\o
United States
Environmental Protection
Agency
nest Methods for Evaluating Solid
Physical/Chemical Methods
-------
Office of Solid Waste and
Emergency Response (5102G)
EPA-SW-846-03-03B
www.epa.gov
August 2002
-------
PROPOSED UPDATE 1MB
TEST METHODS FOR EVALUATING SOLID WASTE
PHYSICAL/CHEMICAL METHODS
(SW-846) THIRD EDITION
THIS PACKET CONTAINS REVISED MATERIAL
PROPOSED FOR INCLUSION IN THE EPA PUBLICATION SW-846
Contents:
1. Cover sheet. (What you are currently reading)
2. Instructions. This section explains how Proposed Update IIIB 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. Proposed Update IIIB Table of Contents. The Table of Contents (dated
August 2002) lists all of the methods (as updated by Third Edition Final
Updates I, II, IIA, IIB, III, and IIIA and Proposed Update IIIB) in the
order of appearance in the manual. It does not reflect Draft Update
IVA or B methods because the Agency plans to publish Final Update
IIIB before the final versions of the Draft Update IVA or B methods.
5. Revised Chapter Five and revised Methods 9010C. 9012B. 9060A. and
9070A.
6. Revised Chapter Six and revised Methods 9045D and 9095B.
7. Revised Chapter Seven
8. Revised Chapter Eight and revised 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, n, HA, DB, and ffl, fflA, and Draft Updates IV A and
IVB. (Currently, the methods and chapters of Final Update IDA and 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 Proposed Update
These instructions describe how to get your basic manual up-to-date and what to do with your
Proposed Update LLLB package. A number of SW-846 update packages have been released to the
public since the original Third Edition was released. The dates and labels on these packages can
be confusing. In general, final updates should always be incorporated into SW-846 in
chronological order (e.g., Update I should be incorporated before Update IT).
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 defined as individuals that have received copies of the Third
Edition and other SW-846 updates (including proposed updates) in the past and have just
received only this Proposed Update nffi package in the mail.
New subscribers are defined as individuals who have recently (6-8 weeks) placed an
order with the GPO and have received new copies of the 4 (four) volume set of the Third
Edition, a copy of Final Update I, a copy of Final Update n/HA, a copy of Final Update
HE, a copy of Final Update HI, a copy of Draft Update FVA, and a copy of this Proposed
Update
Instructions - 1 Proposed Update EHB
August 2002
-------
INCORPORATING PROPOSED UPDATE IIIB IN YOUR MANUAL
Proposed Update TTTR is printed on buff colored paper and has the date of "August 2002" in the
lower right hand corner of each page. This package contains revised material proposed for
addition to SW-846. Because it is a proposed update and not yet final, its proposed methods
cannot yet be used for compliance with required uses of SW-846 methods in the RCRA
regulations. 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
may 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 should augment the manual with other binders of
your choice. The instructions below can be generally 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 your Proposed Update HIB (those who obtained their manual from other
sources, may also find this information useful in putting it together):
Place the original Third Edition of SW-846 (September 1986) in the properly labeled four
3-ring notebooks according to the instructions in Final Update D3.
Incorporate Final Update I (July 1992) into the manual according to the instructions in
Final Update m.
Incorporate Final Updates n (September 1994) and HA (August 1993) into the manual
according to the instructions in Final Update ID.
Incorporate Final Update IIB (January 1995) into the manual according to the instructions
in Final Update IJJ.
Incorporate Final Update HI (December 1996) into the manual according to its
instructions.
Either incorporate Draft Update IV A in the manual (without removing any white pages),
or keep the colored draft update in a separate binder of your choice.
Finally, incorporate Proposed Update HIB into the manual without removing any white pages, or
keep the colored proposed update in a separate binder of your choice.
Instructions - 2 Proposed Update HIB
August 2002
-------
PREVIOUS GPO SUBSCRIBERS - If you are a previous subscriber, it is important to
establish exactly what is currently contained in your manual before addressing Proposed Update
fflB. If your manual is properly updated, the ONLY white pages in the document should be
dated September 1986 (Third Edition), July 1992 (Final Update I), August 1993 (Final Update
HA), September 1994 (Final Update n), January 1995 (Final Update UB), December 1996 (Final
Update HI), and April 1998 (if you have added Final Update UIA from NTIS or the EPA OSW
Methods web site). Remove (and recycle or archive) any white pages from your manual that
have any other dates.
There may also be colored pages (e.g., pink pages for Proposed Update HI) 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. You may keep proposed or
draft update pages in the manual if you wish, but those methods are not promulgated final
methods and thus cannot be used for required uses of SW-846 methods in the RCRA regulations.
Finally, incorporate Proposed Update fflB into the manual without removing any white pages, or
keep the colored proposed update in a separate binder of your choice.
Instructions - 3 Proposed Update fflB
August 2002
-------
UPDATE HISTORY OF SW-846
(Finalized updates are printed in bold and underlined.)
Package
Third Edition
Proposed Update I
Final Update I
Proposed Update II
Final Update I
Proposed Update II
Proposed Update HA
Final Update IIA
(Method 4010, included
with Final Update II.)
Final Update II
Final Update IIB
Proposed Update EII
Final Update III
Draft Update IVA
Final Update IHA*
Draft Update IVB
Proposed Update IUB
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, may
be later if
revised again
and added to
web site
August 2002
Paper Color
White
Green
White
Blue
White
Yellow
White
White
White
White
Pink
White
Salmon
White
Only
available at
www.epa.gov
/SW-846
Buff
Status of Package
Finalized (Promulgated)
Obsolete
Obsolete! Never formally
finalized.
Obsolete! Never formally
proposed.
Finalized (Promulgated)
Obsolete
Obsolete
Finalized (Promulgated)
Finali/ed (Promulnated)
Finalized (Promulgated)
Proposed
Finalized (Promulgated)
Draft
Finalized (Promulgated)
Draft
Proposed
*Contains revised Table of Contents, revised Chapter Five, and revised Methods 9070 and
9071B.
Instructions - 4
Proposed Update HIE
August 2002
-------
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 Proposed Update Hffi
August 2002
-------
STATUS TABLES FOR
SW-846, THIRD EDITION
ADDRESSES METHODS FOUND IN:
FINAL UPDATES I, II, IIA, MB, III, AND IIIA
DRAFT UPDATES IVA AND IVB
OTHER DRAFT METHODS AT THE OSW METHODS WEB SITE AS OF OCTOBER 2002
AND PROPOSED UPDATE NIB
REVISED OCTOBER 2002
-------
HOW TO USE THIS DOCUMENT
This document provides historical status information on 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 current status of published SW-846 methods. Methods
in this status table are listed sequentially by method number. Use the "Status Table for SW-846 Chapter Text and Other Documents" as a reference
guide to identify the historical and current status of published chapters and other SW-846 documents (e.g., the Disclaimer).
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 METH
Octo
Uric
ATUS TABLE
002
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. I
(7/92)
-
-
-
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
-
-
-
~
-
FIN. UP.
Ill (12/96)
IDA (4/98)
-
0011
(Up. Ill)
0023A
(Up. Ill)
(Revision
of Method
23,40
CFR Part
60)
-
0031
(Up. Ill)
PROP.
UP. 1MB
(8/02)
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
DRAFT
UP. IVB
(11/00)
-
25D
Referral
25E
Referral
-
-
OTHER
NEW
SW-846
METHODS
-
-
-
--
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)
CURRENT
PROMUL-
GATED
METHOD
0010
RevO
(9/86)
0011
RevO
(12/96)
0020
RevO
(9/86)
0023A
Rev1
(12/96)
See 40 CFR
60, App. A
See 40 CFR
60, App. A
0030
RevO
(9/86)
0031
RevO
(12/96)
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
-
-
-
-
-
-
FIN. UP.
Ill (12/96)
IIIA (4/98)
0040 -
(Up. Ill)
0050
(Up. Ill)
0051
(Up. Ill)
0060
(Up. Ill)
0061
(Up. Ill)
0100
(Up. Ill)
~
PROP.
UP. IIIB
(8/02)
~
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
-
207-1
Referral
207-2
Referral
OTHER
NEW
SW-846
METHODS
-
~
-
-
~
-
METHOD TITLE
Sampling of Principal Organic
Hazardous Constituents from
Combustion Sources Using
Tedlarฎ Bags
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)
CURRENT
PROMUL-
GATED
METHOD
0040
RevO
(12/96)
0050
RevO
(12/96)
0051
RevO
(12/96)
0060
RevO
(12/96)
0061
RevO
(12/96)
0100
RevO
(12/96)
Not Promul-
gated
Not Promul-
gated
-------
SW-84"" HOD STATUS TABLE (10/02), 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
-
1110
1310
FINAL
UP. I
(7/92)
-
1020A
-
-
1310A
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
FIN. UP.
Ill (12/96)
IIIA (4/98)
1030
(Up. Ill)
-
-
1120
(Up. Ill)
PROP.
UP. IIIB
(8/02)
1010A
1020B
-
-
1110A
1310B
DRAFT
UP. IVA
(1/98)
~
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
1040
1050
-
-
-
OTHER
NEW
SW-846
METHODS
-
-
-
~
-
METHOD TITLE
Pensky-Martens Closed-Cup
Method for Determining Ignitability
1020A (Promulgated): Setaflash
Closed-Cup Method for
Determining Ignitability
1020B (Proposed Up. IIIB): Small
Scale Closed-Cup Method for
Determining Ignitability
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
CURRENT
PROMUL-
GATED
METHOD
1010
RevO
(9/86)
1020A
Rev1
(7/92)
1030
RevO
(12/96)
Not Promul-
gated
Not Promul-
gated
1110
RevO
(9/86)
1120
RevO
(12/96)
1310A
Rev1
(7/92)
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
-
-
1320
1330
3005
3010
-
3020
FINAL
UP. I
(7/92)
1311
~
~
1330A
3005A
301 OA
-
3020A
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
1312
(Up. II)
-
-
3015
(Up. II)
FIN. UP.
111(12/96)
IDA (4/98)
~
-
-
-
-
PROP.
UP. IIIB
(8/02)
-
~
-
-
-
DRAFT
UP. IVA
(1/98)
-
--
-
3015A
DRAFT
UP. IVB
(11/00)
~
-
-
-
-
OTHER
NEW
SW-846
METHODS
-
-
METHOD TITLE
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
Spectroscopy
Microwave Assisted Acid Digestion
of Aqueous Samples and Extracts
Acid Digestion of Aqueous
Samples and Extracts for Total
Metals for Analysis by GFAA
Spectroscopy
CURRENT
PROMUL-
GATED
METHOD
1311
RevO
(7/92)
1312
RevO
(9/94)
1320
RevO
(9/86)
1330A
Rev 1
(7/92)
3005A
Rev 1
(7/92)
3010A
Rev1
(7/92)
3015
RevO
(9/94)
3020A
Rev1
(7/92)
1
-------
SW-84^ HOD STATUS TABLE (10/02), 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)
-
3040
3050
-
-
[3060, in
the
2nd Ed.]
3500
3510
3520
FINAL
UP. I
(7/92)
-
-
3050A
-
3500A
351 OA
3520A
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
-
3051
(Up. II)
-
-
-
3510B
(Up. II)
3520B
(Up. II)
FIN. UP.
111(12/96)
III A (4/93)
3031
(Up. Ill)
3040A
(Up. Ill)
3050B
(Up. Ill)
3052
(Up. Ill)
3060A
(Up. Ill)
3500B
(Up. Ill)
351 OC
(Up. Ill)
3520C
(Up. Ill)
PROP.
UP. 1MB
(8/02)
-
DRAFT
UP. IVA
(1/98)
3051A
-
-
DRAFT
UP. IVB
(11/00)
-
~
-
3500C
OTHER
NEW
SW-846
METHODS
-
-
-
-
-
-
METHOD TITLE
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
Continuous Liquid-Liquid Extraction
CURRENT
PROMUL-
GATED
METHOD
3031
RevO
(12/96)
3040A
Rev 1
(12/96)
3050B
Rev 2
(12/96)
3051
RevO
(9/94)
3052
RevO
(12/96)
3060A
Rev1
(12/96)
3500B
Rev 2
(12/96)
351 OC
Rev 3
(12/96)
3520C
Rev 3
(12/96)
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
3540
~
-
3550
~
FINAL
UP. 1
(7/92)
3540A
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
3540B
(Up. II)
3541
(Up. II)
-
3550A
(Up. II)
-
FIN. UP.
111(12/96)
IIIA (4/98)
3535
(Up. Ill)
3540C
(Up. Ill)
-
3542
(Up. Ill)
3545
(Up. Ill)
3550B
(Up. Ill)
3560
(Up. Ill)
PROP.
UP. IIIB
(8/02)
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
3535A
-
-
3545A
-
-
-
DRAFT
UP. IVB
(11/00)
3535A
(Replaces
IVA
version)
-
3545A
(Replaces
IVA
version)
3546
3550C
-
OTHER
NEW
SW-846
METHODS
-
-
-
-
METHOD TITLE
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
Supercritical Fluid Extraction of
Total Recoverable Petroleum
Hydrocarbons
CURRENT
PROMUL-
GATED
METHOD
3535
RevO
(12/96)
3540C
Rev 3
(12/96)
3541
RevO
(9/94)
3542
RevO
(12/96)
3545
RevO
(12/96)
Not Promul-
gated
3550B
Rev 2
(12/96)
3560
RevO
(12/96)
-------
SW-846
HOD STATUS TABLE (10/02), 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. I
(7/92)
-
-
3580A
-
3600A
361 OA
3611 A
3620A
3630A
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
3600B
(Up. II)
3630B
(Up. II)
FIN. UP.
111(12/96)
IMA (4/98)
3561
(Up. Ill)
-
-
3585
(Up. Ill)
3600C
(Up. Ill)
361 OB
(Up. Ill)
361 1B
(Up. Ill)
3620B
(Up. Ill)
3630C
(Up. Ill)
PROP.
UP. IIIB
(8/02)
-
-
-
--
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
3562
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
~
~
-
-
-
3620C
OTHER
NEW
SW-846
METHODS
-
-
-
-
-
METHOD TITLE
Supercritical Fluid Extraction of
Polynuclear Aromatic
Hydrocarbons
Supercritical Fluid Extraction of
Polychlorinated Biphenyls (PCBs)
and Organochlorine Pesticides
Waste Dilution
Waste Dilution for Volatile Organics
Cleanup
Alumina Cleanup
Alumina Column Cleanup and
Separation of Petroleum Wastes
Florisil Cleanup
Silica Gel Cleanup
CURRENT
PROMUL-
GATED
METHOD
3561
RevO
(12/96)
Not Promul-
gated
3580A
Rev 1
(7/92)
3585
RevO
(12/96)
3600C
Rev 3
(12/96)
361 OB
Rev 2
(12/96)
361 1B
Rev 2
(12/96)
3620B
Rev 2
(12/96)
3630C
Rev 3
(12/96)
-------
SW-846 METHOD STATUS TABLE (10/02), 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. I
(7/92)
-
3650A
3660A
-
-
-
--
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
3640A
(Up. II)
-
-
3665
(Up. II)
-
FIN. UP.
111(12/96)
IDA (4/98)
3650B
(Up. Ill)
3660B
(Up. Ill)
3665A
(Up. Ill)
-
-
4000
(Up. Ill)
PROP.
UP. NIB
(8/02)
-
~
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
~
-
Noticed
for
removal
from
SW-846
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
-
3815
~
-
OTHER
NEW
SW-846
METHODS
-
~
-
-
-
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
CURRENT
PROMUL-
GATED
METHOD
3640A
Rev1
(9/94)
3650B
Rev 2
(12/96)
3660B
Rev 2
(12/96)
3665A
Rev1
(12/96)
3810
RevO
(9/86)
Not Promul-
gated
3820
RevO
(9/86)
4000
RevO
(12/96)
-------
STATUS TABLE (10/02), 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)
4010
(Up. IIA)
-
~
~
~
FIN. UP.
111(12/96)
IMA (4/98)
401 OA
(Up. Ill)
4015
(Up. Ill)
4020
(Up. Ill)
4030
(Up. Ill)
4035
(Up. Ill)
4040
(Up. Ill)
4041
(Up. Ill)
4042
(Up. Ill)
PROP.
UP. 1MB
(8/02)
-
-
-
-
DRAFT
UP. IVA
(1/98)
DRAFT
UP. IVB
(11/00)
-
-
-
-
-
-
OTHER
NEW
SW-846
METHODS
-
-
-
-
-
METHOD TITLE
Screening for Pentachlorophenol
by Immunoassay
Screening for
2,4-Dichlorophenoxyacetic Acid by
Immunoassay
Screening for Polychlorinated
Biphenyls 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
CURRENT
PROMUL-
GATED
METHOD
4010A
Rev1
(12/96)
4015
RevO
(12/96)
4020
RevO
(12/96)
4030
RevO
(12/96)
4035
RevO
(12/96)
4040
RevO
(12/96)
4041
RevO
(12/96)
4042
RevO
(12/96)
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
-
FIN. UP.
111(12/96)
IDA (4/98)
4050
(Up. Ill)
4051
(Up. Ill)
-
5000
(Up. Ill)
5021
(Up. Ill)
PROP.
UP. IIIB
(8/02)
-
-
-
DRAFT
UP. IVA
(1/98)
-
4500
4670
DRAFT
UP. IVB
(11/00)
-
4425
~
OTHER
NEW
SW-846
METHODS
4025
(10/02)
-
-
-
-
-
METHOD TITLE
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
Immunoassay
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
Volatile Organic Compounds in
Soils and Other Solid Matrices
Using Equilibrium Headspace
Analysis
CURRENT
PROMUL-
GATED
METHOD
Not Promul-
gated
4050
RevO
(12/96)
4051
RevO
(12/96)
Not Promul-
gated
Not Promul-
gated
Not Promul-
gated
5000
RevO
(12/96)
5021
RevO
(12/96)
-------
SW-846 IOD STATUS TABLE (10/02), 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
~
5040
-
6010
FINAL
UP. I
(7/92)
5030A
-
-
-
6010A
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
~
-
-
5040A
(Up. II)
5041
(Up. II)
5050
(Up. II)
FIN. UP.
Ill (12/96)
IIIA (4/98)
5030B
(Up. Ill)
5031
(Up. Ill)
5032
(Up. Ill)
5035
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
5041 A
(Up. Ill)
6010B
(Up. Ill)
PROP.
UP. NIB
(8/02)
-
-
-
~
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
-
-
-
6010C
OTHER
NEW
SW-846
METHODS
-
5035A
(7/02)
-
METHOD TITLE
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 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
CURRENT
PROMUL-
GATED
METHOD
5030B
Rev 2
(12/96)
5031
RevO
(12/96)
5032
RevO
(12/96)
5035
RevO
(12/96)
Deleted
from
SW-846
5041 A
Rev 1
(12/96)
5050
RevO
(9/94)
6010B
Rev 2
(12/96)
11
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
~
-
~
7000
-
7020
FINAL
UP. I
(7/92)
-
-
7000A
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
6020
(Up. II)
-
-
FIN. UP.
111(12/96)
IIIA (4/98)
-
~
-
-
PROP.
UP. IIIB
(8/02)
-
-
DRAFT
UP. IVA
(1/98)
6020A
6200
6500
6800
7000B
7010
Noticed
for
removal
from
SW-846
DRAFT
UP. IVB
(11/00)
-
-
OTHER
NEW
SW-846
METHODS
-
-
-
METHOD TITLE
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
7000A (Promulgated): Atomic
Absorption Methods
7000B (Draft Up. IVA): Flame
Atomic Absorption
Spectrophotometry
Graphite Furnace Atomic
Absorption Spectrophotometry
Aluminum (Atomic Absorption,
Direct Aspiration)
CURRENT
PROMUL-
GATED
METHOD
6020
RevO
(9/94)
Not Promul-
gated
Not Promul-
gated
Not Promul-
gated
7000A
Rev 1
(7/92)
Not Promul-
gated
7020
RevO
(9/86)
-------
SW-84 HOD STATUS TABLE (10/02), 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)
7040
7041
7060
7061
-
-
FINAL
UP. 1
(7/92)
7061 A
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
7060A
(Up. II)
-
7062
(Up. II)
-
FIN. UP.
111(12/96)
IDA (4/98)
7063
(Up. Ill)
PROP.
UP. 1MB
(8/02)
-
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
NEW
SW-846
METHODS
~
METHOD TITLE
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)
CURRENT
PROMUL-
GATED
METHOD
7040
RevO
(9/86)
7041
RevO
(9/86)
7060A
Rev1
(9/94)
7061A
Rev1
(7/92)
7062
RevO
(9/94)
7063
RevO
(12/96)
13
-------
SW-846 METHOD STATUS TABLE (10/02), 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. I
(7/92)
7081
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
7080A
(Up. II)
FIN. UP.
111(12/96)
MIA (4/98)
PROP.
UP. IIIB
(8/02)
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
NEW
SW-846
METHODS
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)
CURRENT
PROMUL-
GATED
METHOD
7080A
Rev1
(9/94)
7081
RevO
(7/92)
7090
RevO
(9/86)
7091
RevO
(9/86)
7130
RevO
(9/86)
-------
STATUS TABLE (10/02), 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
FINAL
UP. I
(7/92)
__
_,.
__
7196A
FIN. UP.
II (9/94)
HA (8/93)
IIB (1/95)
7131A
(Up. II)
-_
..
ป
__
FIN. UP.
Ill (12/96)
MIA (4/98)
__
__
ซ
__
__
PROP.
UP. NIB
(8/02)
__
__
__
-_
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
NEW
SW-846
METHODS
__
__
__
__
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)
CURRENT
PROMUL-
GATED
METHOD
7131A
Rev 1
(9/94)
7140
RevO
(9/86)
7190
RevO
(9/86)
7191
RevO
(9/86)
7195
RevO
(9/86)
7196A
Rev1
(7/92)
15
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
7197
7198
w_
7200
7201
7210
FINAL
UP. I
(7/92)
_
__
FIN. UP.
II (9/94)
HA (8/93)
MB (1/95)
__
_
FIN. UP.
111(12/96)
IMA (4/98)
-_
7199
(Up. Ill)
PROP.
UP. IIIB
(8/02)
_-
ซ.
_..
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
NEW
SW-846
METHODS
__
__
_
__
METHOD TITLE
Chromium, Hexavalent
(Chelation/Extraction)
Chromium, Hexavalent (Differential
Pulse Polarography)
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)
CURRENT
PROMUL-
GATED
METHOD
7197
RevO
(9/86)
7198
RevO
(9/86)
7199
RevO
(12/96)
7200
RevO
(9/86)
7201
RevO
(9/86)
7210
RevO
(9/86)
-------
SW-ฃ
Note:
'HOD STATUS TABLE (10/02), CONTINUED
trie 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. I
(7/92)
7211
7381
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
FIN. UP.
111(12/96)
IIIA (4/98)
PROP.
UP. IIIB
(8/02)
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
NEW
SW-846
METHODS
METHOD TITLE
Copper (Atomic Absorption,
Furnace Technique)
Iron (Atomic Absorption, Direct
Aspiration)
Iron (Atomic Absorption, Furnace
Technique)
Lead (Atomic Absorption, Direct
Aspiration)
Lead (Atomic Absorption, Furnace
Technique)
CURRENT
PROMUL-
GATED
METHOD
7211
RevO
(7/92)
7380
RevO
(9/86)
7381
RevO
(7/92)
7420
RevO
(9/86)
7421
RevO
(9/86)
17
-------
SW-846 METHOD STATUS TABLE (10/02), 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. 1
(7/92)
7430
_
7461
FIN. UP.
II (9/94)
MA (8/93)
MB (1/95)
__
7470A
(Up. II)
7471 A
(Up. II)
FIN. UP.
111(12/96)
IIIA (4/98)
__
__
._
PROP.
UP. IIIB
(8/02)
__
__
__
__
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
747 1B
DRAFT
UP. IVB
(11/00)
__
__
__
__
OTHER
NEW
SW-846
METHODS
__
METHOD TITLE
Lithium (Atomic Absorption, Direct
Aspiration)
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)
CURRENT
PROMUL-
GATED
METHOD
7430
RevO
(7/92)
7450
RevO
(9/86)
7460
RevO
(9/86)
7461
RevO
(7/92)
7470A
Rev1
(9/94)
7471 A
Rev 1
(9/94)
-------
SW-84~HOD STATUS TABLE (10/02), CONTINUED
Note: rnlfllte 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. I
(7/92)
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
~
~
FIN. UP.
111(12/96)
MIA (4/98)
7472
(Up. Ill)
PROP.
UP. NIB
(8/02)
-
~
DRAFT
UP. IVA
(1/98)
~
7473
7474
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
Noticed
for
removal
from
SW-846
DRAFT
UP. IVB
(11/00)
-
OTHER
NEW
SW-846
METHODS
--
METHOD TITLE
Mercury in Aqueous Samples and
Extracts by Anodic Stripping
Voltammetry (ASV)
Mercury in Solids and Solutions by
Thermal Decomposition,
Amalgamation, and Atomic
Absorption Spectrophotometry
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)
CURRENT
PROMUL-
GATED
METHOD
7472
RevO
(12/96)
Not Promul-
gated
Not Promul-
gated
7480
RevO
(9/86)
7481
RevO
(9/86)
7520
RevO
(9/86)
19
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
MA (8/93)
IIB (1/95)
7741A
(Up. II)
FIN. UP.
111(12/96)
IDA (4/98)
7521
(Up. Ill)
7580
(Up. Ill)
__
PROP.
UP. NIB
(8/02)
__
__
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
NEW
SW-846
METHODS
_^
__
METHOD TITLE
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)
CURRENT
PROMUL-
GATED
METHOD
7521
RevO
(12/96)
7550
RevO
(9/86)
7580
RevO
(12/96)
7610
RevO
(9/86)
7740
RevO
(9/86)
7741A
Rev 1
(9/94)
-------
SW-846=IOD STATUS TABLE (10/02), 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.I
(7/92)
-
7760A
7761
7780
FIN. UP.
II (9/94)
HA (8/93)
IIB (1/95)
7742
(Up. II)
FIN. UP.
111(12/96)
MIA (4/98)
-
PROP.
UP. IIIB
(8/02)
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
NEW
SW-846
METHODS
-
METHOD TITLE
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)
CURRENT
PROMUL-
GATED
METHOD
7742
RevO
(9/94)
7760A
Rev1
(7/92)
7761
RevO
(7/92)
7770
RevO
(9/86)
7780
RevO
(7/92)
7840
RevO
(9/86)
21
-------
SW-846 METHOD STATUS TABLE (10/02), 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. I
(7/92)
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
FIN. UP.
Ill (12/96)
IIIA (4/98)
PROP.
UP. NIB
(8/02)
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
NEW
SW-846
METHODS
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)
CURRENT
PROMUL-
GATED
METHOD
7841
RevO
(9/86)
7870
RevO
(9/86)
7910
RevO
(9/86)
7911
RevO
(9/86)
7950
RevO
(9/86)
n
-------
SW-84M HOD STATUS TABLE (10/02), 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
8010A
8011
8015A
8021
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
-
8010B
(Up. II)
-
8020A
(Up. II)
8021 A
(Up. II)
FIN. UP.
Ill (12/96)
IMA (4/98)
8000B
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
8015B
Deleted
from
SW-846
(Up. Ill)
8021 B
(Up. Ill)
PROP.
UP. IIIB
(8/02)
-
-
DRAFT
UP. IVA
(1/98)
Noticed
for
removal
from
SW-846
-
-
DRAFT
UP. IVB
(11/00)
-
801 5C
OTHER
NEW
SW-846
METHODS
-
~
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
CURRENT
PROMUL-
GATED
METHOD
7951
RevO
(7/92)
8000B
Rev 2
(12/96)
Deleted from
SW-846
8011
RevO
(7/92)
801 5B
Rev 2
(12/96)
Deleted from
SW-846
802 1B
Rev 2
(12/96)
23
-------
SW-846 METHOD STATUS TABLE (10/02), 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
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
8031
(Up. II)
8032
(Up. II)
-
8061
(Up. II)
FIN. UP.
111(12/96)
IIIA (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)
PROP.
UP. 1MB
(8/02)
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
~
-
DRAFT
UP. IVB
(11/00)
-
-
-
8041A
-
OTHER
NEW
SW-846
METHODS
-
-
-
-
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)
CURRENT
PROMUL-
GATED
METHOD
Deleted from
SW-846
8031
RevO
(9/94)
8032A
Rev1
(12/96)
8033
RevO
(12/96)
Deleted from
SW-846
8041
RevO
(12/96)
Deleted from
SW-846
8061A
Rev1
(12/96)
-------
SW-846
HOD STATUS TABLE (10/02), 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
-
FINAL
UP. 1
(7/92)
8070
-
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
-
8080A
(Up. II)
8081
(Up. II)
-
FIN. UP.
111(12/96)
IIIA (4/98)
8070A
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
8081A
(Up. Ill)
8082
(Up. Ill)
Deleted
from
SW-846
(Up. Ill)
8091
(Up. Ill)
PROP.
UP. NIB
(8/02)
-
-
DRAFT
UP. IVA
(1/98)
-
8081 B
8082A
-
DRAFT
UP. IVB
(11/00)
8081 B
(Replaces
IVA
version)
8082A
(Replaces
IVA
version)
8085
-
OTHER
NEW
SW-846
METHODS
METHOD TITLE
Nitrosamines by Gas
Chromatography
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
CURRENT
PROMUL-
GATED
METHOD
8070A
Rev 1
(12/96)
Deleted from
SW-846
8081A
Rev1
(12/96)
8082
RevO
(12/96)
Not Promul-
gated
Deleted from
SW-846
8091
RevO
(12/96)
25
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
-
8100
-
8120
-
-
8140
FINAL
UP. I
(7/92)
-
~
8110
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
~
--
8120A
(Up. II)
8121
(Up. II)
-
FIN. UP.
Ill (12/96)
MIA (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)
PROP.
UP. IIIB
(8/02)
-
~
-
~
~
DRAFT
UP. IVA
(1/98)
-
-
-
-
~
DRAFT
UP. IVB
(11/00)
8095
-
OTHER
NEW
SW-846
METHODS
-
-
-
-
~
METHOD TITLE
Explosives by Gas
Chromatography
Polynuclear Aromatic
Hydrocarbons
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
CURRENT
PROMUL-
GATED
METHOD
Not Promul-
gated
8100
RevO
(9/86)
Deleted from
SW-846
8111
RevO
(12/96)
Deleted from
SW-846
8121
RevO
(9/94)
8131
RevO
(12/96)
Deleted from
SW-846
-------
SW-846= IOD STATUS TABLE (10/02), 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)
8141
8150A
8240A
8260
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
8141A
(Up. II)
81 508
(Up. II)
8151
(Up. II)
8240B
(Up. II)
8250A
(Up. II)
8260A
(Up. II)
FIN. UP.
111(12/96)
IMA (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)
PROP.
UP. IIIB
(8/02)
DRAFT
UP. IVA
(1/98)
8141B
DRAFT
UP. IVB
(11/00)
8141B
(Replaces
IVA
version)
-
OTHER
NEW
SW-846
METHODS
-
METHOD TITLE
8141A (Promulgated):
Organophosphorus Compounds by
Gas Chromatography: Capillary
Column Technique
8141 B (Draft Up. IVB):
Organophosphorus Compounds by
Gas Chromatography
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
Spectrometrv (GC/MS)
CURRENT
PROMUL-
GATED
METHOD
8141A
Rev 1
(9/94)
Deleted from
SW-846
8151A
Rev1
(12/96)
Deleted from
SW-846
Deleted from
SW-846
8260B
Rev 2
(12/96)
27
-------
SW-846 METHOD STATUS TABLE (10/02), 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
FINAL
UP. I
(7/92)
8270A
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
8270B
(Up. II)
8275
(Up- II)
FIN. UP.
Ill (12/96)
IDA (4/98)
~
8270C
(Up. Ill)
8275A
(Up. Ill)
PROP.
UP. 1MB
(8/02)
-
DRAFT
UP. IVA
(1/98)
8270D
DRAFT
UP. IVB
(11/00)
8261
--
OTHER
NEW
SW-846
METHODS
8265
(3/02)
METHOD TITLE
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
Spectrometry (DSITMS)
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
Spectrometrv (TE/GC/MS)
CURRENT
PROMUL-
GATED
METHOD
Not Promul-
gated
Not Promul-
gated
8270C
Rev 3
(12/96)
8275A
Rev 1
(12/96)
-------
STATUS TABLE (10/02), 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)
8280
8310
ซ_
FINAL
UP. I
(7/92)
_._
__
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
__
8290
(Up. II)
8315
(Up. II)
8316
(Up. II)
FIN. UP.
Ill (12/96)
IMA (4/98)
8280A
(Up. Ill)
__
__
8315A
(Up. Ill)
PROP.
UP. IIIB
(8/02)
DRAFT
UP. IVA
(1/98)
8280B
8290A
.
DRAFT
UP. IVB
(11/00)
__
OTHER
NEW
SW-846
METHODS
__
__
METHOD TITLE
8280A (Promulgated): The
Analysis of Polychlorinated
Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans by
High Resolution Gas
Chromatography/Low Resolution
Mass Spectrometry (HRGC/LRMS)
8280B (Draft Up. IVA):
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 Chromatoqraphy (HPLC)
CURRENT
PROMUL-
GATED
METHOD
8280A
Rev1
(12/96)
8290
RevO
(9/94)
8310
RevO
(9/86)
831 5A
Rev1
(12/96)
8316
RevO
(9/94)
29
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
MA (8/93)
KB (1/95)
8318
(Up. II)
8321
(Up. II)
8330
(Up. II)
8331
(Up. II)
-
8410
(Up. II)
FIN. UP.
111(12/96)
IIIA (4/98)
-
8321A
(Up. Ill)
8325
(Up. Ill)
-
8332
(Up. Ill)
PROP.
UP. 1MB
(8/02)
-
-
~
DRAFT
UP. IVA
(1/98)
8321 B
8330A
-
-
DRAFT
UP. IVB
(11/00)
831 8A
8321 B
(Replaces
IVA
version)
-
-
OTHER
NEW
SW-846
METHODS
-
-
-
METHOD TITLE
A/-Methylcarbamates by High
Performance Liquid
Chromatography (HPLC)
Solvent-Extractable Nonvolatile
Compounds by High Performance
Liquid Chromatography/
Thermospray/Mass Spectrometry
(HPLC/TS/MS) or Ultraviolet (UV)
Detection
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
Orqanics: Capillary Column
CURRENT
PROMUL-
GATED
METHOD
8318
RevO
(9/94)
8321A
Rev1
(12/96)
8325
RevO
(12/96)
8330
RevO
(9/94)
8331
RevO
(9/94)
8332
RevO
(12/96)
8410
RevO
(9/94)
-------
SW-84HOD STATUS TABLE (10/02), 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
FINAL
UP. 1
(7/92)
-
-
-
~
~
-
-
~
9010A
FIN. UP.
II (9/94)
HA (8/93)
MB (1/95)
-
-
FIN. UP.
111(12/96)
MIA (4/98)
8430
(Up. Ill)
8440
(Up. Ill)
8515
(Up. Ill)
8520
(Up. Ill)
-
9010B
(Up. Ill)
PROP.
UP. IIIB
(8/02)
-
-
-
-
901 OC
DRAFT
UP. IVA
(1/98)
--
-
~
-
-
-
9000
9001
DRAFT
UP. IVB
(11/00)
-
-
8510
-
-
8535
8540
-
~
OTHER
NEW
SW-846
METHODS
-
-
-
-
-
METHOD TITLE
Analysis of Bis(2-chloroethyl) Ether
and Hydrolysis Products by Direct
Aqueous Injection GC/FT-IR
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
CURRENT
PROMUL-
GATED
METHOD
8430
RevO
(12/96)
8440
RevO
(12/96)
Not Promul-
gated
8515
RevO
(12/96)
8520
RevO
(12/96)
Not Promul-
gated
Not Promul-
gated
Not Promul-
gated
Not Promul-
gated
9010B
Rev 2
(12/96)
31
-------
SW-846 METHOD STATUS TABLE (10/02), 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)
9012
-
-
9020
-
9022
--
9030
-
FINAL
UP. I
(7/92)
~
9013
-
9020A
9021
-
-
9030A
9031
FIN. UP.
II (9/94)
MA (8/93)
IIB (1/95)
-
9020B
(Up. II)
-
-
-
-
-
FIN. UP.
Ill (12796)
IMA (4/98)
9012A
(Up. Ill)
-
9014
(Up. Ill)
-
9023
(Up. Ill)
9030B
(Up. Ill)
-
PROP.
UP. 1MB
(8/02)
9012B
-
~
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
-
-
-
-
OTHER
NEW
SW-846
METHODS
-
-
-
METHOD TITLE
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
CURRENT
PROMUL-
GATED
METHOD
9012A
Rev 1
(12/96)
9013
RevO
(7/92)
9014
RevO
(12/96)
9020B
Rev 2
(9/94)
9021
RevO
(7/92)
9022
RevO
(9/86)
9023
RevO
(12/96)
9030B
Rev 2
(12/96)
9031
RevO
(7/92)
-------
HOD STATUS TABLE (10/02), 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)
9035
9036
9038
9040
9041
9045
FINAL
UP. I
(7/92)
-
-
-
-
9041A
9045A
FIN. UP.
II (9/94)
IIA (8/93)
MB (1/95)
-
-
9040A
(Up. II)
9040B
(Up. IIB)
-
9045B
(Up. II)
9045C
(Uo. IIB)
FIN. UP.
111(12/96)
IIIA (4/98)
9034
(Up. Ill)
~
-
~
-
PROP.
UP. IIIB
(8/02)
-
9040C
9045D
DRAFT
UP. IVA
(1/98)
-
-
-
-
DRAFT
UP. IVB
(11/00)
~
-
OTHER
NEW
SW-846
METHODS
-
-
~
-
METHOD TITLE
Titrimetric Procedure for Acid-
Soluble and Acid-Insoluble Sulfides
Sulfate (Colorimetric, Automated,
Chloranilate)
Sulfate (Colorimetric, Automated,
Methylthymol Blue, AA II)
Sulfate (Turbidimetric)
pH Electrometric Measurement
pH Paper Method
Soil and Waste pH
CURRENT
PROMUL-
GATED
METHOD
9034
RevO
(12/96)
9035
RevO
(9/86)
9036
RevO
(9/86)
9038
RevO
(9/86)
9040B
Rev 2
(1/95)
9041 A
Rev1
(7/92)
9045C
Rev 3
(1/95)
33
-------
SW-846 METHOD STATUS TABLE (8/02), 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)
9050
-
9060
9065
9066
9067
FINAL
UP. 1
(7/92)
-
FIN. UP.
II (9/94)
HA (8/93)
MB (1/95)
-
9056
(Up. II)
-
FIN. UP.
111(12/96)
MIA (4/98)
9050A
(Up. Ill)
-
9057
(Up. Ill)
--
-
-
-
PROP.
UP. IIIB
(8/02)
-
-
-
9060A
-
-
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
9056A
9058
-
--
-
OTHER
NEW
SW-846
METHODS
-
-
-
-
-
-
METHOD TITLE
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)
Phenolics (Colorimetric, Automated
4-AAP with Distillation)
Phenolics (Spectrophotometric,
MBTH with Distillation)
CURRENT
PROMUL-
GATED
METHOD
9050A
Rev 1
(12/96)
9056
RevO
(9/94)
9057
RevO
(12/96)
Not Promul-
gated
9060
RevO
(9/86)
9065
RevO
(9/86)
9066
RevO
(9/86)
9067
RevO
(9/86)
-------
SW-sJ-HHJrHOD STATUS TABLE (8/02), 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)
9070
9071
__
FINAL
UP.I
(7/92)
ซ.
__
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
__
9071A
(Up. II)
9075
(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)
PROP.
UP. IIIB
(8/02)
9070A
(Suffix and
title added)
_
_
_
DRAFT
UP. IVA
(1/98)
__
_
9074
..
DRAFT
UP. IVB
(11/00)
ซ
_
_
OTHER
NEW
SW-846
METHODS
ป
_
__
METHOD TITLE
9070 (Final Update IIIA): No title
9070A (Prop. Up. IIIB): n-Hexane
Extractable Material (HEM) for
Aqueous Samples
Text refers reader 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
Spectrometrv (XRF)
CURRENT
PROMUL-
GATED
METHOD
The
current
promul-
gated
version of
Method
16641 is
Rev. A
9071 B
Rev 2
(4/98)
Not Promul-
gated
9075
RevO
(9/94)
1 Method 1664 (EPA Publication No. EPA-821-R-98-002) is available via the Internet at http://www.epa.qov/OST . It is also
available from the National Technical Information Service (NTIS), NTIS Publication No. PB99-121949 (call 703-605-6000 or 800-553-
6847).
35
-------
SW-846 METHOD STATUS TABLE (8/02), 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
FINAL
UP. 1
(7/92)
-
-
-
-
-
9090A
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
9076
(Up. II)
9077
(Up. II)
-
-
-
-
~
~
FIN. UP.
111(12/96)
IIIA (4/98)
-
9078
(Up. Ill)
9079
(Up. Ill)
9095A
(Up. Ill)
PROP.
UP. 1MB
(8/02)
-
-
9095B
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
-
-
-
OTHER
NEW
SW-846
METHODS
-
-
METHOD TITLE
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)
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
CURRENT
PROMUL-
GATED
METHOD
9076
RevO
(9/94)
9077
RevO
(9/94)
9078
RevO
(12/96)
9079
RevO
(12/96)
9080
RevO
(9/86)
9081
RevO
(9/86)
9090A
Rev1
(7/92)
9095A
Rev 1
(12/96)
-------
SW-846 METHOD STATUS TABLE (8/02), 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)
-
9250
9251
9252
FINAL
UP.I
(7/92)
-
-
-
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
-
9252A
(Up. II)
9253
(Up. II)
FIN. UP.
111(12/96)
MIA (4/98)
9213
(Up. Ill)
9214
(Up. Ill)
9215
(Up. Ill)
~
-
Deleted
from
SW-846
(Up. Ill)
PROP.
UP. IIIB
(8/02)
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
9216
-
DRAFT
UP. IVB
(11/00)
-
-
-
-
OTHER
NEW
SW-846
METHODS
-
--
-
METHOD TITLE
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)
Chloride (Colorimetric, Automated
Ferricyanide AAII)
Chloride (Titrimetric, Mercuric
Nitrate)
Chloride (Titrimetric, Silver Nitrate)
CURRENT
PROMUL-
GATED
METHOD
9213
RevO
(12/96)
9214
RevO
(12/96)
9215
RevO
(12/96)
Not Promul-
gated
9250
RevO
(9/86)
9251
RevO
(9/86)
Deleted
from
SW-846
9253
RevO
(9/94)
-------
SW-8= THOD STATUS TABLE (8/02), 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)
-
9100
9131
9132
9200
-
-
~
FINAL
UP. 1
(7/92)
-
-
~
-
-
~
-
FIN. UP.
II (9/94)
I1A (8/93)
IIB (1/95)
9096
(Up. II)
-
-
-
-
-
-
FIN. UP.
111(12/96)
IIIA (4/98)
-
-
-
-
Deleted
from
SW-846
(Up. Ill)
9210
(Up. Ill)
9211
(Up. Ill)
9212
(Up. Ill)
PROP.
UP. IIIB
(8/02)
-
-
-
-
-
-
DRAFT
UP. IVA
(1/98)
-
-
-
-
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
9210A
OTHER
NEW
SW-846
METHODS
-
-
~
-
-
-
METHOD TITLE
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
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
CURRENT
PROMUL-
GATED
METHOD
9096
RevO
(9/94)
9100
RevO
(9/86)
9131
RevO
(9/86)
9132
RevO
(9/86)
Deleted from
SW-846
9210
RevO
(12/96)
9211
RevO
(12/96)
9212
RevO
(12/96)
37
-------
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
Chapter Four -- Organic Analytes
THIRD ED.
(9/86)
/
/
/
/
/
/
/
/
/
FINAL
UP.I
(7/92)
/
/
/
/
/
/
FIN. UP.
II (9/94)
IIA (8/93)
IIB (1/95)
/ (Up. II)
/
(Up. II & IIB)
/ (Up. II)
/ (Up. II)
/ (Up. II)
FINAL UP.
111(12/96)
IMA 4/98)
/ (Up. Ill)
/
(Up. Ill & IMA)
/ (Up. Ill)
/ (Up. Ill)
/(Up. Ill)
/(Up. Ill)
DRAFT
UP. IVA
/
/
/
/
DRAFT
UP. IVB
/
(Replaces
IVA version)
/
(Replaces
IVA version)
/
(Replaces
IVA version)
/
(Replaces
IVA version)
PROP
UP. 1MB
/
CURRENT
FINAL
VERSION
Rev 1
(12/96)
Rev 2
(9/94)
Rev 5
(4/98)
RevO
(9/86)
Rev1
(12/96)
RevO
(9/86)
Rev1
(7/92)
Rev 3
(12/96)
Rev 3
(12/96)
Rev 3
(12/96)
-------
SW-8= THOD STATUS TABLE (8/02), 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)
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)
I1B (1/95)
-
-
-
HCN Test
Method
(Up. II)
H2S Test
Method
(Up. II)
FIN. UP.
111(12/96)
IIIA (4/98)
-
-
-
HCN Test
Method
(Up. Ill)
H2S Test
Method
(Up. Ill)
PROP.
UP. IIIB
(8/02)
-
-
~
Proposed
Removal
from
SW-846
Proposed
Removal
from
SW-846
DRAFT
UP. IVA
(1/98)
-
-
-
DRAFT
UP. IVB
(11/00)
-
-
-
--
OTHER
NEW
SW-846
METHODS
-
-
--
METHOD TITLE
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
CURRENT
PROMUL-
GATED
METHOD
9310
RevO
(9/86)
9315
RevO
(9/86)
9320
RevO
(9/86)
Guidance
Only
Rev 3
(12/96)
Guidance
Only
Rev 3
(12/96)
39
-------
TITLE
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
Appendix - Company References
THIRD ED.
(9/86)
/
/
/
/
/
/
/
/
/
/
FINAL
UP. 1
(7/92)
~
/
~
FIN. 1
II (9/94)
HA (8/93)
IIB (1/95)
/ (Up. II)
/
(Up. II & IIB)
/ (Up. II)
/ (Up. II)
~
FINAL UP.
111(12/96)
IDA 4/98)
/
(Up. Ill & IIIA)
/(Up. Ill)
/ (Up. Ill)
/(Up. Ill)
/(Up. Ill)
DRAFT
UP. IVA
/
DRAFT
UP. IVB
/
(Replaces
IVA version)
/
/
PROP
UP. 1MB
/
/
/
/
CURRENT
FINAL
VERSION
Rev 3
(4/98)
Rev 2
(12/96)
Rev 3
(12/96)
Rev 2
(12/96)
RevO
(9/86)
Rev 2
(12/96)
RevO
(9/86)
RevO
(9/86)
RevO
(9/86)
RevO
(9/86)
41
-------
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
CONTENTS -1 Revision 6
August 2002
-------
Method 3020A:
Method 3031:
Method 3040A:
Method 3050B:
Method 3051:
Method 3052:
Method 3060A:
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
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 7061 A: 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 7131A: 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)
CONTENTS - 2
Revision 6
August 2002
-------
Method 7430:
Method 7450:
Method 7460:
Method 7461:
Method 7470A:
Method 7471A:
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:
7741A:
7742:
7760A:
7761:
7770:
7780:
7840:
7841:
7870:
7910:
7911:
7950:
7951:
Lithium (Atomic Absorption, Direct Aspiration)
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)
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 promulgated revision of the method, even
though the method number does not include the appropriate letter suffix.
CONTENTS - 3
Revision 6
August 2002
-------
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
Method 5021: Volatile Organic Compounds in Soils and Other Solid Matrices Using
Equilibrium Headspace Analysis
Method 5030B: Purge-and-Trap for Aqueous Samples
CONTENTS - 4 Revision 6
August 2002
-------
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, Nonpurgeable, Water-Soluble Compounds by Azeotropic
Distillation
Volatile Organic Compounds by Vacuum Distillation
Closed-System Purge-and-Trapand 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:
Method 8131:
Method 8141 A:
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
Aniline and Selected Derivatives by Gas Chromatography
Organophosphorus Compounds by Gas Chromatography: Capillary
Column Technique
CONTENTS - 5
Revision 6
August 2002
-------
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 Acrolein by High Performance Liquid
Chromatography (HPLC)
Method 8318: N-Methylcarbamates by High Performance Liquid Chromatography
(HPLC)
Method 8321A: Solvent Extractable Nonvolatile Compounds by High Performance
Liquid Chromatography/Thermospray/Mass Spectrometry
(HPLC/TS/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
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
CONTENTS - 6 Revision 6
August 2002
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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-l ,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
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 promulgated revision of the method, even
though the method number does not include the appropriate letter suffix.
CONTENTS - 7 Revision 6
August 2002
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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, AA II)
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 - 8
Revision 6
August 2002
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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 forTotal 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 9041 A:
Method 9045D:
Method 9050A:
Method 9080:
Method 9081:
Method 9090A:
Method 9095B:
Method 9096:
Appendix A:
Method 9100:
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
CONTENTS - 9
Revision 6
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Method 9310: Gross Alpha and Gross Beta
Method 9315: 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 1010A: Pensky-Martens Closed-Cup Method for Determining Ignitability
Method 1020B: Small Scale Closed Cup Method for Determining Ignitability
8.2 Corrosivity
Method 9040C: pH Electrometric Measurement
Method 1110A: Corrosivity Toward Steel
8.3 Reactivity
8.4 Toxicity
Method 131 OB: Extraction Procedure (EP) Toxicity Test Method and Structural
Integrity Test
Method 1311: Toxicity Characteristic Leaching Procedure
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 promulgated revision of the method, even
though the method number does not include the appropriate letter suffix.
CONTENTS-10 Revision
August 2002
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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
Method 0100: Sampling for Formaldehyde and Other Carbonyl Compounds in
Indoor Air
CONTENTS -11 Revision 6
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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 promulgated revision of the method, even
though the method number does not include the appropriate letter suffix.
CONTENTS-12 Revision 6
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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. (Note: 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:
Method 9075:
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, AA II)
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
Test Method for Total Chlorine in New and Used Petroleum
Products by X-Ray Fluorescence Spectrometry (XRF)
FIVE -1
Revision 4
August 2002
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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 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
Revision 4
August 2002
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METHOD 901OC
TOTAL AND AMENABLE CYANIDE: DISTILLATION
1.0 SCOPE AND APPLICATION
1.1 Method 9010 is 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. Method 9010 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 notdetermined 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 ortitrametrically 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 sulfami
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.
9010C-1 Revision 3
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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. 6.8 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 (0.1 N), NaAsO2. Dissolve 3.2 g NaAsO2 in 250 mL water.
5.3.2 Ascorbic acid, C6H8O6.
5.3.3 Sodium hydroxide solution (50%), NaOH. Commercially available.
9010C-2 Revision 3
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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 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 Sulfuricacid(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-Referto Method 9014forthe 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 additional 5 mL of sodium
arsenite solution for each liter of sample. Ascorbic acid can be used as an alternative although it
901OC-3 Revision 3
August 2002
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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 4ฐC.
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.
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.
901OC-4 Revision 3
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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 4ฐC in tightly sealed
flasks.
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 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.
901OC-5 Revision 3
August 2002
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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 CN', the
standard deviations for precision were + 0.005 to + 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.
4. Britton, P.; Winter, J.; Kroner, R.C. "EPAMethod Study 12, Cyanide in Water"; final reportto
the U.S. Environmental Protection Agency. National Technical Information Service: Springfield, VA,
1984; PB80-196674.
901OC-6 Revision 3
August 2002
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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. i 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 Centerfor Environmental Research Information: Cincinnati, OH, 1983; EPA-
600/4-79-020.
11. Rohrbough. 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. 18thed.:Greenberg.A.E.:
Clesceri, L.S.; Eaton, A.D.; Eds.; American Water Works Association, Water Pollution Control
Federation, American Public Health Association: Washington, DC, 1992.
13. Umafia, 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.
901OC-7 Revision 3
August 2002
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FIGURE!
APPARATUS FOR CYANIDE DISTILLATION
Cooling Water
Inlet Tube
Screw Clamp
4
Heater
To Low Vacuum Source
<- Gas Scrubber
Condenser
Distilling Flask
O
901OC-8
Revision 3
August 2002
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FIGURE 2.
APPARATUS FOR CYANIDE DISTILLATION
Connecting Tubing
Allihn Condenser
Air Inlet Tube
One-Liter
Boiling Flask
^ Suction
901OC-9
Revision 3
August 2002
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METHOD 9010C
TOTAL AND AMENABLE CYANIDE: DISTILLATION
7.2.3 Add bismuth Y
nitrnta solttiinn to ^~"
boilincj flask.
7.2.4 Aijr) sulfamic
aci'J Eol'.itinn to ^ Y
hoihnf) flaซ:k. ^
V
7.1 Pretreat sample
to determine
cyanides amenable
to chlorination.
1
7.2.1 Place sample
in round bottom
NaOH solution into
scrubber; construct
distillation
assembly.
1
7.2.2 Turn vacuum
on and adjust
A
/ 7.2.3 Do\.
ฃ!/ samples contains
>v sulfide? /
K Mn
p PJO
/\
es /7-2A N'nrale\
\. samples? /
No
V
P
7.2.5 Add sulfuric
acid; rinse inlet
tube with water;
add magnesium
inlet tube with
water.
1
7.2.6 Boil
solution; reflux;
cool; close vacuum
source.
1 .
7.2.7 Transfer
solution to a
volumetric
flask.
1
7.2.8 Proceed to
determinative
method.
9010C-10
Revision 3
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METHOD 9012B
TOTAL AND AMENABLE CYANIDE (AUTOMATED COLORIMETRIC.
WITH OFF-LINE DISTILLATION)
1.0 SCOPE AND APPLICATION
1.1 Method 9012 is used to determine the concentration of inorganic cyanide (CAS
Registry Number 57-12-5) in wastes or leachate. The 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 Method 9012.
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 pretreatmentwith sulfami
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.
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.
9012B-1 Revision 2
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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 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.
9012B-2 Revision 2
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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 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 Bi(NO)3ป 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 Sulfamicacid (0.4N), H2NSO3H. Dissolve 40 g H2NSO3H in 1 liter of water.
5.5.4 Sulfuricacid(18N), H2SO4. Slowly and carefully add 500 mL of concentrated
H2SO4 to 500 mL of water.
5.5.5 Magnesium chloride solution (2.5M), MgCI2ซ 6H2O. Dissolve 510 g of MgCI2
6H2O in 1 liter of water.
5.5.6 Lead acetate paper.
5.6 Reagents for automated colorimetric determination
9012B-3 Revision 2
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5.6.1 Pyridine-barbituric acid reagent: Place 15 g of barbituric acid in a250-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
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 0.1 N 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 4ฐC.
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.
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
9012B-4 Revision 2
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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 0.1N 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.
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.
9012B-5 Revision 2
August 2002
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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 Heatthe 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.
7.2.6 Transferee solution from the scrubber into a 250-mLvolumetricflask. 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
= 10ugCN-) (ug 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
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).
9012B-6 Revision 2
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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 + 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.
10.0 REFERENCES
1. Annual Book of ASTM Standards, Part 31, "Water," Standard D2036-75, Method B, p. 505
(1976).
9012B-7 Revision 2
August 2002
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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
August 2002
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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
August 2002
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Figure 2. Cyanide Distillation Apparatus
Cooling Water
Inlet Tube
Screw Clamp
Heater
To Low Vacuum Source
<- Gas Scrubber
Condenser
Distilling Flask
O
9012B-10
Revision 2
August 2002
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METHOD 9012B
TOTAL AND AMENABLE CYANIDE (AUTOMATED COLORIMETRIC
WITH OFF-LINE DISTILLATION )
7.1 Pretraat to
determine
cyanides amenable
to chlorination.
7.1.6 Treat
sample by
adding bismuth
nitrate solution.
7.2.1 Placa sample
in flask; pipet
sodium hydroxide
into absorbing
tube.
7.2.2 Introduce
air stream into
boiling flask.
7.2.4 Add
rinse tube with
Type II water
add magnesium
chloride.
I
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.
7.2.3 Add
sulfamic
acid solution
through air
inlet tube.
9012B-12
Revision 2
August 2002
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METHOD 9012B (continued)
7.5.1 Distill
standards in
same manner
as sample.
7.4
Does
sample
contain
sulfide?
7.4.1 Prepare a
series of
CN standards.
7.5.2 Prepare
standard curve
of absorbance.
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.
Stop
J)
9012B-13
Revision 2
August 2002
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METHOD 9060A
TOTAL ORGANIC CARBON
1.0 SCOPE AND APPLICATION
1.1 Method 9060 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 Sections 2.0 and 3.0.
1.2 Method 9060 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 CH 4 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 Method
9060 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.
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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.
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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 (4ฐC) 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 < 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.
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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).
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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.
Stop
J)
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METHOD 9070A
n-HEXANE EXTRACTABLE MATERIAL (HEM) FOR AQUEOUS SAMPLES
See Method 1664, Publication No. EPA-821-R-98-002, for this method procedure.
Revision 1
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CHAPTER SIX
PROPERTIES
This chapter addresses procedures for method-defined parameters, where the analytical
result is wholly dependant on the process used to make the measurement. 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 Chapter Six:
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:
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
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METHOD 9045D
SOIL AND WASTE pH
1.0 SCOPE AND APPLICATION
1.1 Method 9045 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.
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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 25ฐC] is required, the analyst should control
sample temperature at 25ฑ1 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 minutes. 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 hour to allow most of the
suspended clay to settle out from the suspension or filter or centrifuge off the aqueous
phase for pH measurement.
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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 2ฐC 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 minutes. 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 minutes 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 2ฐC 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.
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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.
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METHOD 9045D
SOIL AND WASTE pH
7.1 Calibrate
each instrument/
electrode
system.
7.2.1 Add 20 mL
water to 20 g soil;
stir continuously
for 5 minutes.
7.3.1 Add 20 mL
water to 20 g waste;
stir continuously
for 5 minutes.
7.2.2 Let soil
suspension
stand for 1
hour or filter.
7.3.2 Let waste
suspension
stand for 1 5
minutes or filter.
Repeat experiment
with 20 g waste
and 40 mL water.
Decant oily
phase;
measure pH of
aqueous phase.
Aqueous
Phase
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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
A100-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 overflow 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, 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.
9095B - 3 Revision 2
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FIGURE 1. PAINT FILTER TEST APPARATUS.
RING STAND
/PAINT FILTER
^-FUNNEL
IGRADUATED CYLINDER
3
_e
9095B - 4
Revision 2
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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 4O
CFR 264.314 or
265.314.
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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
This section discusses the hazardous characteristic of ignitability. The regulatory background
of this characteristic is summarized, and the regulatory definition of ignitability is presented. The
two testing methods associated with this characteristic, Methods 1010 and 1020, can be found in
Chapter Eight.
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.
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.
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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.
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
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treatment standard for that waste has not been met, and further treatment is necessary prior to
land disposal.
7.4.2 Summary of Procedure
The TCLP consists of five steps (refer to Figure 3):
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.
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Under the Land Disposal Restrictions regulations, 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 does 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
Tf o-, m-, and p-cresol concentrations cannot be differentiated, the total cresol (D026) concentration is used. The
regulatory level of total cresol is 200 mg/L.
2Quantitation limit is greaterthan the calculated regulatory level. The quantitation limit therefore becomes the regulatory
level.
SEVEN - 5 Revision 4
August 2002
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FIGURES.
TOXICITY CHARACTERISTIC LEACHING PROCEDURE FLOWCHART
Svparat*
I iquxd* from <
0.8 urn glasi
fibซr filter
Discard
lolidi
( START j
1
Ui. *
ub-ปamplซ of
Hill*
1
./What isV
OS* / th. % \ > 0 SX li
\ vast*' / - 0
N. / f,
100%
Eiamin*
./Mutt thซ X. YซB
\ milUd? /
5ซparatป f ^v
quidifram Liquid / \
B urn glat \ /
b.r filt.r \ /
Solid
Eitraet ซ/
appropriate fluid
1) Bottlt utraetor
for non-volatilซs
2) ZHE d.vic. for
vola tiles
Rซducซ
particli size
to <9 5 mm
SEVEN - 6
Revision 4
August 2002
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FIGURE 3 (continued)
Mซa*ure amount of
liquid and analyze
(mathematically
combine result w/
retult of extract
analysi*)
SEVEN - 7
Revision 4
August 2002
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CHAPTER EIGHT
METHODS FOR DETERMINING CHARACTERISTICS
This chapter addresses procedures for 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.
EIGHT -1 Revision 3
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8.1 Ignitability
This chapter addresses procedures for 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. 8.1 of this chapter:
Method 1010A: Pensky-Martens Closed-Cup Method for Determining Ignitability
Method 1020B : Small Scale Closed-Cup Method for Determining Ignitability
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METHOD 101OA
PENSKY-MARTENS CLOSED-CUP METHOD FOR DETERMINING IGNITABILITY
1.0 SCOPE AND APPLICATION
1.1 Method 1010 uses the Pensky-Martens closed-cup tester to determine the flash point
of liquids including those that tend to form a surface film under test conditions. Liquids containing
non-filterable, suspended solids can also be tested using this method.
1.2 This method is one of two method options required by 40 CFR 261.21(a)(1) in the
determination of the hazardous waste ignitability characteristic. Method 1020 is the other method
option.
2.0 SUMMARY OF METHOD
2.1 The sample is heated at a slow, constant rate with continual stirring. A small flame
is directed into the cup at regular intervals with simultaneous interruption of stirring. The flash point
is the lowest temperature at which application of the test flame ignites the vapor above the sample.
2.2 For complete instructions on how to conduct a test by this method, see Reference 4
below, "D 93-99c, Standard Test Methods for Flash-Point by Pensky-Martens Closed Cup Tester."
3.0 METHOD PERFORMANCE
3.1 The Pensky-Martens and Setaflash Closed Testers (Revision 0 of Method 1020) were
evaluated using five industrial waste mixtures and p-xylene. The results of these studies are shown
below in ฐF along with other data. The sample footnote numbers refer to the source documents
identified under Sec. 4.0 of this method.
Sample
12
22
32
42
52
p-xylene2
p-xylene3
Tanker oil
Tanker oil
Tanker oil
DIBK/xylene
Pensky-Martens (ฐF)
143.7 + 1.5
144.7 + 4.5
93.7 + 1.5
198.0 ฑ4.0
119.3 + 3.1
81.3 + 1.1
77.7 + 0.58
125, 135
180, 180
110, 110
102 + 4"
Setaflash (ฐF)
139.3 ฑ2.1
129.7 ฑ0.6
97.7 ฑ1.2
185.3 ฑ0.6
122.7 ฑ2.5
79.3 ฑ 0.6
-
-
107
a12 determinations over five-day period. "75/25 v/v analyzed by four laboratories.
1010A-1 Revision 1
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4.0 REFERENCES
1. D 93-80, Test Methods for Flash Point by Pensky-Martens Closed Tester, American Society
for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103, 04.09. 1986.
2. Umana, M., Gutknecht, W., Salmons, C., et al., Evaluation of Ignitability Methods (Liquids),
EPA/600/S4-85/053, 1985.
3. Gaskill, A., Compilation and Evaluation of RCRA Method Performance Data, Work
Assignment No. 2, EPA Contract No. 68-01-7075, September 1986.
4. D 93-99c, Standard Test Methods for Flash-Point by Pensky-Martens Closed Cup Tester,
originally published by the American Society for Testing and Materials, 100 Barr Harbor Drive, West
Conshohocken, PA 19428. Available from Global Engineering Documents, 15 Iverness Way East,
Englewood, CO 80112, 1-800-854-7179, http://global.ihs.com
1010A-2 Revision 1
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METHOD 1020B
SMALL SCALE CLOSED-CUP METHOD FOR DETERMINING IGNITABILITY
1.0 SCOPE AND APPLICATION
1.1 Method 1020 makes uses the small scale closed-cup apparatus (formerly the Setaflash
closed tester) to determine the flash point of liquids that have flash points between 0ฐ and 110 ฐC
(32 and 230 ฐF) and viscosities lower than 150 stokes at 25 ฐC (77 ฐF).
1.2 The procedure may be used to determine whether a material will or will not flash at a
specified temperature or to determine the finite temperature at which a material will flash.
1.3 This method is one of two method options required in 40 CFR 261.21(a)(1) for the
determination of the hazardous waste ignitability characteristic. Method 1010 (Pensky-Martens
Closed-Cup Method for Determining Ignitability) is the other method option. Liquids that tend to
form surface films under test conditions or those that contain non-filterable suspended solids
should be tested for the hazardous waste ignitability characteristic using Method 1010.
2.0 SUMMARY OF METHOD
2.1 By means of a syringe, 2-mL of sample is introduced through a leak-proof entry port
into the tightly closed small scale tester or directly into the cup which has been brought to within
3 ฐC (5 ฐF) below the expected flash point.
2.2 As a flash/no-flash test, the expected flash-point temperature may be a specification
(e.g., 60 ฐC). For specification testing, the temperature of the apparatus is raised to the precise
temperature of the specification flash point by slight adjustment of the temperature dial. After 1
minute, a test flame is applied inside the cup and note is taken as to whether the test sample
flashes or not. If a repeat test is necessary, a fresh sample should be used.
2.3 For a finite flash management, the temperature is sequentially increased through the
anticipated range, the test flame being applied at 5 ฐC (9 ฐF) intervals until a flash is observed. A
repeat determination is then made using a fresh sample, starting the test at the temperature of the
last interval before the flash point of the material and making tests at increasing 0.5ฐC (1ฐF)
intervals.
2.4 For the complete instructions on how to conduct the ignitability test by this method, see
Reference 4 below, "D 3278-96, Standard Test Methods for Flash Point of Liquids by Small Scale
Closed-Cup Apparatus."
3.0 METHOD PERFORMANCE
See Method 1010.
4.0 REFERENCES
1. D 3278-78, Test Method for Flash Point of Liquids by Setaflash Closed Tester, American
Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103.
1020B-1 Revision 2
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2. Umana, M., Gutknecht, W., Salmons, C., et al., Evaluation of Ignitability Methods (Liquids),
EPA/600/S4-85/053, 1985.
3. Gaskill, A., Compilation and Evaluation of RCRA Method Performance Data, Work
Assignment No. 2, EPA Contract No. 68-01-7075, September 1986.
4. D 3278-96, Standard Test Methods for Flash Point of Liquids by Small Scale Closed-Cup
Apparatus, American Society for Testing and Materials, 100 Barr Harbor Drive, West
Conshohocken, PA. http//www.astm.org/. Also available from Global Engineering Documents, 15
Iverness Way East, Englewood, CO 80112, 1-800-854-7179, http://global.ihs.com.
1020B-2 Revision 2
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8.2 Corrosivity
This chapter addresses procedures for 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 Method 9040 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.
9040C -1 Revision 3
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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 characteri-zation, 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 25ฑ1 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.
9040C - 2 Revision 3
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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 2ฐC 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:
Accuracy as
Standard Deviation Bias Bias
pH Units pH Units % pH Units
3.5 0.10 -0.29 -0.01
3.5 0.11 -0.00
7.1 0.20 +1.01 +0.07
7.2 0.18 -0.03 -0.002
8.0 0.13 -0.12 -0.01
8.0 0.12 +0.16 +0.01
10.0 REFERENCES
1. National Bureau of Standards, Standard Reference Material Catalog 1986-87, Special
Publication 260.
9040C - 3 Revision 3
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METHOD 9040C
pH ELECTROMETRIC MEASUREMENT
Start
7.1
Calibrate pH
meter.
7 .2 Place sample
or buffer solution
in alass beake'
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.
9040C - 4
Revision 3
August 2002
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METHOD 1110A
CORROSIVITY TOWARD STEEL
1.0 SCOPE AND APPLICATION
1.1 Method 1110 is used to measure 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. 1 25 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:
A =
- cf2)
1110A-1 Revision 1
August 2002
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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 ฑ1% 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%): Dissolve200gNaOHin800mLTypellwaterand
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 Paragraph 4.0, above.
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 55ฐC (130ฐF).
1110A 2 Revision 1
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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
Soakinq Time
5 min
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: 50 g/L H2SO4
Anode: Carbon or lead
Cathode: Steel coupon
Cathode current density: 20 amp/cm2 (129 amp/in.2)
Inhibitor: 2 cc organic inhibitor/liter
Temperature: 74ฐC (165ฐF)
Exposure Period: 3 min.
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.
1110A-3 Revision 1
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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:
Corrosion Rate (mmpy) =
area x time
where: weight loss is in milligrams,
area is in square centimeters,
time is in hours, 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
Revision 1
August 2002
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METHOD 1110
CORROSIVITY TOWARD STEEL
Q Start J
I
7.1 Assemble
test apparatus.
I
0
1
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.
7.8 Determine
corrosion rate.
7.4 Heat.
1110A-6
Revision 1
August 2002
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8.3 Reactivity
There are no required SW-846 methods for the determination of the characteristic of
reactivity.
EIGHT - 4 Revision 3
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8.4 Toxicity
This chapter addresses procedures for 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. 8.4 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) TOXICITY TEST 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+ 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 1-3 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
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.
1310B-1 Revision 2
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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.
6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6.1 Preservatives must not be added to samples.
131 OB-2 Revision 2
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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 + 0.01 g. Handle
membrane and prefilters with blunt curved-tip forceps or vacuum tweezers, or by applying suction
with a pi pet.
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
+ 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:
weight of filtered solid and filters - tared weight of filters
initial weight of waste material
x100= % solids
1310B-3 Revision 2
August 2002
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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 80ฐC. 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 = W, - 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.
7.12 Place the appropriate amount of material (refer to Step 7.11) into the extractor and add
16 times its weight with water.
131 OB-4 Revision 2
August 2002
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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+ 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 at20-40ฐC (68-104ฐF) 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 + 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 + 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:
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).
131 OB-5 Revision 2
August 2002
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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) + (1,000* 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.
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).
131 OB-6 Revision 2
August 2002
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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
August 2002
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TABLE 1. ERA-APPROVED FILTER HOLDERS
Manufacturer
Size
Model No.
Comments
Vacuum Filters
Gelman
Nalgene
Nuclepore
Millipore
Pressure Filters
Nuclepore
Micro Filtration
Systems
Millipore
47 mm
500 mL
47 mm
47 mm
4011
44-0045
410400
XX1004700
142 mm 425900
142mm 302300
142 mm YT30 142 HW
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
August 2002
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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,
HAWP14250
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,
FHLP14250
83485-02,
83486-02
Susceptible to decomposition by certain polar organic solvents.
1310B-9
Revision 2
August 2002
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TABLE 3. PRECISIONS OF EXTRACTION-ANALYSIS
PROCEDURES FOR SEVERAL ELEMENTS
Element
Arsenic
Sample Matrix
1 . Auto Fluff
2. Barrel sludge
3. Lumber treatment
company sediment
Analysis Method
7060
7060
7060
Laboratory
Replicates
1.8, 1.5ug/L
0.9, 2.6 Mg/L
28, 42 mg/L
Barium
1. Lead smelting emission
control dust
2. Auto Fluff
3. Barrel Sludge
6010
7081
7081
0.12, 0.1 2 mg/L
791 ,780
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
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
7191
7191
7191
7191
61, 43
0.81, 0.89 mg/L
Mercury
1. Barrel sludge
2. Wastewater treatment
sludge from electroplating
3. Lead smelting emission
control dust
7470
7470
7470
0.15, 0.09
1.4, 0.4
0.4, 0.4
1310B-10
Revision 2
August 2002
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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, 1490ug/L
1000, 974 pg/L
2550, 2800 ug/L
31,29ug/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
August 2002
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FIGURE!
EXTRACTOR
5.0
-O
4.0
Non-Clogging Support Bushing
1 Inch Blade at 30ฐ to Horizontal
i\
9.0
1310B-12
Revision 2
August 2002
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FIGURE 2.
ROTARY EXTRACTOR
1310B-13
Revision 2
August 2002
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FIGURES.
EPRI EXTRACTOR
l-Gallon PUslic
or Glass Bottle
Foam Bonded to Cover
Box Assembly
Plywood Construction
Totally Endoted
Fan Cooled Motor
30 rpo, 1/8 HP
1310B-14
Revision 2
August 2002
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FIGURE 4.
COMPACTION TESTER
cm
Combined Weight
0.33 kg (0.73 !b)
3.15cm
(1-25*)
/
Sample
Elastomcric
JB
Y 7/H
Sample Holder
7.1 cm
(2.8-)
9.4 on
1310B-15
Revision 2
August 2002
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METHOD 131 OB
EXTRACTION PROCEDURE (EP) TOXICITY TEST METHOD
AND STRUCTURAL INTEGRITY TEST
7 1 W.igh filter
rr>*mbran* and
prซfiltซr
7 2 Aปiซmblซ fill.r
holder . r*iปmbrซnปj ,
and pr*fi.;tซrป
7 3 Htigh out
biantpl* of %* tซ
1 4 let >olid phaiซ
* t'. 1 * ; cantrxfug*
if nซcซisary
? 5 Fi\\rnt out
11quid phaปซ and
rcfrigvrat* i*.
7 6 MซLgh wet ปo1id
7 7 1 Dry flH.r
and weigh
7 7 2 Calculate
cปrcซnt as1idป
1310B-16
Revision 2
August 2002
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METHOD 131 OB
(Continued)
Area >
3 1 cm2/g
or p*ปปซป
through
9 S rrm
leve
7
8 Discard sol ids
? 10 1 Cut or east
cylinder from wซ*ti
malarial for
5lructural
Integrity Prec*duri
7 10 2 Ai.ซnbU
tปป tซ r ; drop harrmvr
IS timซป
7 9 Prepare
ma tena 1 for
extraction fay
cruปhing. cutting.
or gr meing
material , ซeign
transfer *.o
eitt ractor
lid
1310B-17
Revision 2
August 2002
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METHOD 1310B
(Continued)
7 15 Allow > 1 urn**
to * tand tet up
filter apparatu*;
filt*r
1 11 Calculate
amount of liquid
and acid to uie for
mm tract*on
*.12 Place material
into extractor; add
deionized wa I e r
7 11 Uปe IOC 9
material for
M t raction
procedure
7 16 Combine
1iquid* f r on
Sectioni 7 5 *nd
7 . IS to ana 1yxe for
contaminant*
7 13 Agitate for 24
hour* and monitor
pH of >oiution
? i? Obtain
analyticai method
from Chapter* 3 and
A
7 13 Calibrate and
adjust pH meter
7 18 Compare
ex t ract
concentration to
max inure
contamina tior.
limit* to determine
CP loปicaty
714 At end of
extraction period,
add deionixed wate
STOP
1310B-18
Revision 2
August 2002
! U. S. G. P. O. 2002-493-658/70114
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