U239 U200

U249

1330-20-7 Xylene (1)

1CAS Number given for parent compound only.

APPENDIX I-REPRESENTATIVE SAMPLING METHODS

The methods and equipment used for sampling waste materials will vary with the form and consistency of the waste materials to be sampled. Samples collected using the sampling protocols listed below, for sampling waste with properties similar to the indicated materials, will be considered by the Agency to be representative of the waste. Extremely viscous liquid-ASTM Standard D140-70 Crushed or powdered materialASTM Standard D346-75 Soil or rock-like material-ASTM Standard D420-69 Soillike material-ASTM Standard D1452-65 Fly Ash-like material-ASTM Standard D2234-76 [ASTM Standards are available from ASTM, 1916 Race St., Philadelphia, PA 19103]

Containerized liquid wastes-"COLIWASA" described in "Test Methods for the Evaluation of Solid Waste, Physical/Chemical Methods," U.S. Environmental Protection Agency, Office of Solid Waste, Washington, D.C. 20460. [Copies may be obtained from Solid Waste Information, U.S. Environmental Protection Agency, 26 W. St. Clair St., Cincinnati, Ohio 45268] Liquid waste in pits, ponds, lagoons, and similar reservoirs.-"Pond Sampler" described in "Test Methods for the Evaluation of Solid Waste, Physical/Chemical Methods."la

This manual also contains additional information on application of these protocols.

APPENDIX II-EP TOXICITY TEST PROCEDURES

A. Extraction Procedure (EP)

1. A representative sample of the waste to be tested (minimum size 100 grams) shall be obtained using the methods specified in Appendix I or any other method capable of yielding a representative sample within the meaning of Part 260. [For detailed guidance on conducting the various aspects of the EP see "Test Methods for the Evaluation of Solid Waste, Physical/Chemical Methods" (incorporated by reference, see § 260.11).]

2. The sample shall be separated into its component liquid and solid phases using the method described in "Separation Procedure" below. If the solid residue obtained using this method totals less than 0.5% of the original weight of the waste, the residue can be discarded and the operator shall treat the liquid phase as the extract and proceed immediately to Step 8.

3. The solid material obtained from the Separation Procedure shall be evaluated for its particle size. If the solid material has a surface area per gram of material equal to, or greater than, 3.1 cm2 or passes through a 9.5 mm (0.375 inch) standard sieve, the operator shall proceed to Step 4. 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

b The percent solids is determined by drying the filter pad at 80°C until it reaches constant weight and then calculating the percent solids using the following equation: Percent solids =

These methods are also described in "Samplers and Sampling Procedures for Hazardous Waste Streams," EPA 600/2-80018, January 1980.

(weight of pad + solid) (tare weight of pad) initial weight of sample

X 100

it passes through a 9.5 mm (0.375 inch) sieve or, if the material is in a single piece, by subjecting the material to the "Structural Integrity Procedure" described below.

4. The solid material obtained in Step 3 shall be weighed and placed in an extractor with 16 times its weight of deionized water. Do not allow the material to dry prior to weighing. For purposes of this test, an acceptable extractor is one which will impart sufficient agitation to the mixture to not only prevent stratification of the sample and extraction fluid but also insure that all sample surfaces are continuously brought into contact with well mixed extraction fluid.

5. After the solid material and deionized 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 greater than 5.0, the pH of the solution shall be decreased to 5.0 ± 0.2 by adding 0.5 N acetic acid. If the pH is equal to or less than 5.0, no acetic acid should be added. The pH of the solution shall be monitored, as described below, during the course of the extraction and if the pH rises above 5.2, 0.5N acetic acid shall be added to bring the pH down to 5.0 ± 0.2. However, in no event shall the aggregrate amount of acid added to the solution exceed 4 ml of acid per gram of solid. The mixture shall be agitated for 24 hours and maintained at 20°40°C (68°-104°F) 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:

(a) A pH meter shall be calibrated in accordance with the manufacturer's specifications.

(b) The pH of the solution shall be checked and, if necessary, 0.5N acetic acid shall be manually added to the extractor until the pH reaches 5.0±0.2. The pH of the solution shall be adjusted at 15, 30 and 60 minute intervals, moving to the next longer interval if the pH does not have to be adjusted more than 0.5N pH units.

(c) The adjustment procedure shall be continued for at least 6 hours.

(d) 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 gram of solids) has not been added, the pH shall be adjusted to 5.0 ± 0.2 and the extraction continued for an additional four hours, during which the pH shall be adjusted at one hour intervals.

6. At the end of the 24 hour extraction period, deionized water shall be added to

the extractor in an amount determined by the following equation: V=(20)(W)-16(W)-A

V=ml deionized water to be added W=weight in grams of solid charged to extractor

A=ml of 0.5N acetic acid added during extraction

7. The material in the extractor shall be separated into its component liquid and solid phases as described under “Separation Procedure."

8. The liquids resulting from Steps 2 and 7 shall be combined. This combined liquid (or the waste itself if it has less than 1⁄2 percent solids, as noted in Step 2) is the extract and shall be analyzed for the presence of any of the contaminants specified in Table I of § 261.24 using the Analytical Procedures designated below.

Separation Procedure

Equipment: A filter holder, designed for filtration media having a nominal pore size of 0.45 micrometers and capable of applying a 5.3 kg/cm2 (75 psi) hydrostatic pressure to the solution being filtered, shall be used. For mixtures containing nonabsorptive solids, where separation can be effected without imposing a 5.3 kg/cm2 pressure differential, vacuum filters employing a 0.45 micrometers filter media can be used. (For further guidance on filtration equipment or procedures see "Test Methods for Evaluating Solid Waste, Physical/Chemical Methods" incorporated by reference, see § 260.11). Procedure:2

(i) Following manufacturer's directions, the filter unit shall be assembled with a filter bed consisting of a 0.45 micrometer filter membrane. For difficult or slow to filter mixtures a prefilter bed consisting of the following prefilters in increasing pore size (0.65 micrometer membrane, fine glass

"This procedure is intended to result in separation of the "free" liquid portion of the waste from any solid matter having a particle size >0.45 μm. If the sample will not filter, various other separation techniques can be used to aid in the filtration. As described above, pressure filtration is employed to speed up the filtration process. This does not alter the nature of the separation. If liquid does not separate during filtration, the waste can be centrifuged. If separation occurs during centrifugation, the liquid portion (centrifugate) is filtered through the 0.45 μm filter prior to becoming mixed with the liquid portion of the waste obtained from the initial filtration. Any material that will not pass through the filter after centrifugation is considered a solid and is extracted.

fiber prefilter, and coarse glass fiber prefilter) can be used.

(ii) The waste shall be poured into the filtration unit.

(iii) The reservoir shall be slowly pressurized until liquid begins to flow from the filtrate outlet at which point the pressure in the filter shall be immediately lowered to 10-15 psig. Filtration shall be continued until liquid flow ceases.

(iv) The pressure shall be increased stepwise in 10 psi increments to 75 psig and filtration continued until flow ceases or the pressurizing gas begins to exit from the filtrate outlet.

(v) The filter unit shall be depressurized, the solid material removed and weighed and then transferred to the extraction appara

tus, or, in the case of final filtration prior to analysis, discarded. Do not allow the material retained on the filter pad to dry prior to weighing.

(vi) The liquid phase shall be stored at 4°C for subsequent use in Step 8.

B. Structural Integrity Procedure Equipment: A Structural Integrity Tester having a 3.18 cm (1.25 in.) diameter hammer weighing 0.33 kg (0.73 lbs.) and having 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 the specifications shown in Figure 1.