California Code of Regulations › Title 22 - Social Security › Division 4.5 - Environmental Health Standards for the Management of Hazardous Waste › Chapter 11 - Identification and Listing of Hazardous Waste › Appendix II - Waste Extraction Test (Wet) Procedures

Current through Register 2024 Notice Reg. No. 28, July 12, 2024
(a) The Waste Extraction Test (WET) described in this
				  appendix shall be used to determine the amount of extractable substance in a
				  waste or other material as set forth in section
				  66261.24(a)(2).
(b) Except as provided in subdivision (d) of this appendix,
				  the WET shall be carried out if the total concentration in the waste, or other
				  material, of any substance listed in section
				  66261.24(a)(2)
				  equals or exceeds the STLC value, but does not exceed the TTLC value, given for
				  that substance. The total concentrations of substances listed in section
				  66261.24(a)(2)
				  shall be determined by analysis of samples of wastes, or other materials, which
				  have been prepared, or meet the conditions, for analysis as set forth in
				  subdivisions (c) and (d) of this appendix. Methods used for analysis for total
				  concentrations of substances listed in section
				  66261.24(a)(2)
				  shall be those given in the following documents or alternate methods that have
				  been approved by the Department pursuant to section
				  66260.21:
(1) for metal elements and their compounds, the waste shall
				  be digested according to the indicated methods described in "Test Methods for
				  Evaluating Solid Waste, Physical/Chemical Methods," SW-846, 2nd edition, U.S.
				  Environmental Protection Agency, 1982 (incorporated by reference, see section
				  66260.11):
(A) all listed metal elements and their compounds, except
				  hexavalent chromium: Method 3050;
(B) hexavalent chromium: Method 3060;
(2) for all substances listed in section
				  66261.24(a)(2),
				  except organic lead compounds, the methods and references in which the methods
				  can be found are listed in Appendix III, Table 4 of this chapter;
(3) the method used for analysis of organic lead compounds is
				  given in Appendix XI of this chapter.
(c) Samples shall be prepared for analysis for total and
				  extractable content of substances listed in section
				  66261.24(a)(2)(A)
				  and for extractable content of substances listed in section
				  66261.24(a)(2)(B)
				  as follows:
(1) Type i: if the waste or other material is a millable
				  solid, the sample shall be passed directly, or shall be milled to pass, through
				  a No. 10 (two millimeter) standard sieve before it is analyzed. If the sample
				  contains non-friable solid particles which do not pass directly through a No.
				  10 sieve and which are extraneous and irrelevant as hazardous constituents to
				  the waste or other material, they shall be removed to the extent feasible by
				  mechanical means and discarded. Solids which remain in the waste or other
				  material after removal of the aforesaid extraneous particles shall be milled to
				  pass through a No. 10 sieve and shall then be combined and mixed well with the
				  solids which passed through the sieve without milling. The reconstituted sample
				  shall then be analyzed as prescribed in this appendix;
(2) Type ii: if the waste or other material is a filterable
				  mixture of liquid and solids in which the solids constitute five-tenths (0.5)
				  percent by weight or greater of the sample, the liquid and solids shall be
				  separated by filtration through a 0.45 micron membrane filter. The filtrate so
				  obtained is to be designated as Initial Filtrate. Its volume is determined, and
				  it is retained. The separated solids shall be sieved in a No. 10 sieve and any
				  nonfriable extraneous particles of the kinds described in subdivision (c)(1) of
				  this appendix which do not pass through the sieve shall be removed to the
				  extent feasible by mechanical means and discarded. The solids which remain
				  after removal of the extraneous particles shall be milled to pass through a No.
				  10 sieve and shall be recombined with solids which passed through the sieve
				  without milling. This recombined solid material shall be extracted following
				  the procedure in subdivision (g) of this appendix. A ratio of 10 milliliters of
				  extraction solution per gram of solid shall be utilized with appropriate
				  modifications for extraction vessel size. After completion of solids
				  extraction, the filtered extractant is combined with Initial Filtrate, mixed
				  thoroughly and analyzed as described in subdivision (g)(3) of this
				  appendix;
(3) Type iii: if the waste or other material is a
				  nonfilterable and nonmillable sludge, slurry, or oily, tarry or resinous
				  material, it shall be analyzed as received unless it contains non-friable
				  extraneous and irrelevant solid particles of the kinds described in subdivision
				  (c)(1) of this appendix. If it contains such solid particles and they are of
				  such size as not to pass through a No. 10 sieve, they shall be removed to the
				  extent feasible by mechanical means and discarded. The remainder of the sample
				  shall be analyzed as prescribed in this appendix;
(4) if it is necessary to dry a solid sample or the solids
				  fraction of a sample before sieving, milling or removal of extraneous solids,
				  or if a sample is dried prior to analysis, all weight losses due to drying
				  shall be determined, and these losses and the conditions of drying shall be
				  reported.
(d) Samples shall be prepared for analysis for total content
				  of substances listed in section
				  66261.24(a)(2)(B)
				  as follows:
(1) type i: if the waste or other material is a millable
				  solid, the sample shall be passed directly, or shall be milled to pass, through
				  a one-millimeter standard sieve before it is analyzed. If the sample contains
				  non-friable solid particles which do not pass directly through a one-millimeter
				  sieve and which are extraneous and irrelevant as hazardous constituents to the
				  waste or other material, they shall be removed to the extent feasible by
				  mechanical means and discarded. Solids which remain in the waste or other
				  material after removal of the aforesaid extraneous particles shall be milled to
				  pass through a one-millimeter sieve and shall then be combined and mixed well
				  with the solids which passed through the sieve without milling. The
				  reconstituted sample shall then be analyzed as prescribed in this
				  appendix;
(2) type ii: if the waste or other material is a filterable
				  mixture of liquid and solids in which the solids constitute five-tenths (0.5)
				  percent by weight or greater of the sample, the liquid and solids shall be
				  separated by filtration through a 0.45 micron membrane filter. The filtrate so
				  obtained is to be designated as Initial Filtrate. Its volume is determined, and
				  it is retained. The separated solids shall be sieved in a one-millimeter sieve
				  and any nonfriable extraneous particles of the kinds described in subdivision
				  (d)(1) of this appendix which do not pass through the sieve shall be removed to
				  the extent feasible by mechanical means and discarded. The solids which remain
				  after removal of the extraneous particles shall be milled to pass through a
				  one-millimeter sieve and shall be recombined with solids which passed through
				  the sieve without milling. This recombined solid material shall be extracted
				  following the procedure in subdivision (g) of this appendix. A ratio of 10
				  milliliters of extraction solution per gram of solid shall be utilized with
				  appropriate modifications for extraction vessel size. After completion of
				  solids extraction, the filtered extractant is combined with Initial Filtrate,
				  mixed thoroughly and analyzed as described in subdivision (9)(3) of this
				  appendix;
(3) type iii: if the waste or other material is a
				  nonfilterable and nonmillable sludge, slurry, or oily, tarry or resinous
				  material, it shall be analyzed as received unless it contains non-friable
				  extraneous and irrelevant solid particles of the kinds described in subdivision
				  (d)(1) of this appendix. If it contains such solid particles and they are of
				  such size as not to pass through a one-millimeter sieve, they shall be removed
				  to the extent feasible by mechanical means and discarded. The remainder of the
				  sample shall be analyzed as prescribed in this appendix;
(4) if it is necessary to dry a solid sample or the solids
				  fraction of a sample before sieving, milling or removal of extraneous solids,
				  or if a sample is dried prior to analysis, all weight losses due to drying
				  shall be determined, and these losses and the conditions of drying shall be
				  reported.
(e) If the waste or other material is a liquid containing
				  less than five-tenths (0.5) percent by weight of undissolved solids, it shall
				  not be subject to the WET procedure, but shall be analyzed directly for the
				  substances listed in section
				  66261.24(a)(2).
				  The waste shall be classified as a hazardous waste if the total concentration
				  in the waste of any substances listed in section
				  66261.24(a)(2)
				  exceeds the TTLC value given for that substance. If, however, the total
				  concentration is less than the TTLC but exceeds the STLC when expressed on a
				  milligrams per liter basis, the waste or other material shall be filtered
				  through a 0.45 micron membrane filter, the solids discarded and the filtrate
				  shall be analyzed directly for the substances listed in section
				  66261.24(a)(2).
				  The waste shall be classified as a hazardous waste if the concentration in the
				  filtrate of any of the substances listed in section
				  66261.24(a)(2)
				  exceeds the STLC value given for that substance.
(f) The WET extraction solution shall consist of 0.2 M sodium
				  citrate at pH 5.0 + 0.1, which is prepared by titrating an appropriate amount
				  of analytical grade citric acid in deionized water with 4.0 N NaOH, except that
				  the extraction solution for the determination of chromium (VI) shall consist of
				  deionized water.
(g) The extraction procedure shall be as follows:
(1) fifty grams of sample, or less if it is a type ii sample
				  prepared pursuant to subdivision (c)(2) or (d)(2) of this appendix, obtained
				  pursuant to subdivision (c), (d), or (e) of this appendix shall be placed in a
				  clean polyethylene or glass container designated the Treatment, capable of
				  physically withstanding the extraction procedure and which was rinsed
				  previously with, in succession, an aqueous 1:1 ratio by volume nitric acid
				  solution and deionized water. If the extract will be analyzed for any of the
				  organic substances listed in section
				  66261.24(a)(2), a
				  glass container shall be used. Furthermore, a container of the same size, shape
				  and material shall be used for an extraction designated as the Blank, which
				  shall be carried through the same procedure as the Treatment, but without
				  addition of the sample;
(2) five hundred milliliters of extraction solution, or less
				  if the waste sample is a type ii sample prepared pursuant to subdivision (c)(2)
				  or (d)(2) of this appendix, shall be added to the Treatment and Blank
				  containers, which shall be then fitted with covered air scrubbers extended well
				  into the extraction solutions and flushed vigorously with nitrogen gas for 15
				  minutes so as to remove and exclude atmospheric oxygen from the extraction
				  medium. If the sample is to be analyzed for any volatile substance, such as
				  trichloroethylene, the sample shall be added after deaeration with nitrogen to
				  avoid volatilization loss. After deaeration the containers shall be quickly
				  sealed with tightly fitting caps and agitated, using a table shaker, an
				  overhead stirrer or a rotary extractor, operated at a speed which shall
				  maintain the sample in a state of vigorously agitated suspension. Required
				  equipment is described in test method 1310 in "Test Methods for Evaluating
				  Solid Waste, Physical/Chemical Methods," SW-846, 3rd edition, U.S.
				  Environmental Protection Agency, 1986 (incorporated by reference, see section
				  66260.11). The temperature during
				  the extraction shall be maintained between 20 and 40 degrees centigrade. After
				  48 hours of extracting, the contents of the Treatment and Blank containers
				  shall be either filtered directly or centrifuged and then filtered. Filtering
				  shall be through a medium porosity prefilter and then through a 0.45 micron
				  membrane filter, using a clean, thick-walled suction flask. For coarser solids,
				  prefiltration shall not be necessary. Pressure filtration shall be an optional
				  alternative to vacuum filtration. If the extracts are first centrifuged, glass
				  or polyethylene bottles shall be used as prescribed for extraction. For very
				  fine solids, centrifuging at as high as 10,000 X G may be necessary. After
				  centrifugation, the liquids shall be decanted, prefiltered if necessary, and
				  then passed through a 0.45 micron membrane filter. All filters shall be of low
				  and identified extractable heavy metals, fluoride and organic chemicals
				  content;
(3) if the filtered extracts are to be analyzed only for the
				  metal elements listed in section
				  66261.24(a)(2)(A),
				  the filtered extracts from the Treatment and Blank shall be transferred to
				  clean polyethylene bottles and acidified with nitric acid to five percent by
				  volume acid content soon after each extract is filtered. For those wastes or
				  waste materials classified under subdivision (c)(2) or (d)(2) of this appendix,
				  the Treatment shall be the Initial Filtrate combined with the extract generated
				  by the WET extraction of the initially separated solids. Similarly the Blank in
				  this instance shall be the filtrate generated by the WET Blank accompanying the
				  initially separated solids, to which is subsequently added a volume of
				  deionized water equivalent to that of the Initial Filtrate. These procedures
				  shall be followed prior to acidification of Treatment and Blank solutions with
				  nitric acid to five percent (by volume) acid content. The bottle shall then be
				  stored at room temperature or frozen. If the extracts are also to be analyzed
				  for the organic substances listed in section
				  66261.24(a)(2)(B),
				  or for the organic substances only, the filtered extracts shall be transferred
				  to clean glass bottles. If the extracts are to be analyzed for fluoride, they
				  shall be transferred to clean polyethylene bottles. These extracts, containing
				  organic substances or flouride, shall not be acidified, but shall be frozen
				  soon after each extract is obtained and held frozen until the day of analysis,
				  unless the extracts are analyzed within 24 hours.
(h) Sample analysis and data treatment shall be as
				  follows:
(1) each of the filtered extracts from the Treatment and
				  Blank extractions shall have been acidified to five percent by volume nitric
				  acid, and stored at room temperature or frozen in polyethylene bottles or kept
				  frozen without addition of acid in glass bottles until the day of analysis, as
				  prescribed. Each of the extracts shall be thoroughly mixed just prior to being
				  individually analyzed for the substances listed in section
				  66261.24(a)(2) in
				  order to determine whether the extractable concentration (EC) in the waste or
				  other material exceeds the STLC for any of the substances listed. The extracts
				  shall be analyzed according to the procedures identified in subdivisions (b)(2)
				  and (b)(3) of this appendix;
(2) the net EC of a substance in the Treatment sample which
				  is listed in section
				  66261.24(a)(2)
				  shall be calculated and reported as milligrams per liter of sample (mg/l). This
				  value is derived after subtracting the concentration of the substance in the
				  appropriate Blank extract from that concentration determined in the Treatment
				  extract.
1. New section
				  filed 5-24-91; effective 7-1-91 (Register 91, No.
				  22).
Note: Authority cited: Sections
					 208
					 and
					 25141,
					 Health and Safety Code. Reference: Section
					 25141,
					 Health and Safety Code.