April 1998
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4.0 INTERFERENCES
4.1 This method is entirely empirical, and duplicate results having a high degree of
precision can be obtained only by strict adherence to all details. The rate of cycling and time of
extraction in the Soxhlet apparatus must be consistent and length of time required for drying and
cooling extracted materials must be the same in order to generate consistent results. It is important
that the procedures be performed as directed due to the varying solubilities of the different greases
and heavy mineral oils.
4.2 Solvents, reagents, glassware, and other sample-processing hardware may yield
artifacts that could affect the results. All solvents and reagents used in the analysis should be
demonstrated to be free from interferences by processing a method blank with each analytical batch.
Specific selection of reagents, solvent washes, or purification of solvents may be required. Use of
plastic measuring devices, and/or plastic tubing attachments must be avoided.
4.3 Glassware should be cleaned by washing with hot tap water with detergent, rinsing with
tap water and reagent water, and rinsing with solvent. Glassware may also be baked at 200-250ฐC
for 1 hour. Boiling flasks that are used to contain the extracted residues may be dried in an oven
at 105-115ฐC and stored in a desiccator until used. Depending on the project DQOs, strict
adherence to the washing and handling procedures cited above may not be necessary as long as
the laboratory can demonstrate that alternative cleaning procedures yield acceptable method
performance and meet method blank acceptance criteria.
4.4 A gradual increase in weight may result due to the absorption of oxygen; a gradual loss
of weight may result due to volatilization. Extracted residues should be maintained in a desiccator
during cooling and prior to weighing. Extracted residues should be weighed as soon as possible
after cooling.
4.5 The presence of non-oily extractable substance such as sulfur compounds, organic
dyes, and chlorophyll, may result in a positive bias. For the purpose of this method, all materials
extracted and retained during this procedure are defined as HEM.
5.0 SAFETY
5.1 The toxicity or carcinogenicity of each reagent used in this method has not been
precisely determined; however, each chemical should be treated as a potential health hazard.
Exposure to these chemicals should be reduced to the lowest possible level. It is suggested that the
laboratory perform personal hygiene monitoring of each analyst that uses this method. This
monitoring should be performed using Occupational Safety and Health Administration (OSHA) or
National Institute of Occupational Safety and Health (NIOSH) approved personal hygiene monitoring
methods. Results of this monitoring should be made available to the analyst.
5.2 n-Hexane has been shown to have increased neurotoxic effects over other hexanes
and some other solvents. OSHA has proposed a time-weighted average (TWA) of 50 parts-per-
million (ppm); NIOSH concurs that an 8-hour TWA/permissible exposure limit (PEL) of 50 ppm is
appropriate for n-hexane; and the American Conference of Governmental Industrial Hygienists
(ACGIH) has published a threshold limit value (TLV) of 50 ppm for n-hexane. Inhalation of n-hexane
should be minimized by performing all operations with n-hexane in a explosion-proof hood or well-
ventilated area.
9071B-2 Revision 2
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5.3 n-Hexane has a flash point of-23ฐC (-9T), has explosive limits in air in the range of
1 to 7 percent, and poses a serious fire risk when heated or exposed to flame. n-Hexane can react
vigorously with oxidizing materials. The laboratory should include procedures in its operations that
address the safe handling of n-hexane.
5.4 Unknown samples may contain high concentrations of volatile toxic compounds.
Sample containers should be opened in a hood and handled with gloves to prevent exposure.
5.5 This method does not address all safety issues associated with its use. The laboratory
is responsible for maintaining a safe work environment and a current awareness file of OSHA
regulations regarding the safe handling of the chemicals specified in this method. A reference file
of material safety data sheets (MSDSs) should be available to all personnel involved in these
analyses.
6.0 EQUIPMENT AND SUPPLIES
6.1 Soxhlet extraction apparatus.
6.2 Heating mantle - explosion-proof, with temperature control.
6.3 Boiling flask - 125-mL or appropriate size.
6.4 Analytical balance - capable of weighing 0.1 mg.
6.5 Vacuum pump, or other vacuum source.
6.6 Paper extraction thimble for Soxhlet apparatus.
6.7 Glass wool or small glass beads to fill thimble.
6.8 Grease-free, non-absorbent cotton - To remove possible interferences, each batch of
cotton should be washed with n-hexane. Solvent washing may not be necessary if the laboratory
can demonstrate that the unwashed cotton does not affect the performance of the method or that
the concentration of HEM in the sample is so high that low contaminant concentration is
insignificant.
6.9 Beakers - 100- 150-mL
6.10 pH paper.
6.11 Porcelain mortar and pestle.
6.12 Extraction flask - 150-mL or appropriate size.
6.13 Waterbath or steam bath-explosion-proof - capable of maintaining a temperature of at
least 85ฐC.
6.14 Distilling apparatus - For removing n-hexane from extract.
6.14.1 Distilling head-Claisen (VWR Scientific No 26339-005, or equivalent), includes
Claisen-type connecting tube and condenser.
9071B-3 Revision 2
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6.14.2 Distillation adapter (used to attach distilling head and to the waste collection
flask for recovery of solvent).
6.14.3 Distillate collection flask (attached to the distilling adaptor for collection of the
distilled solvent).
6.14.4 Ice bath or recirculating chiller (to aid in the condensation and collection of
the distilled solvent).
6.15 Desiccator - Cabinet or jar type, capable of holding boiling flasks during cooling and
storage.
6.16 Tongs - for handling the boiling flasks.
6.17 Glass fiber filter paper - Whatman No. 40 or equivalent.
6.18 Boiling chips - Silicon carbide or fluoropolymer.
7.0 REAGENTS
7.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is
intended that all reagents shall 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 sufficiently high purity to permit its
use without lessening the accuracy of the determination.
7.2 Reagent water. All references to water in this method refer to reagent water, as defined
in Chapter One.
7.3 Concentrated hydrochloric acid (HCI).
7.4 Magnesium sulfate monohydrate. Prepare MgSO4 H2O by spreading a thin layer in
a dish and drying in an oven at 150ฐC overnight. Store in a tightly sealed glass container until used.
7.5 Sodium sulfate, granular, anhydrous (Na2SO4). Purify by heating at 400ฐC for 4 hours
in a shallow tray, or by precleaning the sodium sulfate with methylene chloride. If the sodium sulfate
is predeaned with methylene chloride, a method blank must be analyzed, demonstrating that there
is no interference from the sodium sulfate. Store in a tightly sealed glass container until used.
7.6 n-Hexane. Purity of 85%, 99.0% minimum saturated C6 isomers, residue less than 1
mg/L Boiling point, 69ฐC.
7.7 Hexadecane(CH3(CH2)14CH3)/stearic acid (CH3(CH2)16COOH). 1:1 spiking solution.
Prepare in acetone at a concentration of 2 mg/mL each.
Weigh 200 ฑ 2 mg of stearic acid and 200 ฑ 2 mg hexadecane into a 100 ml volumetric flask
and fill to the mark with acetone. The total concentration of this stock is 4000 mg/L (ppm) HEM. This
standard may be used for spiking samples and preparing laboratory control samples. Store in a
glass container with a fluoropolymer-lined cap at room temperature. Shield from light.
Note: The spiking solution may require warming for complete dissolution of stearic acid.
9071B-4 Revision 2
April 1998
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8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE
8.1 A minimum of 100 grams of sample should be collected using a metal spatula, spoon,
or equivalent device. Samples should be collected into a pre-cleaned wide-mouth glass container
fitted with a TFE-lined screw cap.
8.2 When practical (i.e., when the sample matrix allows the complete mixing of sample and
acid such as with a pourable sludge or sediment), the sample should be preserved to a pH < 2 by
adding 1 mL of concentrated HCI per 100 gram of sample and cooled to 4 ฑ 2 ฐC. If acidification is
not practical (as with a dry soil), the addition of the HCI is not required and the sample should be
cooled to 4 ฑ 2 ฐC. The laboratory must be notified so that the sample can be acidified prior to
analysis.
8.3 A holding time has not been established for HEM in solids, but it is recommended that
the sample be analyzed as soon as possible.
9.0 QUALITY CONTROL
9.1 Each laboratory that uses this method is required to operate a formal quality control
program. The minimum requirements of this program consist of an initial demonstration of laboratory
capability and the analysis of spiked samples as a continuing check on performance. The laboratory
is required to maintain performance records to define the quality of data that is generated.
9.2 Employ a minimum of one method blank per analytical batch or twenty samples,
whichever is more frequent, to verify that all reagents, solvents, and equipment are contamination
free. Prepare the method blank from 5 g of inert matrix such as pre-cleaned sand or similar material,
and carry it through the analytical process.
9.3 Run one matrix duplicate and matrix spike sample every twenty samples or analytical
batch, whichever is more frequent. Matrix duplicates and spikes are brought through the whole
sample preparation and analytical process.
9.4 The performance of the method should be evaluated by the use of a Laboratory Control
Sample (LCS). The LCS is prepared by spiking an inert matrix (as pre-cleaned sand or similar
material) with an appropriate volume of spiking solution (Sec. 7.7) and carrying it through the
analytical process.
10.0 CALIBRATION AND STANDARDIZATION
10.1 Calibrate the analytical balance at 2 mg and 1000 mg using class "S" weights.
10.2 Calibration shall be within ฑ 10% (i.e., ฑ 0.2 mg) at 2 mg and ฑ 0.5 % (i.e., ฑ 5 mg) at
1000 mg. If values are not within these limits, recalibrate the balance.
9071B - 5 Revision 2
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11.0 PROCEDURE
11.1 Determination of Sample Dry Weight Fraction
11.1.1 When it is necessary to report the HEM on a dry weight basis, determine the
dry weight fraction using a separate aliquot of sample, as discussed below. The aliquot used
for this determination cannot be used to evaluate HEM.
11.1.2 Weigh 5-10 gram (ฑ 0.01 gram) of the sample into pre-weighed crucible.
Determine the weight of the wet sample by subtracting the weight of the crucible.
11.1.3 Place the crucible with the wet sample in an oven overnight at 105ฐC.
Remove crucible from oven and place in a desiccator to cool. Weigh. Determine dry weight
of sample by subtracting the weight of the crucible. Determine the dry weight fraction of the
sample as follows:
NOTE: The drying oven should be contained in a hood or vented. Significant
laboratory contamination may result from a heavily contaminated hazardous
waste sample.
. . .. , .. g of dry sample
dry weight fraction =
g of sample
11.2 Sample Preparation
11.2.1 Sludge/Waste Samples
11.2.1.1 Weigh out 20 ฑ 0.5 grams of wet sample into a 150-mL beaker.
11.2.1.2 If the sample has not been acidified, acidify to a pH <. 2 with
approximately 0.3 mL concentrated HCI.
11.2.1.3 Add 25 grams Mg2SO4 - H2O (Sec. 7.4) and stir to a smooth
paste.
11.2.1.4 Spread paste on sides of beaker to facilitate evaporation. Let
stand about 15-30 min or until material is solidified.
11.2.1.5 Remove solids and grind to fine powder in a mortar.
11.2.1.6 Add the powder to the paper extraction thimble.
11.2.1.7 Wipe beaker and mortar with pieces of filter paper moistened with
n-hexane and add to thimble.
11.2.1.8 Fill thimble with glass wool (or glass beads).
9071B-6 Revision 2
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11.2.2 Sediment/Soil Samples
11.2.2.1 Decant and discard any water layer on a sediment sample. Mix
sample thoroughly, especially composited samples. Discard any foreign objects such
as sticks, leaves, and rocks.
11.2.2.2 Blend 10 grams of the sample with 10 grams of anhydrous sodium
sulfate (Sec. 7.5) as described in Section 11.2.1. Transfer homogenized paste to an
extraction thimble and cover with glass wool or glass beads. The extraction thimble
must drain freely for the duration of the extraction period.
11.3 Extraction
11.3.1 Set-up the Soxhlet apparatus containing the extraction thimble and sample
and attach a 125-mL boiling flask containing 90 ml of n-hexane. Add boiling chips. Adjust the
heating control on the heating mantle so that a cycling rate of 20 cycles/h is obtained. Extract
for a period of 4 hrs.
11.3.2 Tare a clean 250-mL or appropriate sized boiling flask as follows:
11.3.2.1 Dry the flask in an oven at 105-115ฐC for a minimum of 2 h.
11.3.2.2 Remove from the oven and immediately transfer to a desiccator
to cool at room temperature.
11.3.2.3 When cool, remove from the desiccator with tongs and weigh
immediately on a calibrated balance.
11.3.3 At the end of the 4 h extraction period, filter the extract through grease-free
cotton, into the pre-weighed boiling flask (Sec. 11.3.2). Use gloves to avoid adding fingerprints
to the flask.
11.3.4 Rinse flask and cotton with n-hexane and add to the 250-mL boiling flask.
NOTE: If the extract is clear and no suspended particles are present, the filtration
step may be omitted.
11.3.5 Connect the boiling flask to the distilling head apparatus and distill the solvent
by immersing the lower half of the flask in a water bath or a steam bath. A heating mantle may
also be used. Adjust the temperature of the heating device to complete the distillation in less
than 30 minutes. Collect the solvent for reuse or appropriate disposal.
11.3.6 When the distillation is complete, remove the distilling head. Immediately
remove the flask from the heat source and wipe the outside to remove excess moisture and
fingerprints. To remove solvent vapor, sweep out the flask for 15 sec with air by inserting a
glass tube that is connected to a vacuum source.
11.3.7 Cool the boiling flask in a desiccator for 30 min and weigh. Determine the
gain in weight of the boiling flask by subtracting the weight of the boiling flask (Sec. 11.3.2)
from the final boiling flask weight.
9071B-7 Revision 2
April 1998
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12.0 DATA ANALYSIS AND CALCULATIONS
Calculate the concentration of HEM in the sample as follows:
.,,-.. , , .ป gam in weight of flask(mg) X 1000
HEM (mg/kg wet weight) = * . " \. .,
weight of wet solid (g)
NOTE: If it is necessary to report the results on a dry weight basis, divide the result
obtained above by the dry weight fraction calculated in Sec. 11.1.3. Report
the results as mg/kg HEM dry weight. If it is necessary to report the results
as a percentage of the wet or dry weight, divide the wet-weight concentration
or dry weight concentration by 10,000 and report the result as % HEM wet or
dry weight.
13.0 METHOD PERFORMANCE
In a preliminary study designed to find a suitable replacement for Freon-113, three EPA
contract laboratories evaluated a total of 28 solid samples derived from various industrial and
commercial processes for oil and grease. This study evaluated a total of six solvents, including n-
hexane, to determine which of the alternative solvents produced results most closely with that of
Freon-113. In this study, each waste was Soxhlet-extracted in triplicate using Freon-113 and each
of the alternative solvents. Based on the overall results, n-hexane was judged to be the best
alternative solvent. The data provided in Table 1 compare the results for Freon-113 and n-hexane
for each waste. For a complete discussion of this study, refer to reference 1 in Section 16.0.
14.0 POLLUTION PREVENTION
14.1 Pollution prevention encompasses any technique that reduces or eliminates the quantity
and/or toxicity of waste at the point of generation. Numerous opportunities for pollution prevention
exist in laboratory operation. The EPA has established a preferred hierarchy of environmental
management techniques that places pollution prevention as the management option of first choice.
Whenever feasible, laboratory personnel should use pollution prevention techniques to address their
waste generation. When wastes cannot be feasibly reduced at the source, the Agency recommends
recycling as the next best option.
14.2 For information about pollution prevention that may be applicable to laboratories and
research institutions consult Less is Better Laboratory Chemical management for Waste Reduction
available from the American Chemical Society's Department of Government Relations and Science
Policy, 1155 16th St., N.W. Washington, D.C. 20036, (202) 872-4477.
15.0 WASTE MANAGEMENT
The Environmental Protection Agency requires that laboratory waste management practices
be conducted consistent with all applicable Federal, state and local rules and regulations. The
Agency urges laboratories to protect the air, water, and land by minimizing and controlling all
releases from hoods and bench operations, complying with the letter and spirit of any sewer
9071B-8 Revision 2
April 1998
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discharge permits and regulations, and by complying with all solid and hazardous waste regulations,
particularly the hazardous waste identification rules and land disposal restrictions. For further
information on waste management, consult The Waste Management Manual for Laboratory
Personnel available from the American Chemical Society at the address listed in Sec. 14.2.
16.0 REFERENCES
1. Preliminary Report of EPA Efforts to Replace Freon for the Determination of Oil and Grease,
United States Environmental Protection Agency, Office of Water, EPA-821 -93-009. June 1993.
2. Method 1664, Revision A: n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel
Treated N-Hexane Extractable Material (SGT-HEM) by Extraction and Gravimetry.
17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATA
The pages to follow contain Table 1, and a flow diagram of the method procedure.
9071B-9 Revision 2
April 1998
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TABLE 1
SOXHLET EXTRACTION OF SOLIDS USING FREON-113 AND N-HEXANE
All concentrations in mg/kg
Facility/
Process
Paper Mill .
POTW
Leather
Tannery
POTW
Petroleum
Refinery
Industrial
Laundry
Fish Oil
Plant
Coke Plant
Wood
Preserving
Plant
Drilling Fluid
Supplier
Contam.
Soils
Poultry Plant
Rolling Mill
Mayonnaise
Plant
Seafood
Plant
Waste Stream
Dewatered
Sludge
Sewage
Sludge
Dewatered
Sludge
Digested
Sludge
API Separator
Sludge
DAF
Sludge
Oily
Sludge
Waste
Activated
Sludge
Solid
Waste
Used drilling
mud
Kerosene
Contaminated
Soil
Waste
Activated
Sludge
Dewatered
Scale
Oily Sludge
Waste Sludge
'
Solvent:
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Rep
No. 1
11000
6600
98000
110000
11000
21000
130000
54000
320000
240000
310000
290000
890000
440000
8300
14000
150000
140000
1300
1300
2000
2500
38000
5900
11000
14000
880000
590000
64000
34000
9071 B-
Rep
No. 2
5300
2400
81000
86000
12000
15000
97000
76000
350000
320000
310000
360000
1000000
530000
8000
19000
140000
130000
1600
1200
1400
3200
11000
11000
14000
14000
850000
780000
31000
10
Rep
No. 3
7900
11000
81000
80000
12000
19000
66000
48000
250000
240000
240000
180000
770000
460000
18000
15000
140000
130000
1300
1600
1900
2600
40000
46000
17000
16000
780000
520000
53000
27000
Mean
Concen-
tration
8000
6600
87000
91000
12000
18000
98000
59000
310000
270000
290000
280000
890000
480000
11000
16000
140000
130000
1400
1400
1700
2800
30000
21000
14000
15000
840000
630000
58000
31000
Standard
Deviation
2762
4203
9940
13281
732
3201
33028
14516
53257
43822
41717
90819
131249
46318
5505
2732
3512
6557
157
201
352
410
16263
21795
2884
983
50521
132020
7526
3867
Revision 2
April 1998
-------
TABLE 1
(CONTINUED)
Facility/
Process
Seafood
Plant
Poultry
Plant
Railroad
Yard
Can
Manufact
Plant
Soup Plant
Oily Water
Treatment
Plant
Can
Manufact
Plant
Can
Manufact
Plant
Drum
Handling
Facility
Polymer
Plant
Restaurant
Leather
Tannery
Waste Stream
Oily Sludge
OAF Sludge
Oily Sludge
Filter Cake
DAF Sludge
Oily Sludge
Oily Sludge
Filter Cake
Oily Sludge
Dewatered
Sludge
Vegetable Oil
Waste
Waste Sludge
Solvent:
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Source: Reference 1
Rep
No. 1
400000
400000
670000
530000
870000
850000
62000
69000
600000
580000
76000
77000
94000
80000
290000
290000
1200000
990000
13000
8400
760000
1100000
180000
240000
9071 B-
Rep
No. 2
410000
390000
600000
530000
920000
840000
62000
64000
590000
520000
75000
60000
88000
90000
290000
290000
1100000
1000000
12000
6900
610000
980000
220000
270000
11
Rep
No. 3
430000
390000
570000
530000
870000
830000
60000
66000
610000
600000
70000
79000
94000
83000
300000
290000
1200000
980000
8200
9100
780000
980000
190000
210000
Mean
Concen-
tration
410000
400000
610000
530000
890000
840000
61000
66000
600000
570000
74000
72000
92000
85000
290000
290000
1200000
1000000
11000
8100
720000
1000000
190000
240000
Standard
Deviation
16371
7095
49549
2449
27906
6884
976
2615
10066
40361
3215
10713
3291
4992
6217
2029
57735
27319
2524
1122
92060
80064
22140
31177
Revision 2
April 1998
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METHOD 9071B
n-HEXANE EXTRACTABLE MATERIAL (HEM) FOR SLUDGE. SEDIMENT. AND SOLID SAMPLES
Start
J)
11.1 Determine
dry weight fraction
of sample.
11.2.1.1 Weigh
a sample of
wet sludge
and place in
beaker.
11.2.1.2
Acidify to
11.2 Is
sample
sludge or
sediment/
soil?
11.2.2.1 Decant
water; mix
sample; discard
foreign objects.
11.2.2.2 Blend
with sodium
sulfate; add
to extraction
thimble.
11.2.1.3 Add
magnesium sulfate
monohydrate and
stir.
11.2.1.5
Remove and
grind solids
to a fine
powder.
9071 B-12
Revision 2
April 1998
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METHOD 9071B
n-HEXANE EXTRACTABLE MATERIAL (HEIW FOR SLUDGE. SEDIMENT. AND SOLID SAMPLES
(Continued)
11.2.1.6 Add
powder to
paper
extraction
thimble.
11.2.1.7 Wipe
beaker and
mortar; add
to thimble.
11.2.1.8 Fill
thimble with
glass wool.
B
11.3.1 Extract
in Soxhlet
apparatus for
4 hours.
11.3.3 Filter
extract into
boiling flask.
11.3.4 Rinse
flask with
solvent.
11.3.5
Evaporate and
collect
solvent for
reuse.
11.3.6 Remove
solvent vapor.
11.3.7 Cool
and weigh
boiling flask.
12.0
Calculate
concentration
of HEM
Stop
9071 B-13
Revision 2
April 1998
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CHAPTER SIX
PROPERTIES
Prior to employing the methods in this chapter, analysts are advised to consult the
disclaimer statement at the front of this manual and the information in Chapter Two for guidance
on the allowed flexibility in the choice of apparatus, reagents, and supplies. Procedures for
required method-defined parameters are not subject to the same flexibility afforded in other SW-
846 methods. In addition, unless specified in a regulation, the use of SW-846 methods is not
mandatory in response to Federal testing requirements. The information contained in each
procedure is provided by EPA as guidance to be used by the analyst and the regulated community
in making judgements necessary to meet the data quality objectives or needs for the intended use
of the data.
The following methods are found in Chapter Six:
Method 1030:
Method 1120:
Method 1312:
Method 1320:
Method 1330A:
Method 9041A:
Method 90450:
Method 9050A:
Method 9080:
Method 9081:
Method 9090A:
Method 9095B:
Method 9096:
Appendix A:
Method 9100:
Method 9310:
Method 9315:
Ignitability of Solids
Dermal Corrosion
Synthetic Precipitation Leaching Procedure
Multiple Extraction Procedure
Extraction Procedure for Oily Wastes
pH Paper Method
Soil and Waste pH
Specific Conductance
Cation-Exchange Capacity of Soils (Ammonium Acetate)
Cation-Exchange Capacity of Soils (Sodium Acetate)
Compatibility Test for Wastes and Membrane Liners
Paint Filter Liquids Test
Liquid Release Test (LRT) Procedure
Liquid Release Test Pre-Test
Saturated Hydraulic Conductivity, Saturated Leachate
Conductivity, and Intrinsic Permeability
Gross Alpha and Gross Beta
Alpha-Emitting Radium Isotopes
SIX-1
Revision 4
November 2004
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METHOD 9045D
SOIL AND WASTE pH
1.0 SCOPE AND APPLICATION
1.1 This method is an electrometric procedure for measuring pH in soils and waste
samples. Wastes may be solids, sludges, or non-aqueous liquids. If water is present, it must
constitute less than 20% of the total volume of the sample.
2.0 SUMMARY OF METHOD
2.1 The sample is mixed with reagent water, and the pH of the resulting aqueous
solution is measured.
3.0 INTERFERENCES
3.1 Samples with very low or very high pH may give incorrect readings on the meter.
For samples with a true pH of >10, the measured pH may be incorrectly low. This error can be
minimized by using a low-sodium-error electrode. Strong acid solutions, with a true pH of <1,
may give incorrectly high pH measurements.
3.2 Temperature fluctuations will cause measurement errors.
3.3 Errors will occur when the electrodes become coated. If an electrode becomes
coated with an oily material that will not rinse free, the electrode can (1) be cleaned with an
ultrasonic bath, or (2) be washed with detergent, rinsed several times with water, placed in 1:10
HCI so that the lower third of the electrode is submerged, and then thoroughly rinsed with
water, or (3) be cleaned per the manufacturer's instructions.
4.0 APPARATUS AND MATERIALS
4.1 pH meter with means for temperature compensation.
4.2 Glass electrode.
4.3 Reference electrode A silver-silver chloride or other reference electrode of
constant potential may be used.
NOTE: Combination electrodes incorporating both measuring and referenced functions
are convenient to use and are available with solid, gel-type filling materials that
require minimal maintenance.
4.4 Beaker - 50-mL.
4.5 Thermometer and/or temperature sensor for automatic compensation.
4.6 Analytical balance capable of weighing 0.1 g.
9045 D -1 Revision 4
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5.0 REAGENTS
5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it
is intended that all reagents shall 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 sufficiently high purity
to permit its use without lessening the accuracy of the determination.
5.2 Reagent water. All references to water in this method refer to reagent water, as
defined in Chapter One.
5.3 Primary standard buffer salts are available from the National Institute of Standards
and Technology (NIST) and should be used in situations where extreme accuracy is necessary.
Preparation of reference solutions from these salts requires some special precautions and
handling, such as low-conductivity dilution water, drying ovens, and carbon-dioxide-free purge
gas. These solutions should be replaced at least once each month.
5.4 Secondary standard buffers may be prepared from NIST salts or purchased as
solutions from commercial vendors. These commercially available solutions, which have been
validated by comparison with NIST standards, are recommended for routine use.
6.0 SAMPLE PRESERVATION AND HANDLING
Samples should be analyzed as soon as possible.
7.0 PROCEDURE
7.1 Calibration
7.1.1 Because of the wide variety of pH meters and accessories, detailed
operating procedures cannot be incorporated into this method. Each analyst must be
acquainted with the operation of each system and familiar with all instrument functions.
Special attention to care of the electrodes is recommended.
7.1.2 Each instrument/electrode system must be calibrated at a minimum of
two points that bracket the expected pH of the samples and are approximately three pH
units or more apart. Repeat adjustments on successive portions of the two buffer
solutions until readings are within 0.05 pH units of the buffer solution value. If an
accurate pH reading based on the conventional pH scale [0 to 14 at 25 ฐC] is required,
the analyst should control sample temperature at 25 ฑ 1 ฐC when sample pH approaches
the alkaline end of the scale (e.g., a pH of 11 or above).
7.2 Sample preparation and pH measurement of soils:
7.2.1 To 20 g of soil in a 50-mL beaker, add 20 mL of reagent water, cover,
and continuously stir the suspension for 5 min. Additional dilutions are allowed if working
with hygroscopic soils and salts or other problematic matrices.
7.2.2 Let the soil suspension stand for about 1 hr to allow most of the
suspended clay to settle out from the suspension or filter or centrifuge off the aqueous
phase for pH measurement.
9045D - 2 Revision 4
November 2004
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7.2.3 Adjust the electrodes in the clamps of the electrode holder so that, upon
lowering the electrodes into the beaker, the glass electrode will be immersed just deep
enough into the clear supernatant solution to establish a good electrical contact through
the ground-glass joint or the fiber-capillary hole. Insert the electrodes into the sample
solution in this manner. For combination electrodes, immerse just below the suspension.
7.2.4 If the sample temperature differs by more than 2 ฐC from the buffer
solution, the measured pH values must be corrected.
7.2.5 Report the results as "soil pH measured in water at _ฐC" where "_ฐC" is
the temperature at which the test was conducted.
7.3 Sample preparation and pH measurement of waste materials
7.3.1 To 20 g of waste sample in a 50-mL beaker, add 20 mL of reagent water,
cover, and continuously stir the suspension for 5 min. Additional dilutions are allowed if
working with hygroscopic wastes and salts or other problematic matrices.
7.3.2 Let the waste suspension stand for about 15 min to allow most of the
suspended waste to settle out from the suspension or filter or centrifuge off aqueous
phase for pH measurement.
NOTE: If the waste is hygroscopic and absorbs all the reagent water, begin the
experiment again using 20 g of waste and 40 mL of reagent water.
NOTE: If the supernatant is multiphasic, decant the oily phase and measure the pH of
the aqueous phase. The electrode may need to be cleaned (Step 3.3) if it
becomes coated with an oily material.
7.3.3 Adjust the electrodes in the clamps of the electrode holder so that, upon
lowering the electrodes into the beaker, the glass electrode will be immersed just deep
enough into the clear supernatant to establish good electrical contact through the
ground-glass joint or the fiber-capillary hole. Insert the electrode into the sample solution
in this manner. For combination electrodes, immerse just below the suspension.
7.3.4 If the sample temperature differs by more than 2 ฐC from the buffer
solution, the measured pH values must be corrected.
7.3.5 Report the results as "waste pH measured in water at _ฐC" where "_ฐC"
is the temperature at which the test was conducted.
8.0 QUALITY CONTROL
8.1 Refer to Chapter One for the appropriate QC protocols.
8.2 Electrodes must be thoroughly rinsed between samples.
9.0 METHOD PERFORMANCE
9.1 No data provided.
9045D - 3 Revision 4
November 2004
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10.0 REFERENCES
1. Black, Charles Allen; Methods of Soil Analysis: American Society of Agronomy:
Madison, Wl, 1973.
2. National Bureau of Standards, Standard Reference Material Catalog, 1986-87, Special
Publication 260.
9045D - 4 Revision 4
November 2004
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METHOD 9045D
SOIL AND WASTE pH
7.1 Calibrate
each instrument/
electrodo
system.
7.2.1 Add 20 mL
water to 20 g soil;
stir continuously
for 5 minutes.
7.3.1 Add 2O mL
water to 20 g waste;
atir continuously
for 5 minutes.
7.2.2 Let soil
suspension
stand for 1
hour or filter.
7.3.2 Let waste
suspension
stand for 15
minutes or filter.
Is waste N. Yes
hydroscopic?
No / supernatant \ Yes
multiphasic?
Repeal experiment
with 20 g waste
and 40 mL water.
Decant oily
phase;
measure pH of
aqueous phase.
Aqueous
Phase
9045D - 5
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METHOD 9095B
PAINT FILTER LIQUIDS TEST
1.0 SCOPE AND APPLICATION
1.1 This method is used to determine the presence of free liquids in a representative
sample of waste.
1.2 The method is used to determine compliance with 40 CFR 264.314 and 265.314.
2.0 SUMMARY OF METHOD
2.1 A predetermined amount of material is placed in a paint filter. If any portion of the
material passes through and drops from the filter within the 5-min test period, the material is
deemed to contain free liquids.
3.0 INTERFERENCES
3.1 Filter media were observed to separate from the filter cone on exposure to alkaline
materials. This development causes no problem if the sample is not disturbed.
3.2 Temperature can affect the test results if the test is performed below the freezing
point of any liquid in the sample. Tests must be performed above the freezing point and can,
but are not required to, exceed room temperature of 25 ฐC.
4.0 APPARATUS AND MATERIALS
4.1 Conical paint filter - Mesh number 60 +/- 5% (fine meshed size). Available at local
paint stores such as Sherwin-Williams and Glidden.
4.2 Glass funnel - If the paint filter, with the waste, cannot sustain its weight on the
ring stand, then a fluted glass funnel or glass funnel with a mouth large enough to allow at least
1 in. of the filter mesh to protrude should be used to support the filter. The funnel should be
fluted or have a large open mouth in order to support the paint filter yet not interfere with the
movement, to the graduated cylinder, of the liquid that passes through the filter mesh.
4.3 Ring stand and ring, or tripod.
4.4 Graduated cylinder or beaker - 100-mL.
5.0 REAGENTS
5.1 None.
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6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
A 100-mL or 100-g representative sample is required for the test. If it is not possible to
obtain a sample of 100 mL or 100 g that is sufficiently representative of the waste, the analyst
may use larger size samples in multiples of 100 mL or 100 g, i.e., 200, 300, 400 mL or g.
However, when larger samples are used, analysts shall divide the sample into 100-mL or 100-g
portions and test each portion separately. If any portion contains free liquids, the entire sample
is considered to have free liquids. If the sample is measured volumetrically, then it should lack
major air spaces or voids.
7.0 PROCEDURE
7.1 Assemble test apparatus as shown in Figure 1.
7.2 Place sample in the filter. A funnel may be used to provide support for the paint
filter. If the sample is of such light bulk density that it overflows the filter, then the sides of the
filter can be extended upward by taping filter paper to the inside of the filter and above the
mesh. Settling the sample into the paint filter may be facilitated by lightly tapping the side of the
filter as it is being filled.
7.3 In order to assure uniformity and standardization of the test, material such as
sorbent pads or pillows which do not conform to the shape of the paint filter should be cut into
small pieces and poured into the filter. Sample size reduction may be accomplished by cutting
the sorbent material with scissors, shears, a knife, or other such device so as to preserve as
much of the original integrity of the sorbent fabric as possible. Sorbents enclosed in a fabric
should be mixed with the resultant fabric pieces. The particles to be tested should be reduced
smaller than 1 cm (i.e., should be capable of passing through a 9.5 mm (0.375 inch) standard
sieve). Grinding sorbent materials should be avoided as this may destroy the integrity of the
sorbent and produce many "fine particles" which would normally not be present.
7.4 For brittle materials larger than 1 cm that do not conform to the filter, light crushing
to reduce oversize particles is acceptable if it is not practical to cut the material. Materials such
as clay, silica gel, and some polymers may fall into this category.
7.5 Allow sample to drain for 5 min into the graduated cylinder.
7.6 If any portion of the test material collects in the graduated cylinder in the 5-min
period, then the material is deemed to contain free liquids for purposes of 40 CFR 264.314 and
265.314.
8.0 QUALITY CONTROL
8.1 Duplicate samples should be analyzed on a routine basis.
9.0 METHOD PERFORMANCE
9.1 No data provided.
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10.0 REFERENCES
10.1 None provided.
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FIGURE 1
PAINT FILTER TEST APPARATUS
* FUNNEL
RING STAND
/PAINT FILTER
^-GRADUATED CYLINDER
9095B - 4
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METHOD 9095B
PAINT FILTER LIQUIDS TEST
7.1 Assemble
test apparatus.
7.2 Place sample
in filter.
7.3 Allow sample
to drain into
graduated cylinder.
7.4 Did
any test
material collect
in graduated
cylinder?
7.4 Material is
deemed to contain
free liquids; see 40
CFR 264.314 or
265.314.
Stop
9095B- 5
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CHAPTER SEVEN
CHARACTERISTICS INTRODUCTION AND REGULATORY DEFINITIONS
This chapter addresses procedures for required "method-defined parameters," where the
analytical result is wholly dependant on the process used to make the measurement. Examples
include the use of the toxicity characteristic leaching procedure (TCLP) to prepare a leachate, and
the flash point, pH, paint filter liquids, and corrosivity tests. In these instances, changes to the
specific methods may change the end result and incorrectly identify a waste as nonhazardous.
Therefore, when the measurement of such method-defined parameters is required by regulation,
those methods are not subject to the flexibility afforded in other SW-846 methods (such as
described in the Disclaimer and Chapter Two of this manual).
7.1 IGNITABILITY
7.1.1 Introduction
The objective of the ignitability characteristic is to identify wastes that either present fire
hazards under routine storage, disposal, and transportation or are capable of severely
exacerbating a fire once started.
7.1.2 Regulatory Definition
See 40 CFR 261.21 for the regulatory definition of the hazardous waste characteristic of
ignitability. Methods 1010 and 1020 of Chapter Eight refer the reader to the ASTM standards
required by the RCRA regulations for the flash point of liquids at 40 CFR 261.21 (1).
7.2 CORROSIVITY
7.2.1 Introduction
The corrosivity characteristic, as defined in 40 CFR 261.22, is designed to identify wastes
that might pose a hazard to human health or the environment due to their ability to:
1. Mobilize toxic metals if discharged into a landfill environment;
2. Corrode handling, storage, transportation, and management equipment; or
3. Destroy human or animal tissue in the event of inadvertent contact.
In order to identify such potentially hazardous materials, EPA has selected two properties
upon which to base the definition of a corrosive waste. These properties are pH and corrosivity
toward Type SAE 1020 steel.
The procedures for measuring pH of aqueous wastes are detailed in Method 9040,
Chapter Six. Method 1110, Chapter Eight, describes how to determine whether a waste is
corrosive to steel. Use Method 9095, Paint Filter Liquids Test, Chapter Six, to determine free
liquid.
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7.2.2 Regulatory Definition
See 40 CFR 261.22 for the regulatory definition of the hazardous waste characteristic of
corrosivity.
7.3 REACTIVITY
7.3.1 Introduction
The regulation in 40 CFR 261.23 defines reactive wastes to include wastes that have any
of the following properties: (1) readily undergo violent chemical change; (2) react violently or form
potentially explosive mixtures with water; (3) generate toxic fumes when mixed with water or, in the
case of cyanide- or sulfide-bearing wastes, when exposed to mild acidic or basic conditions; (4)
explode when subjected to a strong initiating force; (5) explode at normal temperatures and
pressures; or (6) fit within the Department of Transportation's forbidden explosives, Class A
explosives, or Class B explosives classifications.
This definition is intended to identify wastes that, because of their extreme instability and
tendency to react violently or explode, pose a problem at all stages of the waste management
process. The Agency relies entirely on a descriptive, prose definition of reactivity because
available tests for measuring the variegated class of effects embraced by the reactivity definition
suffer from a number of deficiencies.
7.3.2 Regulatory Definition
See 40 CFR 261.24 for the regulatory definition of the hazardous waste characteristic of
reactivity.
7.4 TOXICITY CHARACTERISTIC LEACHING PROCEDURE
7.4.1 Introduction
The Toxicity Characteristic Leaching Procedure (TCLP) is designed to simulate the
leaching a waste will undergo if disposed of in a sanitary landfill. This test is designed to simulate
leaching that takes place in a sanitary landfill only. The extraction fluid employed is a function of
the alkalinity of the solid phase of the waste. A subsample of a waste is extracted with the
appropriate buffered acetic acid solution for 18 + 2 hours. The extract obtained from the TCLP
(the "TCLP extract") is then analyzed to determine if any of the thresholds established for the 40
Toxicity Characteristic (TC) constituents (listed in Table 7-1) have been exceeded or if the
treatment standards established for the constituents listed in 40 CFR 268.40 have been met under
the Land Disposal Restrictions (LDR) regulations. If the TCLP extract contains any one of the TC
constituents in an amount equal to or exceeding the concentrations specified in 40 CFR 261.24,
the waste possesses the characteristic of toxicity and is a hazardous waste. If the TCLP extract
contains constituents in an amount exceeding the concentrations specified in 40 CFR 268.40, the
treatment standard for that waste has not been met, and further treatment is necessary prior to
land disposal.
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7.4.2 Summary of Procedure
Figure 3 summarizes the procedures in the TCLP. The five basic steps of the TCLP are
summarized below.
1. Separation Procedure
For liquid wastes (i.e.. those containing less than 0.5% dry solid material), the waste, after
filtration through a 0.6 to 0.8 urn glass fiber filter, is defined as the TCLP extract.
For wastes containing greater than or equal to 0.5% solids, the liquid, if any, is separated
from the solid phase and stored for later analysis.
2. Particle Size Reduction
Prior to extraction, the solid material must pass through a 9.5-mm (0.375-in.) standard
sieve, have a surface area per gram of material equal to or greater than 3.1 cm2, or, be smaller
than 1 cm in its narrowest dimension. If the surface area is smaller or the particle size larger than
described above, the solid portion of the waste is prepared for extraction by crushing, cutting, or
grinding the waste to the surface area or particle size described above. (Special precautions must
be taken if the solids are prepared for organic volatiles extraction.)
3. Extraction of Solid Material
The solid material from Step 2 is extracted for 18 + 2 hours with an amount of extraction
fluid equal to 20 times the weight of the solid phase. The extraction fluid employed is a function of
the alkalinity of the solid phase of the waste. A special extractor vessel is used when testing for
volatile analytes.
4. Final Separation of the Extraction from the Remaining Solid
Following extraction, the liquid extract is separated from the solid phase by filtration
through a 0.6 to 0.8 urn glass fiber filter. If compatible, the initial liquid phase of the waste is
added to the liquid extract, and these are analyzed together. If incompatible, the liquids are
analyzed separately and the results are mathematically combined to yield a volume-weighted
average concentration.
5. Testing (Analysis) of TCLP Extract
Inorganic and organic species are identified and quantified using appropriate methods in
the 6000, 7000, and 8000 series of methods in this manual or by other appropriate methods.
7.4.3 Regulatory Definition
Under the Toxicity Characteristic, a solid waste exhibits the characteristic of toxicity if the
TCLP extract from a subsample of the waste contains any of the contaminants listed in Table 7-1
at a concentration greater than or equal to the respective value given in that table. If a waste
contains <0.5% filterable solids, the waste itself, after filtering, is considered to be the extract for
the purposes of analysis.
SEVEN - 3 Revision 4
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Under the Land Disposal Restrictions regulations (40 CFR, Part 268), a restricted waste
identified in 40 CFR 268.40 cannot be land disposed if a TCLP extract of the waste or a TCLP
extract of the treatment residue of the waste exceeds the values shown in the table of 40 CFR
268.40 for any hazardous constituent listed in the table for that waste. If a waste contains <0.5%
filterable solids, the waste itself, after filtering, is considered to be the extract for the purposes of
analysis.
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TABLE 7-1.
MAXIMUM CONCENTRATION OF CONTAMINANTS FOR TOXICITY CHARACTERISTIC
Contaminant
Arsenic
Barium
Benzene
Cadmium
Carbon tetrachloride
Chlordane
Chlorobenzene
Chloroform
Chromium
o-Cresol
m-Cresol
p-Cresol
Cresol
2,4-D
1 ,4-Dichlorobenzene
1 ,2-Dichloroethane
1,1-Dichloroethylene
2,4-Dinitrotoluene
Endrin
Heptachlor (and its hydroxide)
Hexachlorobenzene
Hexachloro-1 ,3-butadiene
Hexachloroethane
Lead
Lindane
Mercury
Methoxychlor
Methyl ethyl ketone
Nitrobenzene
Pentachlorophenol
Pyridine
Selenium
Silver
Tetrachloroethylene
Toxaphene
Trichloroethylene
2,4,5-Trichlorophenol
2,4,6-Trichlorophenol
2,4,5-TP (Silvex)
Vinyl chloride
Regulatory Level
(mg/L)
5.0
100.0
0.5
1.0
0.5
0.03
100.0
6.0
5.0
200.01
200.01
200.01
200.01
10.0
7.5
0.5
0.7
0.132
0.02
0.008
0.132
0.5
3.0
5.0
0.4
0.2
10.0
200.0
2.0
100.0
5.02
1.0
5.0
0.7
' 0.5
0.5
400.0
2.0
1.0
0.2
'If o-, m-, and p-cresol concentrations cannot be differentiated, the total cresol (0026) concentration is used. The
regulatory level of total cresol is 200 mg/L.
2Quantitation limit is greater than the calculated regulatory level. The quantitation limit therefore becomes the regulatory
level.
SEVEN - 5
Revision 4
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FIGURE 3.
TOXICITY CHARACTERISTIC LEACHING PROCEDURE FLOWCHART
appropriate fluid
1] Bolll* titractor
for non-volatila*
2) 2HE d*vicซ for
volatile*
SEVEN - 6
Revision 4
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FIGURE 3 (continued)
Oiacard
tolida
Solid
Svpai
atrac1
olid* ซ
0.8 urn
fib.r {
atซ
f roa
/ 0.6 -
glaas
ilt.r
HMIUCI asounl if
liquid and analyia
{thvaatically
coaibinc raault M/
rซ*ull of tract
I,
liquid
conpatibl
xith thซ
tract?
SEVEN - 7
Revision 4
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CHAPTER EIGHT
METHODS FOR DETERMINING CHARACTERISTICS
This chapter addresses procedures for required method-defined parameters, where the
analytical result is wholly dependant on the process used to make the measurement. Examples
include the use of the toxicity characteristic leaching procedure (TCLP) to prepare a leachate, and
the flash point, pH, paint filter liquids, and corrosivity tests. In these instances, changes to the
specific methods may change the end result and incorrectly identify a waste as nonhazardous.
Therefore, when the measurement of such method-defined parameters is required by regulation,
those methods are not subject to the flexibility afforded in other SW-846 methods (such as
described in the Disclaimer and Chapter Two of this manual).
Methods for determining the characteristics of ignitability for liquids, corrosivity for liquids,
and toxicity are included. The text of the methods identified for the characteristic of ignitability
refer the reader to the appropriate required ASTM methods. There are no required SW-846
methods for the analysis of the characteristic of reactivity.
EIGHT - 1 Revision 3
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8.1 Ignitability
This chapter addresses procedures for required method-defined parameters, where the
analytical result is wholly dependant on the process used to make the measurement. Examples
include the use of the toxicity characteristic leaching procedure (TCLP) to prepare a leachate, and
the flash point, pH, paint filter liquids, and corrosivity tests. In these instances, changes to the
specific methods may change the end result and incorrectly identify a waste as nonhazardous.
Therefore, when the measurement of such method-defined parameters is required by regulation,
those methods are not subject to the flexibility afforded in other SW-846 methods (such as
described in the Disclaimer and Chapter Two of this manual).
The text of the methods identified for the characteristic of ignitability refer the reader to the
appropriate required ASTM methods. The following methods are found in Sec. 8.1 of this chapter:
Method 1010A: Test Methods for Flash Point by Pensky-Martens Closed Cup
Tester
Method 1020B : Standard Test Methods for Flash Point by Setaflash (Small Scale)
Closed-cup Apparatus
EIGHT - 2 Revision 3
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METHOD 1010A
TEST METHODS FOR FLASH POINT BY PENSKY-MARTENS CLOSED CUP TESTER
See American Society for Testing Materials (ASTM) Standard D 93-79 or Standard D 93-80
for these method procedures used in the characterization of flash point of liquids. These
standards are two of three required method options for determination of the ignitability
characteristic in liquid wastes, see 40 CFR 261.21 (a)(1). Currently, these ASTM standards can
be obtained from Global Engineering Documents, 15 Iverness Way East, Englewood, CO 80112,
1-800-854-7179, http://qlobal.ihs.com. At the web site, do a search for "ASTM D 93" (document
number) and at the document search results select "view historical revisions." Select the Revision
79 or 80 version.
1010A-1 Revision 1
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METHOD 1020B
STANDARD TEST METHODS FOR FLASH POINT BY SETAFLASH (SMALL SCALE)
CLOSED-CUP APPARATUS
See American Society for Testing Materials (ASTM) Standard D 3278-78 for these method
procedures used in the characterization of the flash point of liquids. This standard is one of three
required method options for determination of the ignitability characteristic in liquid wastes, see 40
CFR 261.21(a)(1). Currently, this ASTM standard can be obtained from Global Engineering
Documents, 15 Iverness Way East, Englewood, CO 80112, 1-800-854-7179,
http://qlobal.ihs.com. At the web site, do a search for "ASTM D 3278" (document number) and at
the document search results select "view historical revisions." Select the Revision 78 version.
1020B-1 Revision 2
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8.2 Corrosivity
This chapter addresses procedures for required method-defined parameters, where the
analytical result is wholly dependant on the process used to make the measurement. Examples
include the use of the toxicity characteristic leaching procedure (TCLP) to prepare a leachate, and
the flash point, pH, paint filter liquids, and corrosivity tests. In these instances, changes to the
specific methods may change the end result and incorrectly identify a waste as nonhazardous.
Therefore, when the measurement of such method-defined parameters is required by regulation,
those methods are not subject to the flexibility afforded in other SW-846 methods (such as
described in the Disclaimer and Chapter Two of this manual).
The following methods are found in Sec. 8.2 of this chapter:
Method 9040C: pH Electrometric Measurement
Method 111OA: Corrosivity Toward Steel
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METHOD 9040C
pH ELECTROMETRIC MEASUREMENT
1.0 SCOPE AND APPLICATION
1.1 This method is used to measure the pH of aqueous wastes and those multiphase
wastes where the aqueous phase constitutes at least 20% of the total volume of the waste.
1.2 The corrosivity of concentrated acids and bases, or of concentrated acids and
bases mixed with inert substances, cannot be measured. The pH measurement requires some
water content.
2.0 SUMMARY
2.1 The pH of the sample is determined electrometrically using either a glass electrode
in combination with a reference potential or a combination electrode. The measuring device is
calibrated using a series of standard solutions of known pH.
3.0 INTERFERENCES
3.1 The glass electrode, in general, is not subject to solution interferences from color,
turbidity, colloidal matter, oxidants, reductants, or moderate (<0.1 molar solution) salinity.
3.2 Sodium error at pH levels >10 can be reduced or eliminated by using a low-
sodium-error electrode.
3.3 Coatings of oily material or particulate matter can impair electrode response.
These coatings can usually be removed by gentle wiping or detergent washing, followed by
rinsing with distilled water. An additional treatment with hydrochloric acid (1:10) may be
necessary to remove any remaining film.
3.4 Temperature effects on the electrometric determination of pH arise from two
sources. The first is caused by the change in electrode output at various temperatures. This
interference should be controlled with instruments having temperature compensation or by
calibrating the electrode-instrument system at the temperature of the samples. The second
source of temperature effects is the change of pH due to changes in the sample as the
temperature changes. This error is sample-dependent and cannot be controlled. It should,
therefore, be noted by reporting both the pH and temperature at the time of analysis.
4.0 APPARATUS AND MATERIALS
4.1 pH meter -- Laboratory or field model. Many instruments are commercially
available with various specifications and optional equipment.
4.2 Glass electrode.
4.3 Reference electrode - A silver-silver chloride or other reference electrode of
constant potential may be used.
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NOTE: Combination electrodes incorporating both measuring and referenced functions are
convenient to use and are available with solid, gel-type filling materials that require
minimal maintenance.
4.4 Magnetic stirrer and Teflon-coated stirring bar.
4.5 Thermometer and/or temperature sensor for automatic compensation.
5.0 REAGENTS
5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is
intended that all reagents shall 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 sufficiently high purity
to permit its use without lessening the accuracy of the determination.
5.2 Primary standard buffer salts are available from the National Institute of Standards
and Technology (NIST) and should be used in situations where extreme accuracy is necessary.
Preparation of reference solutions from these salts requires some special precautions and
handling, such as low-conductivity dilution water, drying ovens, and carbon-dioxide-free purge
gas. These solutions should be replaced at least once each month.
5.3 Secondary standard buffers may be prepared from NIST salts or purchased as
solutions from commercial vendors. These commercially available solutions have been
validated by comparison with NIST standards and are recommended for routine use.
6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
Samples should be analyzed as soon as possible.
7.0 PROCEDURE
7.1 Calibration
7.1.1 Because of the wide variety of pH meters and accessories, detailed
operating procedures cannot be incorporated into this method. Each analyst must be
acquainted with the operation of each system and familiar with all instrument functions.
Special attention to care of the electrodes is recommended.
7.1.2 Each instrument/electrode system must be calibrated at a minimum of
two points that bracket the expected pH of the samples and are approximately three pH
units or more apart. (For corrosivity characterization, the calibration of the pH meter
should include a buffer of pH 2 for acidic wastes and a pH 12 buffer for caustic wastes;
also, for corrosivity characterization, the sample must be measured at 25 ฑ 1 ฐC if the pH
of the waste is above 12.0.) Various instrument designs may involve use of a dial (to
"balance" or "standardize") or a slope adjustment, as outlined in the manufacturer's
instructions. Repeat adjustments on successive portions of the two buffer solutions until
readings are within 0.05 pH units of the buffer solution value.
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7.2 Place the sample or buffer solution in a clean glass beaker using a sufficient
volume to cover the sensing elements of the electrodes and to give adequate clearance for the
magnetic stirring bar. If field measurements are being made, the electrodes may be immersed
directly into the sample stream to an adequate depth and moved in a manner to ensure
sufficient sample movement across the electrode-sensing element as indicated by drift-free
readings (<0.1 pH).
7.3 If the sample temperature differs by more than 2 ฐC from the buffer solution, the
measured pH values must be corrected. Instruments are equipped with automatic or manual
compensators that electronically adjust for temperature differences. Refer to manufacturer's
instructions.
7.4 Thoroughly rinse and gently wipe the electrodes prior to measuring pH of samples.
Immerse the electrodes into the sample beaker or sample stream and gently stir at a constant
rate to provide homogeneity and suspension of solids. Note and record sample pH and
temperature. Repeat measurement on successive aliquots of sample until values differ by <
0.1 pH units. Two or three volume changes are usually sufficient.
8.0 QUALITY CONTROL
8.1 Refer to Chapter One for the appropriate QC protocols.
8.2 Electrodes must be thoroughly rinsed between samples.
9.0 METHOD PERFORMANCE
9.1 Forty-four analysts in twenty laboratories analyzed six synthetic water samples
containing exact increments of hydrogen-hydroxyl ions, with the following results:
pH Units
3.5
3.5
7.1
7.2
8.0
8.0
Standard Deviation
pH Units
0.10
0.11
0.20
0.18
0.13
0.12
Accuracy as
Bias
%
-0.29
-0.00
+1.01
-0.03
-0.12
+0.16
Bias
pH Units
-0.01
+0.07
-0.002
-0.01
+0.01
9040C - 3
Revision 3
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10.0 REFERENCES
1. National Bureau of Standards, Standard Reference Material Catalog 1986-87, Special
Publication 260.
9040C - 4 Revision 3
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METHOD 9040C
pH ELECTROMETRIC MEASUREMENT
f Start )
>
r
7.1 Calibrate pH
meter.
>
f
7.2 Place sample
or buffer solution
in glass beaker.
7.3 Does
temperature
differ by more
than 2C from
buffer?
7.3 Correct
measured pH
values.
7.4 Immerce
electrodes and
measure pH of
sample.
7.4 Note and record
pH and temperature:
repeat 2 or 3 times
with different
aliquots.
f Stop J
9040C - 5
Revision 3
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METHOD 1110A
CORROSIVITY TOWARD STEEL
1.0 SCOPE AND APPLICATION
1.1 This method measures the corrosivity toward steel of both aqueous and
nonaqueous liquid wastes.
2.0 SUMMARY OF METHOD
2.1 This test exposes coupons of SAE Type 1020 steel to the liquid waste to be
evaluated and, by measuring the degree to which the coupon has been dissolved, determines
the corrosivity of the waste.
3.0 INTERFERENCES
3.1 In laboratory tests, such as this one, corrosion of duplicate coupons is usually
reproducible to within 10%. However, large differences in corrosion rates may occasionally
occur under conditions where the metal surfaces become passivated. Therefore, at least
duplicate determinations of corrosion rate should be made.
4.0 APPARATUS AND MATERIALS
4.1 An apparatus should be used, consisting of a kettle or flask of suitable size
(usually 500 to 5,000 mL), a reflux condenser, a thermowell and temperature regulating device,
a heating device (mantle, hot plate, or bath), and a specimen support system. A typical resin
flask set up for this type of test is shown in Figure 1.
4.2 The supporting device and container shall be constructed of materials that are not
affected by, or cause contamination of, the waste under test.
4.3 The method of supporting the coupons will vary with the apparatus used for
conducting the test, but it should be designed to insulate the coupons from each other
physically and electrically and to insulate the coupons from any metallic container or other
device used in the test. Some common support materials include glass, fluorocarbon, or
coated metal.
4.4 The shape and form of the coupon support should ensure free contact with the
waste.
4.5 A circular specimen of SAE 1020 steel of about 3.75 cm (1.5 in.) diameter is a
convenient shape for a coupon. With a thickness of approximately 0.32 cm (0.125 in.) and a
0.80-cm (0.4-in.)-diameter hole for mounting, these specimens will readily pass through a 45/50
ground-glass joint of a distillation kettle. The total surface area of a circular specimen is given
by the following equation:
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A =' " + (0(3.14)(D) + (0(3.14)(d)
where:
t = thickness.
D = diameter of the specimen.
d = diameter of the mounting hole.
If the hole is completely covered by the mounting support, the last term in the equation,
(t)(3.14)(d), is omitted.
4.5.1 All coupons should be measured carefully to permit accurate calculation
of the exposed areas. An area calculation accurate to ฑ 1% is usually adequate.
4.5.2 More uniform results may be expected if a substantial layer of metal is
removed from the coupons prior to testing the corrosivity of the waste. This can be
accomplished by chemical treatment (pickling), by electrolytic removal, or by grinding with
a coarse abrasive. At least 0.254 mm (0.0001 in.) or 2-3 mg/cm2 should be removed.
Final surface treatment should include finishing with #120 abrasive paper or cloth. Final
cleaning consists of scrubbing with bleach-free scouring powder, followed by rinsing in
distilled water and then in acetone or methanol, and finally by air-drying. After final
cleaning, the coupon should be stored in a desiccator until used.
4.5.3 The minimum ratio of volume of waste to area of the metal coupon to be
used in this test is 40 ml_/cm2.
5.0 REAGENTS
5.1 Sodium hydroxide (NaOH). 20%: Dissolve 200 g NaOH in 800 ml Type II water
and mix well.
5.2 Zinc dust.
5.3 Hydrochloric acid (HCI): Concentrated.
5.4 Stannous chloride (SnCI2).
5.5 Antimony chloride (SbCI3).
6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
This method does not provide sample collection, preservation, and handling guidelines.
7.0 PROCEDURE
7.1 Assemble the test apparatus as described in Sec. 4.0, above.
1110A-2 Revision 1
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7.2 Fill the container with the appropriate amount of waste.
7.3 Begin agitation at a rate sufficient to ensure that the liquid is kept well mixed and
homogeneous.
7.4 Using the heating device, bring the temperature of the waste to 55 ฐC (130 ฐF).
7.5 An accurate rate of corrosion is not required; only a determination as to whether
the rate of corrosion is less than or greater than 6.35 mm per year is required. A 24-hr test
period should be ample to determine whether or not the rate of corrosion is > 6.35 mm per year.
7.6 In order to determine accurately the amount of material lost to corrosion, the
coupons have to be cleaned after immersion and prior to weighing. The cleaning procedure
should remove all products of corrosion while removing a minimum of sound metal. Cleaning
methods can be divided into three general categories: mechanical, chemical, and electrolytic.
7.6.1 Mechanical cleaning includes scrubbing, scraping, brushing, and
ultrasonic procedures. Scrubbing with a bristle brush and mild abrasive is the most
popular of these methods. The others are used in cases of heavy corrosion as a first step
in removing heavily encrusted corrosion products prior to scrubbing. Care should be
taken to avoid removing sound metal.
7.6.2 Chemical cleaning implies the removal of material from the surface of the
coupon by dissolution in an appropriate solvent. Solvents such as acetone,
dichloromethane, and alcohol are used to remove oil, grease, or resinous materials and
are used prior to immersion to remove the products of corrosion. Solutions suitable for
removing corrosion from the steel coupon are:
Solution
20% NaOH + 200 g/L zinc dust
Cone. HCI + 50 g/L SnCI2 + 20 g/L SbCI3
SoakingJ'ime
5min
Until clean
Temperature
Boiling
Cold
7.6.3 Electrolytic cleaning should be preceded by scrubbing to remove loosely
adhering corrosion products. One method of electrolytic cleaning that can be employed
uses:
Solution:
Anode:
Cathode:
50 g/L H2SO4
Carbon or lead
Steel coupon
Cathode current density: 20 amp/cm2 (129 amp/in.2)
Inhibitor: 2 cc organic inhibitor/liter
Temperature: 74 ฐC (165 ฐF)
Exposure Period: 3 min.
1110A-3
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NOTE: Precautions must be taken to ensure good electrical contact with the coupon to
avoid contamination of the cleaning solution with easily reducible metal ions and to
ensure that inhibitor decomposition has not occurred. Instead of a proprietary
inhibitor, 0.5 g/L of either diorthotolyl thiourea or quinolin ethiodide can be used.
7.7 Whatever treatment is employed to clean the coupons, its effect in removing
sound metal should be determined by using a blank (i.e., a coupon that has not been exposed
to the waste). The blank should be cleaned along with the test coupon and its waste loss
subtracted from that calculated for the test coupons.
7.8 After corroded specimens have been cleaned and dried, they are reweighed. The
weight loss is employed as the principal measure of corrosion. Use of weight loss as a
measure of corrosion requires making the assumption that all weight loss has been due to
generalized corrosion and not localized pitting. In order to determine the corrosion rate for the
purpose of this regulation, the following formula is used:
i
Corrosion Rate (mmpy) = (weight loss x 87.60)/(area x time x metal density) (Reference 1),
then,
Corrosion Rate (mmpy) = weight loss x 11.145
area x time
where: weight loss is in milligrams,
area is in square centimeters,
time is in hours,
metal density of SAE type 1020 steel = 7.86 g/cm3, and
corrosion rate is in millimeters per year (mmpy).
8.0 QUALITY CONTROL
8.1 All quality control data should be filed and available for auditing.
8.2 Duplicate samples should be analyzed on a routine basis.
9.0 METHOD PERFORMANCE
9.1 No data provided.
10.0 REFERENCES
1. National Association of Corrosion Engineers, "Laboratory Corrosion Testing of Metals for
the Process Industries," NACE Standard TM 01 69 (1972 Revision), NACE, 3400 West Loop
South, Houston, TX 77027.
1110A-4 Revision 1
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Figure 1. Typical resin flask that can be used as a versatile and convenient apparatus to
conduct simple immersion tests. Configuration of the flask top is such that more sophisticated
apparatus can be added as required by the specific test being conducted. A = thermowell, B =
resin flask, C = specimens hung on supporting device, D = heating mantle, E = liquid interface,
F = opening in flask for additional apparatus that may be required, and G = reflux condenser.
1110A-5
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METHOD 1110
CORROSIVITY TOWARD STEEL
7.1 Assemble
test apparatus.
7.6 Clean coupons
by mechanical,
chemical, and/or
electrolytic
methods.
7.2 Fill container
with waste.
7.7 Check effect
of cleaning
treatment on
removing sound
metal.
7.3 Agitate.
I
7.8 Determine
corrosion rate.
7.4 Heat.
1110A-6
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8.3 Toxicity
This chapter addresses procedures for required method-defined parameters, where the
analytical result is wholly dependant on the process used to make the measurement. Examples
include the use of the toxicity characteristic leaching procedure (TCLP) to prepare a leachate, and
the flash point, pH, paint filter liquids, and corrosivity tests. In these instances, changes to the
specific methods may change the end result and incorrectly identify a waste as nonhazardous.
Therefore, when the measurement of such method-defined parameters is required by regulation,
those methods are not subject to the flexibility afforded in other SW-846 methods (such as
described in the Disclaimer and Chapter Two of this manual).
The following methods are found in Sec. 8.3 of this chapter:
Method 131 OB: Extraction Procedure (EP) Toxicity Test Method and
Structural Integrity Test
Method 1311: Toxicity Characteristic Leaching Procedure
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METHOD 131 OB
EXTRACTION PROCEDURE (EP) TOXICITYTEST METHOD
AND STRUCTURAL INTEGRITY TEST
1.0 SCOPE AND APPLICATION
1.1 This method is used to determine whether a waste exhibits the characteristic of
Extraction Procedure Toxicity.
1.2 The procedure may also be used to simulate the leaching which a waste may
undergo if disposed of in a sanitary landfill. Method 1310 is applicable to liquid, solid, and
multiphase samples.
2.0 SUMMARY OF METHOD
2.1 If a representative sample of the waste contains > 0.5% solids, the solid phase of the
sample is ground to pass a 9.5 mm sieve and extracted with deionized water which is maintained
at a pH of 5 ฑ 0.2, with acetic acid. Wastes that contain < 0.5% filterable solids are, after filtering,
considered to be the EP extract for this method. Monolithic wastes which can be formed into a
cylinder 3.3 cm (dia) x 7.1 cm, or from which such a cylinder can be formed which is
representative of the waste, may be evaluated using the structural integrity procedure instead of
being ground to pass a 9.5-mm sieve.
3.0 INTERFERENCES
3.1 Potential interferences that may be encountered during analysis are discussed in the
individual analytical methods.
4.0 APPARATUS AND MATERIALS
4.1 Extractor - For purposes of this test, an acceptable extractor is one that will impart
sufficient agitation to the mixture to (1) prevent stratification of the sample and extraction fluid and
(2) ensure that all sample surfaces are continuously brought into contact with well-mixed
extraction fluid. Examples of suitable extractors are shown in Figures 1 through 3 of this method
and are available from: Associated Designs & Manufacturing Co., Alexandria, Virginia; Glas-Col
Apparatus Co., Terre Haute, Indiana; Millipore, Bedford, Massachusetts; and Rexnard,
Milwaukee, Wisconsin.
4.2 pH meter or pH controller - Accurate to 0.05 pH units with temperature
compensation.
4.3 Filter holder - Capable of supporting a 0.45-um filter membrane and of withstanding
the pressure needed to accomplish separation. Suitable filter holders range from simple vacuum
units to relatively complex systems that can exert up to 5.3 kg/cm3 (75 psi) of pressure. The type
1310B-1 Revision 2
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of filter holder used depends upon the properties of the mixture to be filtered. Filter holders known
to EPA and deemed suitable for use are listed in Table 1.
4.4 Filter membrane - Filter membrane suitable for conducting the required filtration shall
be fabricated from a material that (1) is not physically changed by the waste material to be filtered
and (2) does not absorb or leach the chemical species for which a waste's EP extract will be
analyzed. Table 2 lists filter media known to the Agency to be suitable for solid waste testing.
4.4.1 In cases of doubt about physical effects on the filter, contact the filter
manufacturer to determine if the membrane or the prefilter is adversely affected by the
particular waste. If no information is available, submerge the filter in the waste's liquid
phase. A filter that undergoes visible physical change after 48 hours (i.e.. curls, dissolves,
shrinks, or swells) is unsuitable for use.
4.4.2 To test for absorption or leaching by the filter:
4.4.2.1 Prepare a standard solution of the chemical species of interest.
4.4.2.2 Analyze the standard for its concentration of the chemical species.
4.4.2.3 Filter the standard and reanalyze. If the concentration of the filtrate
differs from that of the original standard, then the filter membrane leaches or absorbs
one or more of the chemical species and is not usable in this test method.
4.5 Structural integrity tester - A device meeting the specifications shown in Figure 4 and
having a 3.18-cm (1.25-in) diameter hammer weighing 0.33 kg (0.73 Ib) with a free fall of 15.24 cm
(6 in) shall be used. This device is available from Associated Design and Manufacturing
Company, Alexandria, VA 22314, as Part No. 125, or it may be fabricated to meet these
specifications.
5.0 REAGENTS
5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is
intended that all reagents shall 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 sufficiently high purity to
permit its use without lessening the accuracy of the determination.
5.2 Reagent water. All references to water in this method refer to reagent water, as
defined in Chapter One.
5.3 Acetic acid (0.5N), CH3COOH. This can be made by diluting concentrated glacial
acetic acid (17.5N) by adding 57 ml_ glacial acetic acid to 1,000 ml_ of water and diluting to 2
liters. The glacial acetic acid must be of high purity and monitored for impurities.
5.4 Analytical standards should be prepared according to the applicable analytical
methods.
131 OB-2 Revision 2
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6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6.1 Preservatives must not be added to samples.
6.2 Samples can be refrigerated if it is determined that refrigeration will not affect the
integrity of the sample.
7.0 PROCEDURE
7.1 If the waste does not contain any free liquid, go to Step 7.9. If the sample is liquid or
multiphase, continue as follows. Weigh filter membrane and prefilter to ฑ 0.01 g. Handle
membrane and prefilters with blunt curved-tip forceps or vacuum tweezers, or by applying suction
with a pipet.
7.2 Assemble filter holder, membranes, and prefilters following the manufacturer's
instructions. Place the 0.45-um membrane on the support screen and add prefilters in ascending
order of pore size. Do not prewet filter membrane.
7.3 Weigh out a representative subsample of the waste (100 g minimum).
7.4 Allow slurries to stand, to permit the solid phase to settle. Wastes that settle slowly
may be centrifuged prior to filtration.
7.5 Wet the filter with a small portion of the liquid phase from the waste or from the
extraction mixture. Transfer the remaining material to the filter holder and apply vacuum or gentle
pressure (10-15 psi) until all liquid passes through the filter. Stop filtration when air or
pressurizing gas moves through the membrane. If this point is not reached under vacuum or
gentle pressure, slowly increase the pressure in 10-psi increments to 75 psi. Halt filtration when
liquid flow stops. This liquid will constitute part or all of the extract (refer to Step 7.16). The liquid
should be refrigerated until time of analysis.
NOTE: Oil samples or samples containing oil are treated in exactly the same way as any other
sample. The liquid portion of the sample is filtered and treated as part of the EP extract.
If the liquid portion of the sample will not pass through the filter (usually the case with
heavy oils or greases), it should be carried through the EP extraction as a solid.
7.6 Remove the solid phase and filter media and, while not allowing them to dry, weigh
to ฑ 0.01 g. The wet weight of the residue is determined by calculating the weight difference
between the weight of the filters (Step 7.1) and the weight of the solid phase and the filter media.
7.7 The waste will be handled differently from this point on, depending on whether it
contains more or less than 0.5% solids. If the sample appears to have < 0.5% solids, determine
the percent solids exactly (see Note below) by the following procedure:
7.7.1 Dry the filter and residue at 80 ฐC until two successive weighings yield the
same value.
7.7.2 Calculate the percent solids, using the following equation:
131 OB-3 Revision 2
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weight of filtered solid and filters - tared weight of filters
r-;7-r . . , x 100 = % solids
initial weight of waste material
NOTE: This procedure is used only to determine whether the solid must be extracted or
whether it can be discarded unextracted. It is not used in calculating the amount of
water or acid to use in the extraction step. Do not extract solid material that has
been dried at 80 ฐC. A new sample will have to be used for extraction if a percent
solids determination is performed.
7.8 If the solid constitutes < 0.5% of the waste, discard the solid and proceed
immediately to Step 7.17, treating the liquid phase as the extract.
7.9 The solid material obtained from Step 7.5 and all materials that do not contain free
liquids shall be evaluated for particle size. If the solid material has a surface area per g of material
;>3.1 cm2 or passes through a 9.5-mm (0.375-in.) standard sieve, the operator shall proceed to
Step 7.11. If the surface area is smaller or the particle size larger than specified above, the solid
material shall be prepared for extraction by crushing, cutting, or grinding the material so that it
passes through a 9.5-mm (0.375-in.) sieve or, if the material is in a single piece, by subjecting the
material to the "Structural Integrity Procedure" described in Step 7.10.
7.10 Structural integrity procedure (SIP)
7.10.1 Cut a 3.3-cm diameter by 7.1-cm long cylinder from the waste material. If
the waste has been treated using a fixation process, the waste may be cast in the form of a
cylinder and allowed to cure for 30 days prior to testing.
7.10.2 Place waste into sample holder and assemble the tester. Raise the
hammer to its maximum height and drop. Repeat 14 additional times.
7.10.3 Remove solid material from tester and scrape off any particles adhering to
sample holder. Weigh the waste to the nearest 0.01 g and transfer it to the extractor.
7.11 If the sample contains > 0.5% solids, use the wet weight of the solid phase (obtained
in Step 7.6) to calculate the amount of liquid and acid to employ for extraction by using the
following equation:
W = Wf-W,
where:
W = Wet weight in g of solid to be charged to extractor.
W, = Wet weight in g of filtered solids and filter media.
W, = Weight in g of tared filters.
If the waste does not contain any free liquids, 100 g of the material will be subjected to the
extraction procedure.
131 OB-4 Revision 2
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7.12 Place the appropriate amount of material (refer to Step 7.11) into the extractor and
add 16 times its weight with water.
7.13 After the solid material and water are placed in the extractor, the operator shall begin
agitation and measure the pH of the solution in the extractor. If the pH is > 5.0, the pH of the
solution should be decreased to 5.0 ฑ 0.2 by slowly adding 0.5N acetic acid. If the pH is ^ 5.0, no
acetic acid should be added. The pH of the solution should be monitored, as described below,
during the course of the extraction, and, if the pH rises above 5.2, 0.5N acetic acid should be
added to bring the pH down to 5.0 ฑ 0.2. However, in no event shall the aggregate amount of acid
added to the solution exceed 4 ml of acid per g of solid. The mixture should be agitated for 24
hours and maintained at 20-40 ฐC (68-104 ฐF) during this time. It is recommended that the
operator monitor and adjust the pH during the course of the extraction with a device such as the
Type 45-A pH Controller, manufactured by Chemtrix, Inc., Hillsboro, Oregon 97123, or its
equivalent, in conjunction with a metering pump and reservoir of 0.5N acetic acid. If such a
system is not available, the following manual procedure shall be employed.
NOTE: Do not add acetic acid too quickly. Lowering the pH to below the target concentration of
5.0 could affect the metal concentrations in the leachate.
7.13.1 A pH meter should be calibrated in accordance with the manufacturer's
specifications.
7.13.2 The pH of the solution should be checked, and, if necessary, 0.5 N acetic
acid should be manually added to the extractor until the pH reaches 5.0 ฑ 0.2. The pH of the
solution should be adjusted at 15-, 30-, and 60-minute intervals, moving to the next longer
interval if the pH does not have to be adjusted > 0.5 pH units.
7.13.3 The adjustment procedure should be continued for at least 6 hours.
7.13.4 If, at the end of the 24-hour extraction period, the pH of the solution is not
below 5.2 and the maximum amount of acid (4 ml per g of solids) has not been added, the
pH should be adjusted to 5.0 ฑ 0.2 and the extraction continued for an additional 4 hours,
during which the pH should be adjusted at 1-hour intervals.
7.14 At the end of the extraction period, water should be added to the extractor in an
amount determined by the following equation:
V = (20)(W)-16(W)-A
where:
V = mL water to be added.
W = Weight in g of solid charged to extractor.
A = mL of 0.5N acetic acid added during extraction.
7.15 The material in the extractor should be separated into its component liquid and solid
phases in the following manner:
131 OB-5 Revision 2
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7.15.1 Allow slurries to stand to permit the solid phase to settle (wastes that are
slow to settle may be centrifuged prior to filtration) and set up the filter apparatus (refer to
Steps 4.3 and 4.4).
7.15.2 Wet the filter with a small portion of the liquid phase from the waste or from
the extraction mixture. Transfer the remaining material to the filter holder and apply vacuum
or gentle pressure (10-15 psi) until all liquid passes through the filter. Stop filtration when
air or pressurizing gas moves through the membrane. If this point is not reached under
vacuum or gentle pressure, slowly increase the pressure in 10-psi increments to 75 psi. Halt
filtration when liquid flow stops.
7.16 The liquids resulting from Steps 7.5 and 7.15 should be combined. This combined
liquid (or waste itself, if it has < 0.5% solids, as noted in Step 7.8) is the extract.
7.17 The extract is then prepared and analyzed using the appropriate analytical methods
described in Chapters Three and Four of this manual.
NOTE: If the EP extract includes two phases, concentration of contaminants is determined by
using a simple weighted average. For example: An EP extract contains 50 mL of oil and
1,000 mL of an aqueous phase. Contaminant concentrations are determined for each
phase. The final contamination concentration is taken to be:
(50x contaminant cone, in oil)+ (l.OOOx contaminant cone, of aqueous phase)
1050
NOTE: In cases where a contaminant was not detected, use the MDL in the calculation. For
example, if the MDL in the oily phase is 100 mg/L and 1 mg/L in the aqueous phase, the
reporting limit would be 6 mg/L (rounded to the nearest mg). If the regulatory threshold
is 5 mg/L, the waste may be EP toxic and results of the analysis are inconclusive.
8.0 QUALITY CONTROL
8.1 All quality control data should be maintained and available for easy reference or
inspection.
8.2 Employ a minimum of one blank per sample batch to determine if contamination or
any memory effects are occurring.
8.3 All quality control measures described in Chapter One and in the referenced
analytical methods should be followed.
131 OB-6 Revision 2
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9.0 METHOD PERFORMANCE
9.1 The data tabulated in Table 3 were obtained from records of state and contractor
laboratories and are intended to show the precision of the entire method (1310 plus analysis
method).
10.0 REFERENCES
1. Rohrbough, W.G.; et al. Reagent Chemicals. American Chemical Society Specifications. 7th
ed.; American Chemical Society: Washington, DC, 1986.
2. 1985 Annual Book of ASTM Standards. Vol. 11.01; "Standard Specification for Reagent
Water"; ASTM: Philadelphia, PA, 1985; D1193-77.
3. Gaskill, A., Compilation and Evaluation of RCRA Method Performance Data, Work
Assignment No. 2, EPA Contract No. 68-01-7075, September 1986.
131 OB-7 Revision 2
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TABLE 1. ERA-APPROVED FILTER HOLDERS
Manufacturer
Vacuum Filters
Gelman
Nalgene
Nuclepore
Millipore
Pressure Filters
Nuclepore
Micro Filtration
Systems
Millipore
Size
47mm
500 mL
47 mm
47 mm
142mm
142mm
142mm
Model No.
4011
44-0045
410400
XX1004700
425900
302300
YT30 142 HW
Comments
Disposable plastic unit, including
prefilter, filter pads, and reservoir;
can be used when solution is to be
analyzed for inorganic constituents.
1310B-8
Revision 2
November 2004
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TABLE 2. ERA-APPROVED FILTRATION MEDIA
Supplier
Filter to be used
for aqueous systems
Filter to be used
for organic systems
Coarse prefilter
Gelman
Nuclepore
Millipore
Medium prefilters
Gelman
Nuclepore
Millipore
Fine prefilters
Gelman
Nuclepore
Millipore
Fine filters (0.45 um)
Gelman
Pall
Nuclepore
Millipore
Selas
61631,61635
210907,211707
AP25 035 00,
AP2512750
61654, 61655
210905,211705
AP20 035 00,
AP2012450
64798, 64803
210903.211703
AP1503500,
AP1512450
63069, 66536
NX04750, NX14225
142218
HAWP 047 00,
HAWP 142 50
83485-02,
83486-02
61631,61635
210907,211707
AP25 035 00,
AP2512750
210905,211705
AP20 035 00,
AP2012450
64798, 64803
210903,211703
AP1503500,
AP1512450
60540 or 66149, 66151
1422183
FHUP 047 00,
FHLP 142 50
83485-02,
83486-02
Susceptible to decomposition by certain polar organic solvents.
1310B-9
Revision 2
November 2004
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TABLE 3. PRECISIONS OF EXTRACTION-ANALYSIS
PROCEDURES FOR SEVERAL ELEMENTS
Element
Sample Matrix
Analysis Method Laboratory Replicates
Arsenic
1. Auto Fluff
2. Barrel sludge
3. Lumber treatment company
sediment
7060
7060
7060
1.8, 1.5ug/L
0.9, 2.6 ug/L
28, 42 mg/L
Barium
1. Lead smelting emission
control dust
2. Auto Fluff
3. Barrel Sludge
6010
7081
7081
0.12, 0.12 mg/L
791, 780 ug/L
422, 380 ug/L
Cadmium 1. Lead smelting emission 3010/7130
control dust
2. Wastewater treatment 3010/7130
sludge from electroplating
3. Auto fluff
4. Barrel sludge 7131
5. Oil refinery tertiary pond 7131
sludge 7131
120, 120 mg/L
360, 290 mg/L
470, 610 ug/L
1100, 890
3.2,1.9 ug/L
Chromium 1. Wastewater treatment
sludge from electroplating
2. Paint primer
3. Paint primer filter
4. Lumber treatment company
sediment
5. Oil refinery tertiary pond
sludge
3010/7190
1.1,1.2 mg/L
61, 43 ug/L
7191
7191
7191 0.81, 0.89 mg/L
7191
Mercury
1. Barrel sludge
2. Wastewater treatment
sludge from electroplating
3. Lead smelting emission
control dust
7470
7470
7470
0.15, 0.09 pg/L
1.4, 0.4M9/L
0.4, 0.4
1310B-10
Revision 2
November 2004
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TABLE 3 (Continued)
Element
Lead
Sample Matrix
1. Lead smelting emission
control dust
2. Auto fluff
3. Incinerator ash
4. Barrel sludge
5. Oil refinery tertiary pond
sludge
Analysis Method
3010/7420
7421
7421
7421
7421
Laboratory Replicates
940, 920 mg/L
1540, 1490 ug/L
1000, 974 ug/L
2550, 2800 ug/L
31, 29 ug/L
Nickel
1. Sludge 7521
2. Wastewater treatment 3010/7520
sludge from electroplating
2260, 1720 ug/L
130, 140 mg/L
Chromium (VI)
1. Wastewater treatment
sludge from electroplating
7196
18, 19 ug/L
1310B-11
Revision 2
November 2004
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FIGURE!
EXTRACTOR
5.0
.25
4.0
1
Non-Clogging Support Bushing
1 Inch Blade at 30ฐ to Horizontal
9.0
1310B-12
Revision 2
November 2004
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FIGURE 2.
ROTARY EXTRACTOR
1310B-13
Revision 2
November 2004
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FIGURE 3.
EPRI EXTRACTOR
I-Galloo Plastic
or Glass Beetle
Foam Bonded to Cover
Box Assembly
Plywood Construction
Totilly Enclosed
Fta Cooled Motor
30 rpm, 1/8 HP
1310B-14
Revision 2
November 2004
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FIGURE 4.
COMPACTION TESTER
Combined Weight
0.33 kg (0.73 Ib)
Sample
Elastomenc
Sample Holder
1310B-15
Revision 2
November 2004
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METHOD 1310B
EXTRACTION PROCEDURE (EP) TOXICITYTEST METHOD
AND STRUCTURAL INTEGRITY TEST
71 H.igh fill.r
nambranc and
prafiltar
72 Aป*mbl. filt.c
holder, mambranaa,
and prafi1tar*
7.3 W.igh out
aubtampla of wait*
7 4 L*L sol id ph*ปซ
>attlซ; c*ntriฃugซ
if n.c.n.ry
75 Filtซr gut
liquid phaia and
rซfrigซrซte it
1310B-16
Revision 2
November 2004
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METHOD 131 OB
(Continued)
Area >
3 1 cซ2/9
or pa**eป
through
9.5 mm
7
8 Discard solids
7.10 1 Cut or east
cylinder Iron wast*
material for
Structural
Integrity Procedure
7 9 Prepare
materlal for
extraction by
crushing, cutting,
or grinding
7 10 2 At.emble
tester; drop banner
IS times
7 10 3 Remove solid
Material; weigh;
transfer to
extractor
1310B-17
Revision 2
November 2004
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METHOD 131 OB
(Continued)
7
IS Al law i lur neซ
to ป land ; ปe t up
filter apparatus ;
filter
7.11 Calculate
amount of liquid
and acid to uซe for
traction
7.12 Place material
into tractor; add
deionized water
7 11 Uie 100 g of
malarial for
traction
procedure
7.16 Combine
liquid* from
Section* 7 S and
7.15 to analyze for
c o n t a m i na n tป
7.13 Agitat. for 24
hour, and -monitor
pH of *olution
7 17 Obtain
analytical mathod
fron Chapter* 3 and
4
7 .13 Calibrate and
adjust pH meter
7.18 Compare
tract
concentrat ion to
max mum
contamination
1imiti to determine
CP loncity
7.14 At end of
traction period,
add deianizcd water
STOP
1310B-18
Revision 2
November 2004
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