METHOD 1311
TOXICITY CHARACTERISTIC LEACHING PROCEDURE
1.0 SCOPE AND APPLICATION
1.1The TCLP is designed to determine the mobility of both organic and inorganic analytes prent in liquid, solid, and multiphasic wastes.
1.2If a total analysis of the waste demonstrates that individual analytes are not prent in the waste, or that they are prent but at such low concentrations that the appropriate regulatory levels could not possibly be exceeded, the TCLP need not be run.
1.3If an analysis of any one of the liquid fractions of the TCLP extract indicates that a regulated compound is prent at such high concentra-tions that, even after accounting for dilution from the other fractions of the extract, the concentration would be 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.
1.4If an analysis of extract obtained using a bottle extractor shows that the concentration of any regulated volatile analyte 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 ud to demonstrate that the concentration of volatile compounds is below the regulatory level.
2.0SUMMARY OF METHOD
2.1For liquid wastes (i.e., tho containing less than 0.5% dry solid material), the waste, after filtration through a 0.6 to 0.8 µm glass fiber filter, is defined as the TCLP extract.
2.2For wastes containing greater than or equal to 0.5% solids, the liquid, if any, is parated from the solid pha and stored for later analysis; the particle size of the solid pha is reduced, if necessary. The solid pha is extracted with an amount of extraction fluid equal to 20 times the weight of the solid pha. The extraction fluid employed is a function of the alkalinity of the solid pha of the waste. A special extractor vesl is ud when testing for volatile analytes (e Table 1 for a list of volatile compounds). Following extraction, the liquid extract is parated from the solid pha by filtration through a 0.6 to 0.8 µm glass fiber filter.
2.3If compatible (i.e., multiple phas will not form on combination), the initial liquid pha of the waste is added to the liquid extract, and the are analyzed together. If incompatible, the liquids are analyzed parately and the results are mathematically combined to yield a volume-weighted averag
e concentration.
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3.0INTERFERENCES
3.1Potential interferences that may be encountered during analysis are discusd in the individual analytical methods.
4.0APPARATUS AND MATERIALS
4.1Agitation apparatus: The agitation apparatus must be capable of rotating the extraction vesl in an end-over-end fashion (e Figure 1) at 30 + 2 rpm. Suitable devices known to EPA are identified
in Table 2.
4.2Extraction Vesls
4.2.1Zero-Headspace Extraction Vesl (ZHE). This device is
for u only when the waste is being tested for the mobility of volatile analytes (i.e., tho listed in Table 1). The ZHE (depicted in Figure 2)allows for liquid/solid paration within the device, and effectively precludes headspace. This type of vesl allows for initial liquid/solid paration, extraction, and final extract filtration without opening the vesl (e Section 4.3.1). The vesls shall have an internal volume of 500-600 mL, and be equipped to accommodate a 90-110 mm filter. The devices contain VITON O-rings which should be replaced frequently. Suitable ZHE ®1devices known to EPA are identified in Table 3.
狮子座的男人For the ZHE to be acceptable for u, the piston within the ZHE
should be able to be moved with approximately 15 psi 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 analys 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 recheck the pressure.If the device does not have a built-in pressure gauge, pressurize the device to 50 psi, submerge it in water, and check for the prence 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 u gas pressure to actuate the ZHE piston, while others
u mechanical pressure (e Table 3). Whereas the volatiles procedure (e Section 7.3) refers to pounds per square inch (psi), for the mechanically actuated piston, the pressure applied is measured in torque-inch-pounds. Refer to the manufacturer's instructions as to the proper conversion.
4.2.2Bottle Extraction Vesl. 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 vesl.
The extraction bottles may be constructed from various materials, depending on the analytes to be analyzed and the nature of the waste (e Section 4.3.3). It is recommended that borosilicate glass bottles be ud instead of other types of glass, especially when inorganics are of concern. Plastic bottles, other than polytetrafluoroethylene, shall not be ud if organics are to be investigated. Bottles are available from a number of laboratory suppliers. When this type of extraction vesl is ud, the filtration device discusd in Section 4.3.2 is ud for initial liquid/solid paration and final extract filtration.
4.3Filtration Devices: It is recommended that all filtrations be performed in a hood.
4.3.1Zero-Headspace Extractor Vesl (ZHE): When the waste is
evaluated for volatiles, the zero-headspace extraction vesl described in Section 4.2.1 is ud 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 paration (50 psi).
NOTE:When it is suspected that the glass fiber filter has been ruptured, an in-line glass fiber filter may be ud to filter the material早春二月
within the ZHE.
4.3.2Filter Holder: When the waste is evaluated for other than
壮观的英文volatile analytes, any filter holder capable of supporting a glass fiber filter and able to withstand the pressure needed to accomplish paration may be ud. Suitable filter holders range from simple vacuum units to relatively complex systems capable of exerting pressures of up to 50 psi or more. The type of filter holder ud depends on the properties of the material to be filtered (e Section 4.3.3). The 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 ud 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.
4.3.3Materials of Construction: Extraction vesls and
中国大学100强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 ud when eva
luating the mobility of both organic and inorganic components. Devices made of high density polyethylene (HDPE), polypropylene (PP), or polyvinyl chloride (PVC) may be ud only when evaluating the mobility of metals. Borosili-CD-ROM1311- 3Revision 0
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cate glass bottles are recommended for u over other types of glass bottles, especially when inorganics are analytes of concern.
4.4Filters: 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 µm, or equivalent. Filters known to EPA which meet the specifications are identified in Table
5. Pre-filters must not be ud. When evaluating the mobility of metals, filters shall be acid-washed
prior to u by rinsing with 1N nitric acid followed by three concutive rins with deionized distilled water (a minimum of 1 L per rin is recommended). Glass fiber filters are fragile and should be handled with care.
4.5pH Meters: The meter should be accurate to + 0.05 units at 25 E C.
4.6ZHE Extract Collection Devices: TEDLAR bags or glass, stainless ®2steel or PTFE gas-tight syringes are ud to collect the initial liquid pha and the final extract of the waste when using the ZHE device. The devices listed are recommended for u under the following conditions:
4.6.1If a waste contains an aqueous liquid pha or if a waste does not contain a significant amount of nonaqueous liquid (i.e., <1% of total waste), the TEDLAR bag or a 600 mL syringe should be ud to collect ®and combine the initial liquid and solid extract.
兰陵王柳4.6.2If a waste contains a significant amount of nonaqueous liquid in the initial liquid pha (i.e., >1% of total waste), the syringe or the TEDLAR bag may be ud for both the initial solid/liquid paration ®and the final extract filtration. However, analysts should u one or the other, not both.
4.6.3If the waste contains no initial liquid pha (is 100%
solid) or has no significant solid pha (is 100% liquid), either the TEDLAR bag or the syringe may be ud. If the syringe is ud, discard ®the first 5 mL of liquid expresd from the device. The remaining aliquots are ud for analysis.
4.7ZHE 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 (e Section 4.3.2), or other ZHE device).
4.8Laboratory Balance: Any laboratory balance accurate to within + 0.01 grams may be ud (all weight measurements are to be within + 0.1 grams).
4.9Beaker or Erlenmeyer flask, glass, 500 mL.
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Watchglass, appropriate diameter to cover beaker or Erlenmeyer flask.
大年初五是什么日子4.11
Magnetic stirrer.
5.0 REAGENTS 5.1Reagent grade chemicals shall be ud in all tests. Unless otherwi 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 ud,provided it is first ascertained that the reagent is of sufficiently high purity to permit its u without lesning the accuracy of the determination.
5.2Reagent Water. Reagent water is defined as water in which an interferant is not obrved at or above the method's detection limit of the analyte(s) of interest. For nonvolatile extractions, ASTM Type II water or equivalent meets the definition of reagent water. For volatile extractions, it is recommended that reagent water be generated by any of the following methods.Reagent water should be monitored periodically for impurities.
5.2.1Reagent water for volatile extractions may be generated
by passing tap water through a carbon filter bed containing about 500grams of activated carbon (Calgon Corp., Filtrasorb-300 or equivalent).
5.2.2 A water purification system (Millipore Super-Q or
equivalent) may also be ud to generate reagent water for volatile extractions.
5.2.3Reagent water for volatile extractions may also be
prepared by boiling water for 15 minutes. Subquently, 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 al with a Teflon-lined ptum and cap.
5.3
Hydrochloric acid (1N), HCl, made from ACS reagent grade.5.4正月十五看花灯
Nitric acid (1N), HNO , made from ACS reagent grade.35.5
Sodium hydroxide (1N), NaOH, made from ACS reagent grade.5.6
Glacial acetic acid, CH CH OOH, ACS reagent grade.325.7Extraction fluid.
5.7.1Extraction fluid # 1: Add 5.7 mL glacial CH CH OOH to
32500 mL of reagent water (See Section 5.2), add 64.3 mL of 1N NaOH, and dilute to a volume of 1 liter. When correctly prepared, the pH of this fluid will be 4.93 + 0.05.
