Friday . '
June -20, 1S90
•EriVlronixtiehiat' :,', ;• ,
Protecttori' :
40 CFR Parts 261, 264r 265, 260, 271 and
• 3G2, ; •: ,' ;. -.-:..;.; ;;: -; ;'-;•.•-•-;;' •'•>--'•,-• -• ••"'"•
Hazardous Waste Management System;
Identification and ysting of ^Haiardbus
Waste; Texiclty Characteristic Revisions;
Finai ' '"
-------
26086
"'< ' - ,- ' ' *
Federal Register / Vol! 55. No. 126 / Friday, June 29, 1990'JRules ^ and|tRegulation^
ENVIRONMENTAL PROTECTION
AGENCY
40 CFR Parts 261,264,265,268,271
and 302
ISWH-FRL-3792-2; EPA/OSW-FR-90-014]
RIM 2050-AA78
Hazardous Waste Management
System; Identification and Listing of
Hazardous Waste; Toxlclty
Characteristic Revisions
AGENCY: Environmental Protection
Agency.
ACTION; Final rule; corrections.
SUMMARY: On March 29,1990 (55 FR
11798), the Environment! Protection
Agency (EPA) promulgated a rule to
revise the existing toxicity
characteristics, which are used to
identify those wastes which are
hazardous and thus subject to regulation
under subtitle C of the Resource
Conservation and Recovery Act (RCRA)
due to their potential to leach significant
concentrations of specific toxic
constituents. Since promulgation, the
Agency has found the need to make
corrections to the rule in order to ensure
consistency of the toxicity characteristic
leaching procedure (TCLP), Method
1311, with other methods contained in
Test Methods for Evaluating Solid
Waste (Physical/Chemical Methods),
SW-848 and to clarify the section on
quality assurance. This notice also
corrects several errors in the March 29,
1990 notice.
DATES: Effective date: September 25,
1990, The effective date and compliance
dates are not changed by this document.
FOB FURTHER INFORMATION CONTACT:
For general information about this
notice, contact the RCRA/Superfund
Hotline at (800) 424-9346 (toll free) or
(202) 382-3000 in the Washington, DC
metropolitan area. For information on
specific aspects of this notice, contact
Steve Cochran, Office of Solid Waste
(OS-332), U.S. Environmental Protection
Agency, 401M Street SW, Washington,
DC 20400. (202) 475-8551.
I. SUPPLEMENTARY INFORMATION:
A. Background
On March 29,1990 (55 FR 11798), EPA
promulgated a rale to revise the existing
toxicity characteristics, which are used
to identify those wastes which are
hazardous and thus subject to regulation
under subtitle C of RCRA. The rule
broadened and refined the scope of the
hazardous waste regulatory program
and fulfilled specific statutory mandates
under the Hazardous and Solid Waste
Amendments of 1984.
Today's notice makes corrections to
appendix II of the regulatory language of
the March 29,1990 final rule, Method
1311, the TCLP. The method has been
reorganized to correspond to the current
version of Test Methods for Evaluating
Solid Waste (Chemical/Physical
Methods), SW-848. In addition, the
quality assurance section has been
renumbered and has been clarified to
eliminate confusion. Today's notice also
corrects several typographical errors
and other omissions that appeared in
the final rule revising the toxicity
characteristics.
The preamble to the March 29,1990
final rule stated that any person that
would like to use the TCLP before the
effective date of the rule (September 25,
1990) may do so in order to determine
whether the eight heavy metals and six
pesticides that are currently regulated
under the Extraction Procedure (EP)
Toxicity Characteristic leach at levels of
regulatory concern. This language was
included because the TCLP is required -
for both waste determination (on
September 25,1990, the TC effective
date) and the land disposal restrictions
program. The Agency today is clarifying
• that, while it is appropriate to use just
one leach test to fulfill both
requirements, persons that would like to
continue using the EP leach test until the
effective date of the TC rule may do so.
It should be noted, however, that the EP
test may still be required as a matter of
state law, and this regulation does not
affect such state law requirements.
B. Method 1311 and Quality Assurance
Today's notice makes technical
corrections to mistakes made in Method
1311, and to errors made during
typesetting, and provides clarifications
. to specific procedures of the method.
The method also is being reorganized by
placing the leaching procedure in one
section and the quality assurance in a
separate section to conform with the
format used in SW-846.
A correction is being made in the
calculation for the weight of waste to
charge the Zero-Headspace Extractor
(ZHE). In the final rule published March
29,1990, the method incorrectly stated
that the optimum sample size to charge
into the ZHE should be determined for
wastes containing >0.5% solids. This
calculation results in'a charge sample
greater than the capacity of the ZHE.
The Agency today is correcting the
procedure to require a determination on
wastes containing > 5% solids. The
sample holding times and errors made
during typesetting are also being
corrected by today's notice.
The Agency received inquiries
indicating that confusion exists
concerning correction factors and how
they should be applied. Therefore, the
Agency is making a technical correction
in § 8.2.5 of Method 1311, published in
today's notice, by adding a formula for
correcting measured values for
analytical bias. Also, inquiries indicate
that EPA's discussion of the appropriate
GC and GC/MS methods to be used was
improper. The preamble language is
corrected by today's notice to indicate
the appropriate GC and GC/MS
methods to be used.
Method 1311 is also being reorganized
by today's notice by placing the leaching
procedure itself in one section, 7.0. (The
steps of the leaching procedure were
previously presented in sections 7, 8,
and 9 in the March 29,1990 final rule.) In
addition, this notice makes minor
corrections to the quality assurance
section and it is renumbered 8.0. This
reorganization provides consistency
with SW-846.
Appendix II, Method 1311 of the
March 29,1990 final rule is replaced in
its entirety by Method 1311 of this notice
in order to incorporate the corrections,
reorganizations, and clarifications
which are being made by .today's notice.
The March 29,1990 final rule provided
an exclusion under 40 CFR 261.4 for
petroleum-contaminated media and
debris that fail the Toxicity
Characteristic. This exclusion applies
only to petroleum-contaminated media
and debris which exhibit the TC for any
one or more of the newly identified
organic constituents, and which are
subject to corrective action under part"
280. The regulatory language of this
exclusion in the final rule is revised by
today's notice to correctly reflect this
application.
C. Corrections *
1. On page 11798, column one, under
"DATES," in the second line of the
compliance dates paragraph, change
"generators: September 25,1990. Small"
to "generators and treatment, storage,
and disposal facilities (TSDFs):
September 25,1990. Small".
2. On page 11804, Table II.2—Toxicity
Characteristics Constitutents and
Regulatory Levels, change the column
heading "Constituent (mg/L)" to
"Constituent".
3. On page 11804, Table H.2—Toxicity
Characteristic Constituents and
Regulatory Levels, line twenty, change
"Heptachlor (and its hydroxide)" to
"Heptachlor (and its epoxide)".
4. On page 11815, column three, Table
C-l—Chronic Toxicity Reference
Levels, lines nineteen and twenty,
change "Heptachlor (and its hydroxide)"
to "Heptachlor (and its epoxide)".
-------
5. On page 11825, column one, fourth
;bullet, first line, change "The data
extracted from RFSs" to "The data. '*
extracted from RFAs".
6^ On page 11829, columns one,7 the
first Ml paragraph (lines twenty-four)
through thirty-six) is replaced by the
following: "The Agency agrees that the
GC method (Method 8040) or the GC/MS
method (Method 8270) for phenols and
the GG/Mectron Capture Detection
(GG/ECD) for paenoxyacid herbicides'
(Method 8150) are more advantageous
for the analysis of these analytes
because the equipment is more readily
available than the HPLC, despite, the
associated difficulties. HPLC methods '_,,
for phenol and phenoxyacid herbicides,
are not included in the third edition of
SW^846 because of a lack of validation
'data. The Agency will allow only the
use of the previously mentioned GC and
GG/MS methods (Methods 8040 or 8270)
or their equivalents for phenols and
Method 8150 for phenoxyacid herbicides
until such time that the Agency proposes
an HPLC method." . ;,
7,. On page 11831, column two,
paragraph b, seventh line, change "rule
of 40 CFR 262.3(a)(2)(iv) oEthe" to "role
of 40 CFR 261.3(a3(2)fiv) or the".
8. On page 11335, column one, first
and second line, change "July 25,1985"
to "July 15,1985".
9. On page Il837v column one, third
complete paragraph, thirteenth line,
change "for TSDFs on February 5,1987
(53 FR." to "for TSDFs on February 5,
1987(52FR",-:
10. On page 11840, column three, first
bullet of second complete paragraph,
first/line! change "Solid waste thai is a
hazardous waste" to "Used oil that is a
hazardous Waste".
11. On page 11844, Table IV-1,—TC
Constituent and Regulatory Levels
Proposed June 13,1986—Continued,
fourth line, change the CASNQ for D034
from "76-44-2" to "76-44-8".
12. On page 11844, Table IV-1.—TC
Constituent and Regulatory Levels
Proposed June 13,1988—Continued, line
twenty-one,.change to read as follows:.
D045. . . . 1,1,1,2-Tetrachloroethane
.... 630-20-8. . . .10.0.
13. On page 11844, column two, Table
IV-2.—Organic Constituents, fourth line,
change the CASNO for D021 from "1Q6-
80-7" to ",108-93-7".
14. On page 11S44, column three,
Table IV-2.-!-Organic Constituents-
Continued, first line, change "DG31. . . .
Heptachlor (and ita hydroxide).... 76-
44-2" to "D031.... Heptachlor (and its
epoxide)... .76-44-8".
15. On page 11846, Table IV-3—
Toxicity Characteristic Constituents and
Regulatory Levels—Continued, tenth
line, change "Heptachlor (and its
hydroxide)" to "Heptachlor (and its
epoxidej". -•• '- ; : . •
.18. Also on page 11846, column two,
third line, change "270 of chapter 40." to
"270 of title 40.".
PART 261— [AMENDED] : " ;". --." ' : .
;;§ 261.4
17. On page 11882, column two, in
§ 281.4 paragraph (b)(10), is corrected to'
read as follows: '.>--'- '-" " ' - <'
----- 10. PeU'oleum-contam'iriiated media
and debris that fail the test for the
Toxicity Characteristic of § 261;24
(Hazardous Waste Codes D018 through
-BQ43 only) and are subject to the
corrective action regulations under part
•280 of this chapter. ;
§261.24 [Corrected]
18. Also on page 11862, column three,
in § 261.24 Table I.—- Maximum
Concentration of Contaminants for the
Toxicity Characteristic, lin.es twenty-
eight and twenty-nine, change
"Heptachlor (and its hydroxide)" to
"Heptachlor (and its epoxide)".
PART 271— [AMENDED-]- ' ••[..-•.
'§271.1 [Corrected] . ; • -- -"
19. Onpage 11878, hi | 271.1(|), Table
1— Regulations Implementing the
Hazardous and Solid Waste
Amendments of 1984, the Federal
Register reference should be "55 FR
11798-11S77". , ;...-.
•PART.SOSHiAMENDED] ':-.- -' :- - /
§302.4 [Corrected]
20. On page 11877, m § 302.4, Table
302.4, List of Hazardous Substances and
Reportable Quantities, in the first
column, make the following corrections:
A. In the ninth line, change
"Heptachlor (and hydroxide) (D031)" to
"Heptachlor (and epoxide) (D031}." '
B. In line twenty-five, change
"Thrichloroethylene (D040)" to
"Trichloroethylene (D040)"i
G. In to.e twenty-six, change "2,4,5-
Trichlorethylene (D041)" to "2,4,5-
Trichlorophenol (D041)".,
Dated: June 22, 1990. ' '-.-_..-
"Mary A. Cade, - ' : " ."•'../
Acting Assistant Administrator.
In addition to the corrections made
above, part 261 is amended by revising
appendix II to read as follows:
Appendfe H— Method 1311 Toxicity
Characteristic Leaehfcg Procedure •
(TCLP). ., • - • • ";.;-• -- -. /: -
1.0 Scope and Application
1.1 The TCLP is designed to determine the
mobility of both organic and inorganic
analytes present inliquidf solid, and •'.-.--.-•..
c multiphasie wastes. '.. ,
1.2 If a total analysis of the waste
demonstrates that individual analytes are not
present in the waste, or that they are present
"butat such low iGoncentrations that the,
appropriate regulatory levels could not
possibly be exceeded, the TCLP need not be ;
run. .-.-••"'.- ,.- •'.;--' - . . •'- ;
1.3 If an analysis of any one of the liquid
factions of the TGLP extract indicates that a
regulated compound is present "at such high
"concentrations that, even after accounting for
dilution from the ;other fractions of the
.extract, the concentration would be equal to
or above the regulatory level for that
compound, then the waste is hazardous and it
is not necessary to analyze the remaining
fractions of the extract,
1.4 If an analysis of extract obtained .' •'.
using a bottle extractor shows "that.the:"-"-
concentration of any regulated volatile
analyte equals or exceeds the regulatory
level for that compound, then the waste is :
hazardous and extraction using the ZHE is
not necessary. However, extract from a bottle
extractor cannot be used to demonstrate that
the concentration of volatile compounds is ,
below the regulatory level. " ":•_
2.0 Summary of Method
2.1 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
fim glass fiber-filter, is defined as the TCLP
extract.
• ' 2.2 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; the particle' size of the solid
phase is reduced, if necessary. The solid
phase is exfracted with an amount of
extraction fluid equal to 20 tunes 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 testjng for volatile . -. "
analytes (see Table 1 for a list of volatile
compounds). Following extraction, the liquid
extract is" separated from the solid phase by
filtration through a 0,6 to 0.8 /im glass fiber :
filter. ; _ '--.'..
2,3 If compatible; (i.e., multiple phases will
not forin on combination), the initial liquid
phase of &8 waste'is added to the liquid
extract, tod these are analyzed together. If
incompatible, the liquids are'analyzed
separately and the results are mathematically
combined to yield a volume-weighted
average concentration.
SO 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 Agitation apparatus: The agitation
apparatus must be capable of rotating the
extraction vessel in an end-dver-end fashion '
(see Figure 1) at 30 ±2 rpm. Suitable devices
known to EPA are identified ia Table 2.
4.2 Extraction Vessels. -.-•"". •'-.'•'
4.2.1 Zero-Headspace Extraction Vessel
(ZHE). This ;device is for use only when the
waste is being tested for the mobility of
-------
26988 Federal Register / Vol. 55, No. 126 /Friday. June 29, 1990 / Rulea^and ^Regulation's
volatile analy tes (I.e., those listed in Table 1).
The ZHE (depleted in Figure 2) allows for
liquid/solid separation within the device, and
effectively precludes headspace. This type of
vessel allows for initial liquid/solid
separation, extraction, and final extract
filtration without opening the vessel (see
section 4.3.1). The vessels shall have an
Internal volume of 500-600 ml* and be
equipped to accommodate a 90-110 mm filter.
Tho devices contain V1TON®1 O-rings which
should be replaced frequently. Suitable ZHE
devices known to EPA are identified in Table
3,
For the ZHE to be acceptable for use, the
piston within the ZHE should be able to be
moved with approximately 15 pounds per
square inch (psl) or less. If it takes more
pressure to move the piston, the O-rings in
the device should be replaced. If this does not
solve the problem, the ZHE is unacceptable
for TCLP analyses and the manufacturer
should be contacted.
The ZHE should be checked for leaks after
every extraction. If the device contains a
built-in pressure gauge, pressurize the device
to 50 psi, allow it to stand unattended for 1
hour, and rocheck the pressure. If the device
does not have a built-in pressure gauge,
pressurize the device to SO psi, submerge it in
water, and check for the presence of air
bubbles escaping from any of the fittings. If
pressure is lost, check all fittings and inspect
and replace O-rings, if necessary. Retest the
device. If leakage problems cannot be solved,
the manufacturer should be contacted.
Some ZHEs use gas pressure to actuate the
ZHE piston, -while others use mechanical
pressure (see Table 3). Whereas the volatiles
procedures (see section 7.3) refers to pounds
per square inch (psi), for the mechanically
actuated piston, the pressure applied is
measured in torquo-lncli-pounds. Refer to the
manufacturer's instructions as to the proper
conversion.
4,2.2 Bottle Extraction Vessel. When the
waste is being evaluated using the
nonvolatile extraction, a jar with sufficient
capacity to hold the sample and the
extraction fluid is needed. Headspace is
allowed In this vessel.
The extraction bottles may be constructed
from various materials, depending on the
annlylcs to be analyzed and the nature of the
waste (see section 4.3.3). It is recommended
that borosilicate glass bottles be used instead
of other types of glass, especially when
inorganics are of concern. Plastic bottles,
other than polytetrafluoroethylene, shall not
be used if organics are to be investigated.
Bottles are available from a number of
laboratory suppliers. When this type of
extraction vessel is used, the filtration device
discussed in section 4.3.2 is used for initial
liquid/solid separation and final extract
filtration.
4.3 Filtration Devices: It is recommended
that all filiations be performed in a hood.
4.3.1 Zero-Headspace Extractor Vessel
(ZHE): When the waste is evaluated for
volatiles, the zero-headspace extraction
vessel described in section 4.2.1 is used for
, filtration. The device shall be capable of
supporting and keeping in place the glass
fiber filter and be able to withstand the
pressure needed to accomplish separation (50
psi). '• -
Note: When it is suspected that the glass
fiber filter has been ruptured, an in-line glass
fiber filter may be used to filter the material
within the ZHE.
4.3.2 Filter Holder When the waste is
evaluated for other than volatile analytes,
any filter holder capable of supporting a glass
fiber filter and able to withstand the pressure
needed to accomplish separation may be
used. Suitable filter holders range from
simple vacuum units to relatively complex
systems capable of exerting pressures of up
to SO psi or more. The type of filter holder
used depends on the properties of the
material to be filtered (see section 4.3.3).
These devices shall have a minimum internal
volume of 300 mL and be equipped to
accommodate a minimum filter size of 47 mm
(filter holders having an internal capacity of
1.5 L or greater, and equipped to
accommodate a 142 mm diameter filter, are
recommended). Vacuum filtration can only be
used for wastes with low solids content ,
(<10%) and for highly granular, liquid-
containing wastes. All other types of wastes
should be filtered using positive pressure
filtration. Suitable filter holders known to
EPA are shown in Table 4.
4.3.3 Materials of Construction:
Extraction vessels and filtration devices shall
be made of inert materials which will not
leach or absorb waste components. Glass,
polytetrafluoroethylene (PTFE), or type 316
stainless steel equipment may be used when
evaluating the mobility of both organic and
inorganic components. Devices made of.high
density polyethylene (HOPE), polypropylene
(PP), or polyvinyl chloride (PVC) may be used
only when evaluating the mobility of metals.
Borosilicgte glass bottles are recommended
for use over other types of glass bottles,
especially when inorganics are analytes of
concern.
4.4 Filters: Filters shall be made of
borosilicate glass fiber, shall contain no ,
binder materials, and shall have an effective
pore size of 0.6 to 0.8 fan, or equivalent.
Filters known to EPA Which meet these
specifications are identified in Table 5. Pre-
filters must not be used. When evaluating the
mobility of metals, filters shall be acid-
washed prior to use by rinsing with IN nitric
acid followed by three consecutive rinses
with deionized distilled water (a minimum of
1L per rinse is recommended). Glass fiber
' filter are fragile and should be handled with
care.
4.5 pH Meters: The meter should be
accurate to ± 0.05 units at 25°C.
4.6 ZHE Extract Collection Devices:
TEDLAR® 3 bags or glass, stainless steel or
PTFE gag-tight syringes are used to collect
' the initial liquid phase and the final extract of
the waste when using the ZHE device. The
devices listed are recommended for use
under the following conditions:
4.6.1 If a waste contains an aqueous
liquid phase or if a waste does not contain a
significant amount of nonaqueous liquid (i.e.,
1% of total waste), the
syringe or the TEDLAR® bag may be used'
for both the intitial solid/liquid separation
and the final extract filtration. However^ -- :
analysts should use one or the other, not
both.
4.6.3 If the waste contains no initial liquid
phase (is 100% solid) or has no significant
solid phase (is 100% liquid), either the :
TEDLAR® bag or the syringe may be used, If
the syringe is used, discard the first 5 mL of
liquid expressed.from the device. The ' „
remaining aliquots are used for analysis.
4.7 ZHE Extraction Fluid Transfer ^
Devices; Any device capable of transferring
the extraction fluid into the ZHE without
changing the nature of the extraction fluid is
acceptable (e.g, a positive displacement or
peristaltic pump, a gas tight syringe, pressure
filtration unit (see section 4.3.2), or other ZHE
device), •
4,8 Laboratory Balance: Any laboratory
balance accurate to within ± 0.01 grams may
be used (all weight measurements are to ba
within ,± 0,1 grams).
4.9 Beaker or Erlenrneyer flask, glass, 500
mL.
4.10 Watchglass, appropriate diameter to
cover beaker or erlenmeyer flask. ;
4.11 Magnetic stirrer.
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 accaracy'of the
determination.
5.2 Reagent water. Reagent wWer is
defined as water in which an inteiferant is
not observed at or above the methods
detection limit of the analyte(s) of interest.
For nonvolatile extractions, ASTM lype II
water Or equivalent meets the definition of
reagent water. For volatile extraction*, it is
recommended that reagent water be
generated by any of the following methods.
Reagent water should be monitored
periodically for impurities.
5.2.1 Reagent water for volatile
extractions may be generated by passing tap
water through a carbon filter bed containing
about 500 grams of activated carbon (Calgon
Corp., Filtrasorb-300 or equivalent).
5.2.2 A water purification system
(Millipore Super-Q or equivalent) may also be
used to generate reagent water for volatile
extractions.
5.2.3 Reagent water for volatile
extractions may also be prepared by boiling
water for 15 minutes. Subsequently, while
maintaining the water temperature at 90 + 5
degrees C, bubble a contaminant-free inert
gas (e.g., nitrogen) through the water for 1
hour. While still hot, transfer the water to a
narrow mouth screw-cap bottle under zero-
-------
headspace and seal with a Teflon-SSned
septum and cap.
5.3 Hydrochloric acid (IN), HC1. made
from ACS reagent grade.
• 5.4 Nitric acid (IN), HN!% of original
sample weight) has obviously adhered to the
container used-to transfer the sample to the
filtration apparatus, determine the weight of
this residue and subtract >it from the sample
weight determined in section 7.1.1.5 to
determine he weight of the waste sample that
will be filtered.
Gradually apply vacuum or gentle pressure
ofi-10 psi, until air or pressurizing gas moves
through the filter. If this point is hot reached
under 10 psi, and if no additional liquid has
passed through the filter in any 2 minute
interval, slowly increase the pressure in 10
psi increments to a maximum of 50 psi. After
each incremental increase of 10 psi, if the
pressurizing gas has not moved through the
filter, and if no additional liquid has passed
through the filter in any 2 minute interval,
proceed to the next 1Gpsi increment. When-'-.
the pressurizing gas begins to move through
the filter, or when liquid flow has ceased at
SO psi (i.e., filtration does not result in any
additional filtrate within any 2 minute
period), stop tie filtration.
Note: Instantaneous application of high
pressure can degrade the glass fiber filter and
; may cause premature plugging.
7.1.1.8 The material in the filter holder is
defined as the solid phase of the waste, and
the filtrate is defined as the liquid phase.
Note: Some wastes, such as oily wastes
and some paint wastes, will obviously
contain some material, that appears to be a •
liquid. Even after applying vacuum or
pressure filtration, as outlined in section
7.1.1.7, this material may nbt filter. If this is
the case, the material within the filtration
device is defined as a solid. Do not replace
the original filter with a fresh filter under any
circumstances. Use only one filter.
7.1.1.9 Determine the weight of the liquid
phase by subtracting the weight of the filtrate
container (see section 7.1.1.3) from the total
weight of the filtrate-filled container.
Determine the weight of the solid phase of
the waste sample by subtracting the weight '
of the liquid phase from the weight of the
total waste sample, as determined in section
7.l.t5 or 7.1.1.7.
Record the weight of the liquid and solid
phases. Calculate the percent solids as
follows: :.
X 100
-------
26990 Federal Register / Vol. 55, No. 126 /Friday. June 29, 1990 / Rules and Relations
7.1.2 If the percent solids determined in
section 7.1.1.9 is equal to or greater than 0.5%,
then proceed either to section 7.1.3 to
determine whether the solid material requires
particle size reduction or to section 7.1.2.1 if it
is noticed that a small amount of the filtrate
is entrained in wetting of the filter. If the
percent solids determined in section 7.1.1.9 is
loss than 0.555, then proceed to section 7.2.9 if
% dry solids
the nonvolatile TCLP is to be performed and
to section 7.3 with a fresh portion of the
waste if the volatile TCLP is to be performed.
7.1.2.1 Remove the solid phase and filter
from the filtration apparatus.
7.1.2.2 Dry the filter and solid phase at
100± 20°C until two successive weighings
yield the same value within ± 1%. Record the
final weight.
Note: Caution should be taken to ensure
that the subject solid Will not flash upon
heating. It is recommended that the drying
oven be vented to a hood or other
appropriate device.
7.1.2.3 Calculate the percent dry solids as
follows: , - , . - ...... -
(Weight of dry waste+filter)—tared weight of filter
Initial weight of waste (section 7.1.1.5 or 7.1.1.7)
X100
7.1.2.4 If the percent dry solids is less
than 0.596, then proceed to section 7.2.9 if the
nonvolatile TCLP is to be performed, and to
section 7.3 if the volatile TCLP is to be
performed. If the percent dry solids is greater
than or equal to 0.5%, and if the nonvolatile
TCLP is to be performed, return to the
beginning of this section (7.1) and, with a
fresh portion of waste, determine whether
particle size reduction it) necessary (section
7.1.3) and determine the appropriate
extraction fluid (section 7.1.4). If only the
volatile TCLP is to be performed, see the note
in section 7.1.4.
7.1.3 Determination of whether the waste
requires particle size reduction (particle size
is reduced during this step): Using the solid
portion of the waste, evaluate the solid for
pnrtlclo size. Particle size reduction is
required, unless the solid has a surface area
per gram of material eqiial to or greater than
3.1 cm*, or Is smaller than 1 cm in its
narrowest dimension (i.e., is capable of
passing through a 9.5 mm (0.375 inch)
standard sieve). If the surface area is smaller
or the particle size larger than described
above, prepare the solid portion of the waste
for extraction by crushing, cutting, or grinding
the waste to a surface area or particle size as
described above. If the solids are prepared
for organic volatiles extraction, special
precautions must bo taken (see section 7.3.6).
Note: Surface area criteria are meant for
filamentous (e.g., paper, cloth, and similar)
waste materials. Actual measurement of
surface area Is not required, nor is it
recommended. For materials that do not
obviously meet the criteria, sample-specific
methods would need to be developed and
employed to measure the surface area. Such
methodology is currently not available.
7.1.4 Determination of appropriate
extraction fluid: If the solid content of the
waste is greater than or equal to 0.5% and if
the sample will be extracted for nonvolatile
constituents (section 7.2), determine the
appropriate fluid (section 5.7) for the
nonvolatiles extraction as follows:
Note: TCLP extraction for volatile
constituents uses only extraction fluid #1
(section S.7.1). Therefore, if TCLP extraction
for nonvolatiles is not required, proceed to
section 7.3.
7,1.4.1 Weigh out a small subsample of
tho solid phase of the waste, reduce the solid
(If necessary) to a particle size of
approximately 1 mm in diameter or less, and
transfer 5.0 grams of the solid phase of the
waste to a 500 mL beaker or Erlenmeyer
flask.
7.1.4.2 Add 96.5 mL of reagent water to
the beaker, cover with a watchglass, and stir
vigorously for 5 minutes using a magnetic
stirrer. Measure and record the pH. If the pH
is <5.0, use extraction fluid #1. Proceed to
section 7.2.
7.1.4.3 If the pH from section 7.1.4.2 is
>5.0, add 3.5 mL IN NCI, slurry briefly, cover
with a watchglass, heat to 50°C, and hold at
50°C for 10 minutes.
. 7.1.4.4 Let the solution cool to room
temperature and record the pH. If the pH is
<5.0, use extraction fluid #1. If the pH is
>5.0, use extraction fluid #2, Proceed to
section 7.2.
7.1.5 If the aliquot of the waste used for
the preliminary evaluation (sections 7.1.1-.
7.1.4) was determined to be 100% solid at
section 7.1.1.1, then it can be used for the
section 7.2 extraction (assuming at least 100
grams remain), and the section 7.3 extraction
(assuming at least 25 grams remain). If the
aliquot was subjected to the procedure in
section 7.1.1.7, then another aliquot shall be
used for the volatile extraction procedure in
section 7.3. The aliquot of the waste
subjected to the procedure in section 7.1.1.7
might be appropriate for use for the section
7.2 extraction if an adequate amount of solid
(as determined by section 7.1.1.9) was
obtained. The amount of solid necessary is
dependent upon whether a sufficient amount
of extract will be produced to support the
analyses. If an adequate amount of solid
remains, proceed to section 7.2.10 of the, ;
nonvolatile TCLP extraction.
7.2 Procedure When Volatiles are not
Involved. A minimum sample size of 100
grams (solid and liquid phases) is
recommended. In some cases, a larger sample
size may be appropriate, depending on the
solids content of the waste sample (percent
solids, See section 7.1.1), whether the initial
liquid phase of the waste will be miscible
with the aqueous extract of the solid, and
whether inorganics, semivolatile organics,
pesticides, and herbicides are all analytes of
concern. Enough solids should be generated
for extraction such that the volume of TCLP
extract will be sufficient to support all of the
analyses required. If the amount of extract
generated by a single TCLP extraction will
not be sufficient to perform all of the
analyses, more than one extraction may be
performed and the extracts from each
combined and aliquoted for analysis.
7.2.1 If the waste will obviously yield no
liquid when subjected to pressure filtration
(i.e., is 100% solid, see section 7.1.1), weigh
out a subsample of the waste (100 gram
minimum) and proceed to section 7-2.9.
7.2.2 If the sample is liquid or multiphasic,
liquid/solid separation is required. This
involves the filtration device described in .
section 4.3.2 and is outlined in sections 7.2.3 ....
to 7.2.8. ,
7.2.3 Pre-weigh the container that will
receive the filtrate.
7.2.4 Assemble the filter holder and filter
following the manufacturer's instructions.
Place the filter on the support screen and
secure. Acid-wash the filter if evaluating the
mobility of metals (see section 4.4).
Note: Acid-washed filters may be used for
all nonvolatile extractions even when metals
are not of concern.
7.2.5 Weigh out a subsample of the waste
(100 gram minimum) and record the weight. If
the waste contains <0.5% dry solids (section
7.1.2), the liquid portion of the waste, after
filtration, is defined as the TCLP extract
Therefore, enough of the sample should be
filtered so that the amount of filtered liquid
will support all of the analyses required of
the TCLP extract. For wastes containing
>0.5% dry solids (sections 7.1.1 or 7.1.2), use
the percent solids information obtained in
section 7.1.1 to determine the optimum
sample size (100 gram minimum) for filtration.
Enough solids should be generated by
filtration to support the analyses to be
performed on the TCLP extract
7.2.6 Allow slurries to stand to permit the -
solid phase to settle. Wastes that settle
slowly may be centrifuged prior to filtration.
Use centrifugation only as an aid to filtration.
If the waste is centrifuged, the liquid should
be decanted and filtered followed by
filtration of the solid portion of the waste
through the same filtration system.
7.2.7 Quantitatively transfer the waste
sample (liquid and solid phases) to the filter
holder (see section 4.3.2). Spread the waste
sample evenly over the surface of the filter. If
filtration of the waste at 4 °C reduces the
amount of expressed liquid over what would
be expressed at room temperature, then
allow the sample to warm up to room
temperature in the device before filtering.
Note: If waste material (>1% of the original
sample weight) has obviously adhered to the
container used to transfer the sample to the
filtration apparatus, determine the weight of
-------
i; June 29,. 1990 ;/ Rules and Regulations
269@1
this residue and subtract it from the sample
weight determined in section 7.2.5, to
determine the weight of the waste sample
tliat will be filtered.
Gradually apply vacuum or gentle pressure
of 1-riO psi, until air or pressurizing gas moves
through the filter. If this point is reached
under 10 psi, and if no additional liquid has .
passed_tliroUgh the filter in any 2 minute
interval, slowly increase the pressure hi 10
psi increments to a maximum of SO psi. After
each incremental increase of 10 psi, if the
pressurizing gas has not moved through the
filter, and if-no additibnalliquid has passed
through the filter in any 2 minute interval,
proceed to the next 10'psi increment. When
the pressurizing gas begins to move through
the filter, or when the liquid .flow has ceased
at 50 psi (i.e.; filtration does .not result in any
additional filtrate ivithin'a 2 minute period),
stop the filtration.
Note: Instantaneous application of high
"pressure can degrade the glass fiber filter and
may cause premature plugging. :
7.2,8 The material in the filter holder is
defined as the solid phase of the waste, and •
the filtrate is. defined as the liquid phase.
Weigh the filtrate. The liquid phase may now
be either analyzed (See section 7.2.12) or
stored at 4°C until time of analysis.
Note: Some wastes, such as oily wastes
and some paint wastes, will obviously
contain some material that appears to be a
liquid. Even after applying vacuum or
pressure filtration, as outlined in section 7.2.7,
this material may not filter. If this is the case, ',
the material within the filtration device is
defined as a solid'and is carried through the
extraction as a solid. Do not replace the
original filter with a fresh filter under any
circumstances. Use only one filter!
7.2.9 ' If the waste contains <0.5% dry
solids (sea section 7.1.2), proceed to section
7.2.13. If the waste contains >b.5% dry solids
; (see section 7.1.1 or 7.1.2],' and if particle sizs
reduction of the solid was needec! in section "
7.1.3, proceed to section 7.2,10. If the waste as
.received passes a 9.5 mm sieve, :
quantitatively transfer the solid material into
the extractor bottle along with the filter used
to separate the initial liquid from the solid
phase, and proceed to section 712:11. :'
~ 7.2.10 Prepare the solid portion of the
waste for extraction by crushing, cutting, or
grinding the waste tp a surface area or
particle size as described to section 7.1.3.
When the surface area 'or particle.size has
been appropriately altered, quantitatively
transfer the solid material into an extractor
bottle. Include the filter used to separate the
initiaHiquid from the solid phase.
Note: Sieving of the waste is riot normally
required. Surface area requirements are
meant for filamentous (e.g;, paper, cloth) and
similar waste materials. Actual measurement
of surface area is not recommended. If
sieving is necessary, a Teflon-coated sieve
should be used to avoid contamination of the
sample. •
7.2.11 Determine the amount of extraction
fluid to add to the extractor vessel as follows:;
Weight of extraction fluid =
solids (sociion 7.J.l)x:weight of waste filtered (section 7.2.5 or 7.2.7):
100
Slowly add this amount of appropriate
extraction fluid (see section 7.1.4) to the
extractor vessel. Close the extractor bottle
. tightly (it is recommended that Teflon tape be
used to ensure a tight seal), secure in rotary
agitation device, and rotate at 30 ± 2rpmfor
18 ± 2 hours. Ambient temperature (i.e.,
temperature of room in which extraction
takes place) shall be maintained at 23 ± 2°C
during the extraction period.
. Note: As agitation continues, pressure may
build within the extractor bottle for some
types of wastes (e.g., limed or calcium
carbonate containing was'te may evolve
gases such as carbon dioxide). To relieve
excess pressure, the extractor bottle may be
periodically opened (e.g., after 15 minutes, 30
minutes, and 1 hour) and vented into a hood.
7.2.12 Following the 18 ± 2 hour
extraction, separate the material in the
extractor vessel into its component liquid and
solid phases by filtering through a new glass
fiber filter, as outlined in section 7.2.7. For '
final filtration of the TCLP extract, the glass
fiber filter may be changed, if necessary, to
facilitate filtration, Filter(s) shall be acid-
washed (see section 4.4) if evaluating the
mobility of metals.
7.2.13 Prepare the TCLP extract as
follows: .
7.2.13.1 If the waste contained no initial
liquid phase, the filtered liquid material
obtained from section 7.2.12 is defined as the
TCLP extract. Proceed to section 7.2.14.
7.2.13.2 If compatible (e.g., multiple
phases will not result on combination),
combine the filtered liquid resulting from
section 7.2.12 with the initial liquid phase of
fee waste obtained in section 7.2.7. This
combined liquid is defined as the TCLP
extract. Proceed to section 7.2.14. '
7.2.13.3 If the initial liquid phase of the
waste, as obtained from section 7.2.7, is not
- or may not be compatible with the filtered
liquid resulting from section 7.2.12, do not
combine these liquids. Analyze these liquids,
collectively defined as tlie TCLP extract, and
combine the results mathematically, as -
described in section 7.2.14.
7.2.14 ; Following collection of the TCLP
extract, the pH of the extract, should be
recorded. Immediately aliquot and preserve
the extract for analysis. Metals aliquots must
be acidified with nitric acidjo pH <2. If
precipitation is observed upon addition of
nitric acid to a small aliquot of the extract,
then the remaining portion of the extract for
metals analyses shall not be acidified and the
extract shall be analyzed,a? soon as possible.
All other aliquots must be stored under
refrigeration (4 °C) until analyzed. The TCLP
extract shall be prepared and analyzed
according to appropriate analytical methods.
- TCLP extracts to be analyzed for'metals shall ;
, be acid digested except in those instances
where digestion causes loss of metallic
analytes.-If an analysis of the undigested
extract shows that the concentration of any ;•
regulated metallic analyte exceeds the
regulatory level, then the waste is hazardous
and digestion of the extract is not necessary.
However, data on .undigested extracts alone
cannot be used to demonstrate that the waste
is not hazardous. If the individual phases are -
to be analyzed separately,'determine the
volume of the individual phases (to ± 0.5%],
conduct the appropriate analyses, and
combine the results mathematically by using
a simple volume-Weighted average: '
Final Analyte
Concentration
where:
Vf= The volume of the first phase (L).
Ci =The concentration of the analyte of
concern in the first phase (mg/L).
Yz=The volume of the second phase (L).
C2=The concentration of the analyte of
concern in the second phase (nig/L).
7.2.15 Compare the analyte .
concentrations in the TCLP extract with the
levels identified in the appropriata
regulations_. Refer to section 8.0 for quality
assurance requirements. •
7.3 Procedure When Volatiles are
Involved. Use the ZHE: device to obtain TCLP
extract for analysis of volatile compounds
only. Extract resulting from the use of the
ZHE shall not be used to evaluate the :
mobility of nonvolatile analytes (e.g., metals,
pesticides, etc.).
. The ZHE;device has approximately a 500
mL internal capacity. Tie ZHE can thus
accommodate a maximum of 25 grams of
solid (defined as that fraction of a sample.
from which no additional liquid may be
forced out by an applied pressure-of 50 psi),
due to the heed to add an amount of
extraction fluid equal to 20' times the weight
of the solid phase. ,
.. Charge the ZHE with, sample only once and
do not open the device Until the final extract
(of the solid) has been collected. Repeated
filling of the ZHE to obtain 25 grams of solid
is not permitted.
Do not allow the waste, the initial liquid
phase, or the extract to be exposed to the
"atmosphere for any more time than is
absolutely necessary. Any manipulation of
these materials should be done when cold
(4°G) to minimize loss of volatiles.
7.3.1 Pre-weigh the (evacuated) filtrate • '
collection container (See section 4.6) and set
aside. If using a TEDLAR® bag, express all ; ,
liquid from the ZHE device into .the bag,
-------
26992 Federal Register / Vol. 55, No. 126 / Friday, June 29, 1990 / Rules and Regulations
whether for the Initial or final liquid/solid
separation, and take an aliquot from the
liquid in the bng for analysis. The containers
listed in section 4.8 are recommended for use
under the conditions stated in sections 4.6.1-
4.0.3.
7,3.2 Place the ZHE piston within the
body of the ZHE (it may be helpful first to
moisten the piston O-rings slightly with
extraction fluid). Adjust the piston within the
ZHE body to a height that will minimize the
distance the piston will have to move once
the ZHE is charged with sample (based upon
sample size requirement!) determined from
section 7.3, section 7.1.1 and/or 7.1.2). Secure
the gas inlet/outlet flange (bottom flange)
onto the ZHE body in accordance with the
manufacturer's instructions. Secure the glass
fiber filter between the support screens and
set aside. Set liquid inlet/outlet flange (top
flange) aside.
7.3.3 If the waste is 100% solid (see
section 7.1.1), weigh out a subsample (25
gram maximum) of the waste, record weight,
and proceed to section 7.3.5.
7.3,4 If the waste contains <5% dry solids
(section 7.1.2), the liquid portion of waste,
after Filtration, is defined as the TCLP
extract. Filter enough of the sample so that
the amount of filtered liquid will support all
of the volatile analyses required. For wastes
"containing >S% dry solids (sections 7.1.1
and/or 7.1.2), use the percent solids
information obtained in section 7.1.1 to
determine the optimum sample size to charge
into the ZHE. The recommended sample size
is as follows: , .,
7.3.4.1 For wastes containing <5% solids
(see Section 7.1.1), weigh out a 500 gram
subsample of waste and record the weight
7.3.4.2 For wastes containing >5% solids
(see Section 7.1.1), determine the amount of
waste to charge into the ZHE as follows:
Weight of waste to charge ZHE
25
percent solids (section 7.1.1)
•X100
Weigh out a aubsampl'S of the waste of the
appropriate size and record the weight.
7.3.5 If particle size reduction of the solid
portion of the waste was required in section
7.1.3, proceed to section 7.3.6. If particle size
reduction was not required in section 7.1.3,
proceed to section 7.3.7.
7.3.6 Prepare the was te for extraction by
crushing, cutting, or grinding the solid portion
of the wastq to a surface area or particle size
as described In section 7,1.3.1. Wastes and
appropriate reduction equipment should be
refrigerated, if possible, to 4°C prior to
particle size reduction. The means used to
effect particle size reduction must not
generate heat in and of itself. If reduction of
the solid phase of the waste is necessary,
exposure of the waste to the atmosphere
should be avoided to the extent possible.
Note: Sieving of the waste is not
recommended due to the possibility that
volatiles may be lost. The use of an
appropriately graduated ruler is
recommended as an acceptable alternative.
Surface area requirements are meant for
filamentous, (e.g., paper, cloth) and similar
waste materials. Actual measurement of
surface area is not recommended.
When the surface area or particle size has
been appropriately altered, proceed to
section 73.7.
7.3.7 Waste slurries need not be allowed
to stand to permit the solid phase to settle.
Do not centrifuge wastes, prior to filtration.
7.3,8 Quantitatively transfer the entire
sample (liquid and solid phases) quickly to
tho ZHE. Secure the filter and support
screens onto the top flange of the device and
secure the top flange to the ZHE body in
accordance with the manufacturer's
instructions. Tighten all ZHE fittings and
place the device in the vertical position (gas
inlet/outlet flange on the bottom). Do not
attach the extract collection device to the top
plate.
Note: If waste material (>1% of original
sample weight) has obviously adhered to the
container used to transfer the sample to the
ZHE, determine the weight of this residue
and subtract it from the sample weight
determined in section 7.3.4 to determine the
weight of the waste sample that will be
filtered.
Attach a gas line to the gas inlet/outlet
valve (bottom flange) and, with the liquid
inlet/outlet valve (top flange) open, begin
applying gentle pressure of 1-10 psi (or more
if necessary) to force all headspace slowly
out of the ZHE device into a hood. At the first
appearance of liquid from the liquid inlet/
outlet valve, quickly close the valve and
discontinue pressure. If filtration of the waste
at 4 *C reduces the amount of expressed
liquid over what would be expressed at room
temperature, then allow the sample to warm
up to room temperature in the device before
filtering. If the waste is 100% solid (see
section 7.1.1), slowly increase the pressure to
a maximum of 50 psi to force most of the
headspace out of the device and proceed to
section 7.3.12,
7.3.9 Attach the evacuated pre-weighed
filtrate collection container to the liquid
inlet/outlet valve and open the valve. Begin
applying gentle pressure of 1-10 psi to force
the liquid phase of the sample into the filtrate
collection container. If no additional liquid
has passed through the filter in any 2 minute
interval, slowly increase the pressure in 10
psi increments to a maximum of 50 psi. After
each incremental increase of 10 psi, if no
additional liquid has passed through the filter ,
in any 2 minute interval, proceed to the next
10 psi increment. When liquid flow has
ceased such that continued pressure filtration
at 50 psi does not result in any additional
filtrate within a 2 minute period, stop the
filtration. Close the liquid inlet/outlet valve,
discontinue pressure to the piston, and
disconnect and weigh the filtrate collection
container. .
Note: Instantaneous application of high
pressure can degrade the glass fiber filter and
may cause premature plugging.
7.3.10 The material in the ZHE is defined
as the solid phase of the waste and the
filtrate is defined as the liquid phase.
" Note: Some wastes, such as oily wastes
and some paint wastes, will obviously
contain some material that appears to be a
liquid. Even after applying pressure filtration,
this material will not filter. If this is the case,
the material within the filtration device is
defined as a solid and is carried through the
TCLP extraction as a solid.
If the original waste contained <0.5% dry
solids (see section 7.1.2), this filtrate is
defined as the TCLP extract and is analyzed
directly. Proceed to section 7.3.15.
7,3.11 The liquid phase may now be either
analyzed immediately (See sections 7.3.13
through 7.3.15) or stored at 4°C under minimal
headspace conditions until time of analysis.
Determine the weight of extraction fluid #1
to add to the ZHE as follows:
Weight of extraction fluid
20Xpercent solids (section 7.1.1) X weight of waste filtered (section 7.3.4 or 7.3.8)
100
-------
Federal Register /Vol. 55, No. 126 /Friday, June 29, 1990 /Rules and Regulations 26993
. 7.3.12 The following sections detail how
: to, add the appropriate amount of extraction ,
fluid to the solid material within the ZHE and
agitation of the ZHE vessel. Extraction fluid
#1 is used in all cases (See section 5.7).
7.3.12.1 .With the ZHE in the vertical
position, attach a line from the extraction
fluid reservoir to the liquid inlet/outlet valve.:
The line used shall contain fresh extraction
fluid and should be preflushed with fluid to
eliminate any air pockets in the line. Release
gas pressure on the ZHE piston (from the gas
inlet/outlet valve), open the liquid inlet/
outlet valve, and begin transferring extraction'
fluid (by pumping or similar means) into the
ZHE. Continue pumping extraction fluid into
the ZHE until the appropriate amount of fluid
has been introduced into the device. •
7.3.12.2 After the extraction fluid has
been added, immediately close ihe liquid
inlet/outlet valve and disconnect the
extraction fluid line. Check the ZHE to ensure
that all valves are in their closed positions.
Manually rotate the device in an end-over-
erid fashion 2 or 3 times. Reposition the ZHE '.
in the vertical position with the liquid inlet/
outlet valve on top. Pressurize the ZHE to 5^
10 psi (if necessary) and slowly open the
. liquid inlet/outlet valve to bleed out any
headspace (into a hood) that may have been
introduced due to the addition of extraction
fluid. This bleeding shall be done quickly and
shall be stopped at the first appearance of
liquid from the valve. Re-pressurize the ZHE
with 5-10 psi and check all ZHE fittings to
ensure that they are closed. ;
7;3.12.3 Place the ZHE in the rotary
agitation apparatus (if it is not already there)
and rotate at 30 ± 2 rpm for 18 ± 2 hours.
Ambient temperature (i.e., temperature of
room in which extraction occurs) shall be
maintained at 22' ± 3°C during agitation.
7.3.13 Following the 18 ± 2 hour agitation
period, check the pressure behind the ZHE
pistpn by quickly opening and closing the gas
inlet/outlet valve and noting the escape of
gas. If the pressure has not been maintained
(i.e., no gas release observed), the device is
leaking. Check the ZHE for leaking as
specified in section 4.2.1, and perform the
extraction again with a new sample of waste.
If the pressure within the device has been
; maintained, the material in the extractor
vessel is once again separated into its
component liquid and-solid phases. If the
waste contained an initial liquid phase, the
liquid may be filtered directly into the same
filtrate collection container (i.e., TEDLAR® ,
bag) holding the initial liquid phase of the
waste, A separate filtrate collection container
must bei used if combining would create'"
multiple phases, or there is hot enough :
volume left within the Filtrate collection -
container. Filter through the glass fiber filter,
using the ZHE device as discussed in section
7.3.9. All extract shall 'be filtered and
collected if the TEDLAR® bag is used, if the
extract is multiphasic; or if the waste
contained an initial liquid phase (see sections
4.6 and 7.3.1). V "
: Note: An in-line glass fiber filter may be
used to filter the material within the ZHE if it
is suspected that the glass' fiber filter has
"been ruptured. . . . ..,;..
7.3.14 If the original waste contained no
'initial liquid phase, the filtered liquid
material obtained from section 7.3.13 is .
defined as the TCLP extract. If the waste
contained an initial liquid phase, the filtered
liquid material obtained from section 7.3.13
and the initial liquid phase (section 7.3.9) are
collectively:defined as the TCLP extract.
7.3,15 Following collection of the TCLP
'extract, immediately prepare the extract for
analysis and store with minimal headspace at
4°C until analyzed. Analyze the TCLP extract
according to the appropriate analytical . •
methods. If the individual phases are to be
analyzed separately (i.e., are not miscible),
determine the volume of the individual
phases (to 6.5%), conduct the appropriate
analyses, and combine the results
mathematically by using a simple volume-
weighted average:
Final Analtye
Concentration""
"
where: , , '
Vi =The volume of .the first phases (L). '
Ci =The concentration of the analyte of
concern m the first phase (mg/L).
V2=The volume of the second phase (L).
Cs =The concentration of the analyte of
concern in the second phase (mg/L).
7.3.16 Compare the analyte ;
concentrations hi the TCLP extract with the
levels identified in the appropriate
regulations. Refer to section ao for quality
assurance requirements.
8.0 Quality Assurance ..- . .;'. ,
8.1 A minimum of one blank (using the
same extraction fluid'as used for the
samples) must be analyzed for every 20
extractions that have been conducted in an
extraction vessel. „ .
8.2': A matrix spike shall be performed for
each waste type (e.g.; wastewater treatment
sludge, contaminated soil, etc.) unless the
result exceeds the regulatory level and the
data is being used solely to demonstrate that •
the was.te property exceeds the regulatory
level. A minimum of one matrix spike must
be analyzed for each analytical batch. The
bias determined from the matrix spike
determination shairbe used, to correct the
measured values. (See sections 8.2.4 and ,
8;2.5.) As a minimum, follow the matrix spike
jiddition guidance provided in each analytical
method. ", • r~ ';..-'
.. 8.2.1 Matrix spikes are to be added after
filtration of the TCLP extract and before
preservation. .Matrix spikes should not be
added prior to TCLP extraction of the sample.
8.2.2 In most cases, matrix spikes, should
be added at a concentration equivalent to "the
corresponding regulatory level. If the analyte
concentration is less than one half the
regulatory level, the spike concentration may
be as low as one half of the analyte
concentration, but may not be not less than
five times the method de'tectibn limit. In.order,
to avoid differences in matrix effects, the
matrix spikes must be added to the same
nominal volume of TCLP extract as that :
which was analyzed for the uhspiked sample,
8.2.3 The purpose of the matrix spike is to
monitor the performance of the analytical .
methods used, and to" determine whether
matrix interferences exist. Use of other
internal calibration methods, modification of
the analytical methods, or use of alternate
analytical methods may be needed to
accurately measure the analyte cbngentration
of the TCLP. extract when the recovery of the
matrix spike is below the expected analytical
method performance. • •
8.2.4 Matrix spike recoveries are
calculated by the following formula:'
%R (% Recovery)=l6o (X.-XJ/K .(1 .
where: ' ,," "•'," • .'•''"" '.'•'"
Xa=measure;d,va?ue for the spiked sample,
Xu=measured value for the unspiked sample,
, " and .•...- ;- . •'.'- '•. -
K= known value of the spike in the sample,
8.2.5 Measured values are corrected for
analytical bias using the following formula:
Xc=100 (XU/%R) ••"."•';
where: ''-.'';'-•'•-' • . ' '.'•-, •
Xc—corrected value, and
Xy=measured value of the unspiked sample.
8.3; All quality control measures described
in the appropriate analytical methods shall
be followed. ,!_• •
. 8.4 Samples must undergo TCLP' '.•;• . ]
extractioh within the. following time periods::
-------
26994
Federal Register / Vol. 55. No. 126 / Mday. une '
SAMPLE MAXIMUM HOLDING TIMES (DAYS)
VotaKkn - _ -.
Sorotvotatilcs
MfKHHy
M&ytJs, excopt mofcury »»«»....»«...«»»»...»».»....».»»..» «....«.»»...»...» .»..„........« «.,
From:
Field
collection
to: TCLP
extraction
14
: 14
28
180
From:
TCLP
extraction
to:
Prepara-
tive
extraction
MA
7
MA
NA
From:
prepara-
extraction
determ!-,
native
analysis
14
40
28
180
Total
elapsed.
time
28
61
58
360
NA-Not BpoScabte,
If sample holding times are exceeded,
the values obtained will be considered
minimal concentrations. Exceeding the
holding time is not acceptable in
establishing that a waste does not
exceed the regulatory level. Exceeding
the holding time will not invalidate
characterization if the waste exceeds
the regulatory level.
TABLE 1.—VOLATILE ANALYTES *•*
TABLE 2.—SUITABLE ROTARY AGITATION
APPARATUS '—Continued
TABLE 4.—SUITABLE FILTER HOLDERS *
Compound
n-Bulyl afcohof«
Caiboo disuBRfe
Cartoon tetrachtortde.
Metliyfaoa chtoffcto
Methyl «ihyi kotoo«.._..
M«lhyi Isobutyt kctona..
Tclrnctrforoothylene.
CAS No.
67-64-1
71-43-2
71-35-3
75-15-O
56-23-5
108-90-7
67-66-3
107-06-2
75-35-4
141-78-6
100-41-4
60-29-7
78-83-1
67-58-1
75-09-2
78-93-3
108-10-1
127-18-4
108-83-3
71-55-8
79-01-6
75-69-4
76-13-1
75-01-4
1330-20-7
1 Whon testing for any or a3 oJ thesa anatytes, the
zsrc-hoadspace extractor vessel shall be used in-
ttaad o( tha bottia extractor.
*Btnzane, carbon tetrachtortda, chtorobenzene,
cWoroform, 1,2-cSchtofaBwno, 1,1-dichloroethylene,
meihy) altiyl kctona, totrachloroethylene, trfchlor-
oathv'too*, and! vinyi chtorida are toxfcity characteris-
TABLE 2. — SUITABLE ROTARY AGITATION
APPARATUS *
Company
Anolyticiii
Testing and
Consulting
Services, Inc.
Location
Wanington, PA,
(215) 343-
4490.
Model No.
4-vessel
(DC20S), 8-
vessel
(DC20), 12-
vessel
(DC20B).
Company ' •
Associated
Design and
Manufactur-
ing Company.
Environmental
Machine and
Design, Inc.
IRA Machine
Shop and
Laboratory.
Lars Lande
Manufactur-
ing.
Milllpora Corp. ....
Location
Alexandria VA,
(703) 549-
5999.
Lynchburg, VA,
(804) 845-
6424.
Santurca, PR,
(809) 752-
4004.
Whitmore Lake,
Ml, (313)
449-4116.
Bedford, MA,
(800) 225-
, 3384.
Modal No.
2-vesss! (3740-
2), 4-vesssl
(3740-4), 6-
VGSSSl (3740-
6), 8-vessel
(3740-8), 12-
vessel (3740-
12), 24-
vessel (3740-
24).
8-vessel (08-
00-00)4-
vesssl (04-
00-00).
8-vessel
(011001).
10-vessel
(01VRE), 5-
vessel
(5VRE).
4-ZHEOT41-
llter, bottle
extractor.
(YT30ORAHW).
'Any device that rotates the extraction vessel in
an end-over-end fashion at 30 ± 2 rpm is accepta-
ble.
TABLE 3.—SUITABLE ZERO-HEADSPACE
EXTRACTOR VESSELS *
Company
Analytical
Testing &
Consulting
Services, Inc..
Associated
Design and
Manufactur-
ing Company.
Lars Lande
Manufactur-
ing3.
Millipore
Corporation.
Environmental
Machine and
Design, Inc..
Location
Wamngton, PA,
(215) 343-
4490.
Aiexandria VA,
(703)549-
5999.
Whitmore Lake,
Ml, (313)
449-4116.
Bedford, MA,
(000) 225-
3384.
Lynchburg, VA,
(804)845-
6424.
Model No.
C102,
Mechanical
Pressure
Device.
3745-ZHE, Gas
Pressure
Device.
ZHE-11, Gas
Pressure
Device.
YT30090HW,
Gas Pressure
Device. •
VOLA-TOX1,
Gas Pressure
Device.
1 Any device that meets the specifications listed in
section 4.2.1. of the method is acceptable.
* This device uses a 110 mm filter.
Company
Nucleo-
pore
Corpo-
ration.
Micro
Filtra-
tion
Sys-
tems.
Millipore
Corpo-
ration.
Location
Pleasan-
ton,
CA,
(soo;
882-
7711.
Dublin,
CA,
(800)
334-
7132,
(415)
828-
6010.
Bedford,
MA,
(800)
225-
3334.
Model/catalogua
No.
425910
410400
302400
311400
...
YT30142HW
XX1004700
Size
142mm,
47
mm.
142 mm,
47
mm.
142 rwn,
47
mm.
1 Any device'capable of separating the liquid" from
the solid phase of the waste is suitable, providing
thai ft is chemically compatible with the waste and
the constituents to ba analyzed Plastic devices (not
|ioted above) may be used when only inorganic
anafytes are of concern. The 142 mm size tiltet
holder is recommended
TABLE 5.—SUITABLE FILTER MEDIA 1
Company
Millipore
Corporation.
Nucleopora
Corporation.
Whatman
Laboratory
Products,
Inc..
Micro Filtration
Systems.
Location
Bedford, MA,
(800)225-
3384.
Pleasanton,
CA, (415)
463-2530.
Clifton, NJ,
(201) 773-
5800.
Dublin, CA,
(800) 334-
7132, (415)
828-6010.
Model
AP40
211625
GFF
GF75
Pore
Size
(fimi
0.7
0.7
-
O.I
0.7
1 Any filter that meets the specifications in section
4.4 of the Method is suitable.
BILLING CODE 6SGO-Se-ES
-------
June 29.1990 /Rules and Regulations 26995
±2
Figure 1.- Rotary Agitation. Apparatus
-------
26996
Fedorat Register / Vol. 65, No. 126 / Friday, fune 29,1990 / Rales and Regulations
Top Range
Suppoirt Seree
Vitoni
,1,
Bonom Range
Pressurized! Gas
Inlet/Out!®! Valve
Figure 2. Zero-Headspace Extractor (ZHE)
-------
Register /Vol. S5, No. 126 /Friday, June 29.1990 /Rules and Regulations
•26997V
vTOXICIT¥CHARACTERiSTICl€ACHATE-PROCEDURE, :;:^
Separate
liquids from
solids with
0.6 ~ 0.8 urn
glass fiber
filter '
Discard
solids
Use' Oh
<0.5%.
solids In -the
?'-. -Extract with ";--
-dppropriate fluid
11 Bottle sxtractor
for non-volatiles
2) ZHE devict for
volatilts
Liquid
s from
solids with
0;6- 0.8 um
filter
v .Reduce
particle-size;
> mm
1J
-------
269S3
Federal Register / Vol. 55, No. 126 / Friday, June 29,1990 / Rules and Regulations
METHOD 1311 (CONTINUE?)
TOXICITY CHARACTERISTIC LEACHATE PROCEDURE
Separate
extract from
solids with
0.6 - 0.8 urn
glass fiber
filter
Solid
Combine
extract with
liquid phas®
Analyze
STOP
Measure amount of
liquid and analyze
(mathematically
combine result with
result'of extract
analysis):
IFR Doc. 90-15048 Filed 6-28-90; 8:45 am]
CIUJHO COOE G5W-50-C
-------
-------
------- |