美国环保局 EPA 试验 方法美国环保局 EPA 试验 方法 9045dSoil and Waste pH

METHOD 9045D

SOIL AND WASTE pH

1.0SCOPE AND APPLICATION

1.1This method is an electrometric procedure for measuring pH in soils and waste samples. Wastes may be solids, sludges, or non-aqueous liquids. If water is present, it must constitute less than 20% of the total volume of the sample.

2.0SUMMARY OF METHOD

2.1The sample is mixed with reagent water, and the pH of the resulting aqueous solution is measured.

3.0INTERFERENCES

3.1Samples with very low or very high pH may give incorrect readings on the meter. For samples with a true pH of >10, the measured pH may be incorrectly low. This error can be minimized by using a low-sodium-error electrode. Strong acid solutions, with a true pH of <1, may give incorrectly high pH measurements.

3.2Temperature fluctuations will cause measurement errors.

3.3Errors will occur when the electrodes become coated. If an electrode becomes coated with an oily material that will not rinse free, the electrode can (1) be cleaned with an ultrasonic bath, or (2) be washed with detergent, rinsed several times with water, placed in 1:10 HCl so that the lower third of the electrode is submerged, and then thoroughly rinsed with water, or (3) be cleaned per the manufacturer's instructions.

4.0APPARATUS AND MATERIALS

4.1pH meter with means for temperature compensation.

4.2Glass electrode.

4.3Reference electrode -- A silver-silver chloride or other reference electrode of constant potential may be used.

NOTE:Combination electrodes incorporating both measuring and referenced functions are convenient to use and are available with solid, gel-type filling materials that require

minimal maintenance.

4.4Beaker -- 50-mL.

4.5Thermometer and/or temperature sensor for automatic compensation.

4.6Analytical balance -- capable of weighing 0.1 g.

5.0REAGENTS

5.1Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.

5.2Reagent water. All references to water in this method refer to reagent water, as defined in Chapter One.

5.3Primary standard buffer salts are available from the National Institute of Standards and Technology (NIST) and should be used in situations where extreme accuracy is necessary. Preparation of reference solutions from these salts requires some special precautions and handling, such as low-conductivity dilution water, drying ovens, and carbon-dioxide-free purge gas. These solutions should be replaced at least once each month.

5.4Secondary standard buffers may be prepared from NIST salts or purchased as solutions from commercial vendors. These commercially available solutions, which have been validated by comparison with NIST standards, are recommended for routine use.

6.0SAMPLE PRESERVATION AND HANDLING

Samples should be analyzed as soon as possible.

7.0PROCEDURE

7.1Calibration

7.1.1Because of the wide variety of pH meters and accessories, detailed

operating procedures cannot be incorporated into this method. Each analyst must be

acquainted with the operation of each system and familiar with all instrument functions.

Special attention to care of the electrodes is recommended.

7.1.2Each instrument/electrode system must be calibrated at a minimum of

two points that bracket the expected pH of the samples and are approximately three pH units or more apart. Repeat adjustments on successive portions of the two buffer

solutions until readings are within 0.05 pH units of the buffer solution value. If an

accurate pH reading based on the conventional pH scale [0 to 14 at 25 E C] is required, the analyst should control sample temperature at 25 ± 1 E C when sample pH approaches the alkaline end of the scale (e.g., a pH of 11 or above).

7.2Sample preparation and pH measurement of soils:

7.2.1To 20 g of soil in a 50-mL beaker, add 20 mL of reagent water, cover, and

continuously stir the suspension for 5 min. Additional dilutions are allowed if working with hygroscopic soils and salts or other problematic matrices.

7.2.2Let the soil suspension stand for about 1 hr to allow most of the

suspended clay to settle out from the suspension or filter or centrifuge off the aqueous

phase for pH measurement.

7.2.3Adjust the electrodes in the clamps of the electrode holder so that, upon

lowering the electrodes into the beaker, the glass electrode will be immersed just deep enough into the clear supernatant solution to establish a good electrical contact through the ground-glass joint or the fiber-capillary hole. Insert the electrodes into the sample

solution in this manner. For combination electrodes, immerse just below the suspension.

7.2.4If the sample temperature differs by more than 2 E C from the buffer

solution, the measured pH values must be corrected.

7.2.5Report the results as "soil pH measured in water at E C" where " E C" is

the temperature at which the test was conducted.

7.3Sample preparation and pH measurement of waste materials

7.3.1To 20 g of waste sample in a 50-mL beaker, add 20 mL of reagent water,

cover, and continuously stir the suspension for 5 min. Additional dilutions are allowed if working with hygroscopic wastes and salts or other problematic matrices.

7.3.2Let the waste suspension stand for about 15 min to allow most of the

suspended waste to settle out from the suspension or filter or centrifuge off aqueous

phase for pH measurement.

NOTE:If the waste is hygroscopic and absorbs all the reagent water, begin the

experiment again using 20 g of waste and 40 mL of reagent water.

NOTE:If the supernatant is multiphasic, decant the oily phase and measure the pH of the aqueous phase. The electrode may need to be cleaned (Step 3.3) if it

becomes coated with an oily material.

7.3.3Adjust the electrodes in the clamps of the electrode holder so that, upon

lowering the electrodes into the beaker, the glass electrode will be immersed just deep enough into the clear supernatant to establish good electrical contact through the ground-glass joint or the fiber-capillary hole. Insert the electrode into the sample solution in this manner. For combination electrodes, immerse just below the suspension.

7.3.4If the sample temperature differs by more than 2 E C from the buffer

solution, the measured pH values must be corrected.

7.3.5Report the results as "waste pH measured in water at E C" where " E C"

is the temperature at which the test was conducted.

8.0QUALITY CONTROL

8.1Refer to Chapter One for the appropriate QC protocols.

8.2Electrodes must be thoroughly rinsed between samples.

9.0METHOD PERFORMANCE

9.1No data provided.

10.0REFERENCES

1.Black, Charles Allen; Methods of Soil Analysis; American Society of Agronomy:

Madison, WI, 1973.

2.National Bureau of Standards, Standard Reference Material Catalog, 1986-87, Special

Publication 260.

METHOD 9045D SOIL AND WASTE pH

美国环保局 EPA 试验 方法 3541

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美国EPA通用土壤筛选值

美国EPA通用土壤筛选值

美国EPA通用土壤筛选值

CAS 号污染 物 土壤（mg/kg） 地下 （μg/L 居 住 备 注 工 业 备 注 基于 地下 水保 护 饮用 水 1 +04 E+0 5 +00 +04 75-86- 5 丙酮氰 醇 2.0E +02 n 2.1 E+0 3 n 1.2E -02 5.8E +01 75-05- 8 乙腈 8.7E +02 n 3.7 E+0 3 n 2.6E -02 1.3E +02 98-86- 2 乙酰苯 7.8E +03 ns 1.0 E+0nms 1.1E +00 3.7E +03

CAS 号污染 物 土壤（mg/kg） 地下 （μg/L 居 住 备 注 工 业 备 注 基于 地下 水保 护 饮用 水 -8 -01 E-0 1 -06 -02 79-06- 1 丙烯酰 胺 2.3E -01 c 3.4 E+0 c 9.1E -06 4.3E -02 79-10- 7 丙烯酸 3.0E +04 n 2.9 E+0 5 nm 3.7E +00 1.8E +04 107-13 -1 丙烯腈 2.4E -01 c* 1.2 E+0c* 9.9E -06 4.5E -02

CAS 号污染 物 土壤（mg/kg） 地下 （μg/L 居 住 备 注 工 业 备 注 基于 地下 水保 护 饮用 水 60-8 +00 E+0 1 -04 +00 116-06 -3 涕灭威 6.1E +01 n 6.2 E+0 2 n 9.1E -03 3.7E +01 1646-8 8-4 涕灭威 砜 6.1E +01 n 6.2 E+0 2 n 8.0E -03 3.7E +01 309-00 -2 艾氏剂 2.9E -02 c* 1.0 E-0 c 6.5E -04 4.0E -03

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美国环保局 EPA 试验 方法 9066Phenolics (Colorimetric, Automated 4-AAP with Distillation)

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美国环保局 EPA 试验 方法 8318

METHOD 8318 N-METHYLCARBAMATES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC) 1.0SCOPE AND APPLICATION 1.1Method 8318 is used to determine the concentration of N-methylcarbamates in soil, water and waste matrices. The following compounds can be determined by this method: _______________________________________________________________________________ Compound Name CAS No.a ________________________________________________________________________________ Aldicarb (Temik) 116-06-3 Aldicarb Sulfone 1646-88-4 Carbaryl (Sevin) 63-25-2 Carbofuran (Furadan) 1563-66-2 Dioxacarb 6988-21-2 3-Hydroxycarbofuran16655-82-6 Methiocarb (Mesurol) 2032-65-7 Methomyl (Lannate)16752-77-5 Promecarb 2631-37-0 Propoxur (Baygon) 114-26-1 ________________________________________________________________________________ a Chemical Abstract Services Registry Number. 1.2The method detection limits (MDLs) of Method 8318 for determining the target analytes in organic-free reagent water and in soil are listed in Table 1. 1.3This method is restricted to use by, or under the supervision of, analysts experienced in the use of high performance liquid chromatography (HPLC) and skilled in the interpretation of chromatograms. Each analyst must demonstrate the ability to generate acceptable results with this method. 2.0SUMMARY OF METHOD 2.1N-methylcarbamates are extracted from aqueous samples with methylene chloride, and from soils, oily solid waste and oils with acetonitrile. The extract solvent is exchanged to methanol/ethylene glycol, and then the extract is cleaned up on a C-18 cartridge, filtered, and eluted on a C-18 analytical column. After separation, the target analytes are hydrolyzed and derivatized post-column, then quantitated fluorometrically. 2.2Due to the specific nature of this analysis, confirmation by a secondary method is not essential. However, fluorescence due to post-column derivatization may be confirmed by substituting the NaOH and o-phthalaldehyde solutions with organic-free reagent water and reanalyzing the sample. If

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3、潜力因素值F（Potency Factor Estimate） 潜力因素值F定义为1/ED 10。ED 10 等于10%终身致癌风险的致癌剂剂量。 F可以和致癌性的确认证据一起，用来划分化学品潜在致癌性的危险等级。 4、潜力因素分组（Potency factor Grouping） 由于潜力因素值F可表示致癌危险性的相对大小，因而，可将潜在致癌剂的相对潜力因素分为4组。潜力因素最高的化学品分在1组，中等潜力因素的为2组，低潜力因素的为3组，最低潜力因素的为4组。 5、致癌危害等级（Cancer Hazard Ranking） 根据人和动物试验所取得的致癌性证据，结合潜力因素分组数据，可将化学品致癌危害等级分为高、中、低3级。

美国EPA标准方法

DETERMINATION OF ETHYLENE THIOUREA (ETU) IN WATER USING GAS CHROMATOGRAPHY WITH A NITROGEN-PHOSPHORUS DETECTOR Revision 1.0 December 1992 D.J. Munch and R.L. Graves T.M. Engel and S.T. Champagne Battelle, Columbus Division ENVIRONMENTAL MONITORING SYSTEMS LABORATORY OFFICE OF RESEARCH AND DEVELOPMENT U.S. ENVIRONMENTAL PROTECTION AGENCY CINCINNATI, OHIO 45268 509-1

DETERMINATION OF ETHYLENE THIOUREA (ETU) IN WATER USING GAS CHROMATOGRAPHY WITH A NITROGEN-PHOSPHORUS DETECTOR 1.0SCOPE AND APPLICATION 1.1This method utilizes gas chromatography (GC) to determine ethylene thiourea (ETU, Chemical Abstracts Registry No. 96-45-7) in water. 1.2This method has been validated in a single laboratory during development. 1 The method detection limit (MDL) has been determined in reagent water and is listed in Table 2. Method detection limits may vary among laboratories, depending upon the analytical instrumentation used and the experience of the analyst. In addition to the work done during the development of this method and its use in the National Pesticide Survey, an interlaboratory method validation study of this method has been conducted. 1.3This method is restricted to use by or under the supervision of analysts experienced in the use of GC and in the interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results with this method using the procedure described in Section 9.3. 1.4When a tentative identification of ETU is made using the recommended primary GC column (Section 6.7.1), it must be confirmed by at least one additional qualitative technique. This technique may be the use of the confirmation GC column (Section 6.7.2) with the nitrogen-phosphorus detector or analysis using a gas chromatograph/mass spectrometer (GC/MS). 2.0SUMMARY OF METHOD 2.1The ionic strength and pH of a measured 50 mL aliquot of sample are adjusted by addition of ammonium chloride and potassium fluoride. The sample is poured onto an Extrelut column. ETU is eluted from the column in 400 mL of methylene chloride. A free radical scavenger is then added in excess to the eluate. The methylene chloride eluant is concentrated to a volume of 5 mL after solvent substitution with ethyl acetate. Gas chromatographic conditions are described which permit the separation and measurement of ETU with a nitrogen-phosphorus detector (NPD). 3.0DEFINITIONS 3.1Artificial Ground Water -- An aqueous matrix designed to mimic a real ground water sample. The artificial ground water should be reproducible for use by others. 509-2

美国环保局 EPA 试验 方法 504_1

1,2-DIBROMOETHANE (EDB), 1,2-DIBROMO-3-CHLORO-PROPANE (DBCP), AND 1,2,3-TRICHLOROPROPANE (123TCP) IN WATER BY MICROEXTRACTION AND GAS CHROMATOGRAPHY Revision 1.1 Edited by J.W. Munch (1995) T. W. Winfield - Method 504, Revision 1.0 (1986) T. W. Winfield - Method 504, Revision 2.0 (1989) James W. Eichelberger - Method 504.1, Revision 1.0 (1993) NATIONAL EXPOSURE RESEARCH LABORATORY OFFICE OF RESEARCH AND DEVELOPMENT U.S. ENVIRONMENTAL PROTECTION AGENCY CINCINNATI, OHIO 45268 504.1-1

1,2-DIBROMOETHANE (EDB), 1,2-DIBROMO-3-CHLOROPROPANE (DBCP), AND 1,2,3-TRICHLOROPROPANE (123TCP) IN WATER BY MICROEXTRACTION AND GAS CHROMATOGRAPHY 1.0SCOPE AND APPLICATION 1-3 1.1This method is applicable to the determination of the following compounds in finished drinking water and groundwater: Chemical Abstract Services Analyte Registry Number 1,2-Dibromoethane106-93-4 1,2-Dibromo-3-Chloropropane96-12-8 1,2,3-Trichloropropane96-18-4 1.2For compounds other than the above mentioned analytes, or for other sample sources, the analyst must demonstrate the usefulness of the method by collecting precision and accuracy data on actual samples and provide qualitative confirmation of results by gas chromatography/mass spectrometry (GC/MS).4 5 1.3The experimentally determined method detection limits (MDL) for EDB and DBCP were calculated to be 0.01 μg/L and the MDL for 123TCP was calculated to be 0.02 μg/L. The method has been useful for these analytes over a concentration range from approximately 0.03-200 μg/L. Actual detection limits are highly dependent upon the characteristics of the gas chromatographic system used. 2.0SUMMARY OF METHOD 2.1Thirty-five mL of sample are extracted with 2 mL of hexane. Two μL of the extract are then injected into a gas chromatograph equipped with a linearized electron capture detector for separation and detection. Analytes are quantitated using procedural standard calibration (Section 3.12). 2.2The extraction and analysis time is 30-50 minutes per sample depending upon the analytical conditions chosen. 2.3Confirmatory evidence should be obtained for all positive results. This data may be obtained by using retention data from a dissimilar column, or when concentrations are sufficiently high by GC/MS. Purge and trap techniques using Methods 502.2 or 524.2 may also be used. Confirmation of all positive results of EDB are especially important, because of the potential for misidentification of dibromochloromethane (DBCM) as EDB. 504.1-2

美国环保局 EPA 试验 方法9012bTotal and Amenable Cyanide (Automated Colorimetric, with Off-Line Dis

METHOD 9012B TOTAL AND AMENABLE CYANIDE (AUTOMATED COLORIMETRIC, WITH OFF-LINE DISTILLATION) 1.0 SCOPE AND APPLICATION 1.1 This method is used to determine the concentration of inorganic cyanide (CAS Registry Number 57-12-5) in wastes or leachate. This method detects inorganic cyanides that are present as either soluble salts or complexes. It is used to determine values for both total cyanide and cyanide amenable to chlorination. The "reactive" cyanide content of a waste is not determined by this method. Refer to 40 CFR 261.23 for information on the characteristic of reactivity. 2.0 SUMMARY OF METHOD 2.1 The cyanide, as hydrocyanic acid (HCN), is released from samples containing cyanide by means of a reflux-distillation operation under acidic conditions and absorbed in a scrubber containing sodium hydroxide solution. The cyanide ion in the absorbing solution is then determined by automated UV colorimetry. 2.2 In the automated colorimetric measurement, the cyanide is converted to cyanogen chloride (CNCl) by reaction with Chloramine-T at a pH less than 8 without hydrolyzing to the cyanate. After the reaction is complete, color is formed on the addition of pyridine-barbituric acid reagent. The concentration of NaOH must be the same in the standards, the scrubber solutions, and any dilution of the original scrubber solution to obtain colors of comparable intensity. 3.0 INTERFERENCES 3.1Interferences are eliminated or reduced by using the distillation procedure. Chlorine and sulfide are interferences in this method. 3.2Oxidizing agents such as chlorine decompose most cyanides. Chlorine interferences can be removed by adding an excess of sodium arsenite to the waste prior to preservation and storage of the sample to reduce the chlorine to chloride which does not interfere. 3.3Sulfide interference can be removed by adding an excess of bismuth nitrate to the waste (to precipitate the sulfide) before distillation. Samples that contain hydrogen sulfide, metal sulfides, or other compounds that may produce hydrogen sulfide during the distillation should be treated by the addition of bismuth nitrate. 3.4High results may be obtained for samples that contain nitrate and/or nitrite. During the distillation, nitrate and nitrite will form nitrous acid, which will react with some organic compounds to form oximes. These compounds once formed will decompose under test conditions to generate HCN. The possibility of interference of nitrate and nitrite is eliminated by pretreatment with sulfamic acid just before distillation. Nitrate and nitrite are interferences when present at levels higher than 10 mg/L and in conjunction with certain organic compounds.