METHOD 8290
POLYCHLORINATED DIBENZODIOXINS (PCDDs) AND POLYCHLORINATED DIBENZOFURANS (PCDFs)BY HIGH-RESOLUTION GAS CHROMATOGRAPHY/HIGH-RESOLUTION
MASS SPECTROMETRY (HRGC/HRMS)
1.0SCOPE AND APPLICATION
1.1This method provides procedures for the detection and quantitative measurement of polychlorinated dibenzo-p-dioxins (tetra- through octachlorinated homologues; PCDDs), and polychlorinated dibenzofurans (tetra- through octachlorinated homologues; PCDFs) in a variety of environmental matrices and at part-per-trillion (ppt) to part-per-quadrillion (ppq) concentrations. The following compounds can be determined by this method:
_______________________________________________________________________________
Compound Name CAS No a 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) 1746-01-6
1,2,3,7,8-Pentachlorodibenzo-p-dioxin (PeCDD)40321-76-4
1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin (HxCDD)57653-85-7
1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin (HxCDD)39227-28-6
1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin (HxCDD)19408-74-3
1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin (HpCDD)35822-39-4
1,2,3,4,6,7,8,9-Octachlorodibenzo-p-dioxin (OCDD) 3268-87-9
2,3,7,8-Tetrachlorodibenzofuran (TCDF)51207-31-9
1,2,3,7,8-Pentachlorodibenzofuran (PeCDF)57117-41-6
2,3,4,7,8-Pentachlorodibenzofuran (PeCDF)57117-31-4
1,2,3,6,7,8-Hexachlorodibenzofuran (HxCDF)57117-44-9
1,2,3,7,8,9-Hexachlorodibenzofuran (HxCDF)72918-21-9
1,2,3,4,7,8-Hexachlorodibenzofuran (HxCDF)70648-26-9
2,3,4,6,7,8-Hexachlorodibenzofuran (HxCDF)60851-34-5
1,2,3,4,6,7,8-Heptachlorodibenzofuran (HpCDF)67562-39-4
1,2,3,4,7,8,9-Heptachlorodibenzofuran (HpCDF)55673-89-7
1,2,3,4,6,7,8,9-Octachlorodibenzofuran (OCDF)39001-02-0
________________________________________________________________________________ a
Chemical Abstract Service Registry Number
1.2The analytical method calls for the use of high-resolution gas chromatography and high-resolution mass spectrometry (HRGC/HRMS) on purified sample extracts. Table 1 lists the various sample types covered by this analytical protocol, the 2,3,7,8-TCDD-based method calibration limits (MCLs), and other pertinent information. Samples containing concentrations of specific congeneric analytes (PCDDs and PCDFs) considered within the scope of this method that are greater than ten times the upper MCLs must be analyzed by a protocol designed for such concentration levels, e.g., Method 8280. An optional method for reporting the analytical results using a 2,3,7,8-TCDD toxicity equivalency factor (TEF) is described.
1.3The sensitivity of this method is dependent upon the level of inter-ferences within a given matrix. The calibration range of the method for a 1 L water sample is 10 to 2000 ppq for TCDD/TCDF and PeCDD/PeCDF, and 1.0 to 200 ppt for a 10 g soil, sediment, fly ash, or tissue sample for the same analytes (Table 1). Analysis of a one-tenth aliquot of the sample permits measurement of concentrations up to 10 times the upper MCL. The actual limits of detection and quantitation will differ from the lower MCL, depending on the complexity of the matrix.
1.4This method is designed for use by analysts who are experienced with residue analysis and skilled in HRGC/HRMS.
1.5Because of the extreme toxicity of many of these compounds, the analyst must take the necessary precautions to prevent exposure to materials known or believed to contain PCDDs or PCDFs. It is the responsibility of the laboratory personnel to ensure that safe handling procedures are employed. Sec.11 of this method discusses safety procedures.
2.0SUMMARY OF METHOD
2.1This procedure uses matrix specific extraction, analyte specific cleanup, and HRGC/HRMS analysis techniques.
2.2If interferences are encountered, the method provides selected cleanup procedures to aid the analyst in their elimination. A simplified analysis flow chart is presented at the end of this method.
2.3 A specified amount (see Table 1) of soil, sediment, fly ash, water,sludge (including paper pulp), still bottom, fuel oil, chemical reactor residue,fish tissue, or human adipose tissue is spiked with a solution containing specified amounts of each of the nine isotopically (C ) labeled PCDDs/PCDFs 1312listed in Column 1 of Table 2. The sample is then extracted according to a matrix specific extraction procedure. Aqueous samples that are judged to contain 1 percent or more solids, and solid samples that show an aqueous phase, are filtered, the solid phase (including the filter) and the aqueous phase extracted separately, and the extracts combined before extract cleanup. The extraction procedures are:
a)
Toluene: Soxhlet extraction for soil, sediment, fly ash, and paper pulp samples;
b)
Methylene chloride: liquid-liquid extraction for water samples; c)Toluene: Dean-Stark extraction for fuel oil, and aqueous sludge
samples;
d)Toluene extraction for still bottom samples;
e)Hexane/methylene chloride: Soxhlet extraction or methylene
chloride: Soxhlet extraction for fish tissue samples; and
f)
Methylene chloride extraction for human adipose tissue samples.
g)As an option, all solid samples (wet or dry) may be extracted with
toluene using a Soxhlet/Dean Stark extraction system.
The decision for the selection of an extraction procedure for chemical reactor residue samples is based on the appearance (consistency, viscosity) of the samples. Generally, they can be handled according to the procedure used for still bottom (or chemical sludge) samples.
2.4The extracts are submitted to an acid-base washing treatment and dried. Following a solvent exchange step, the extracts are cleaned up by column chromatography on alumina, silica gel, and activated carbon.
2.4.1The extracts from adipose tissue samples are treated with
silica gel impregnated with sulfuric acid before chromatography on acidic silica gel, neutral alumina, and activated carbon.
2.4.2Fish tissue and paper pulp extracts are subjected to an acid
wash treatment only, prior to chromatography on alumina and activated carbon.
2.5The preparation of the final extract for HRGC/HRMS analysis is accomplished by adding 10 to 50 μL (depending on the matrix) of a nonane solution containing 50 pg/μL of the recovery standards C -1,2,3,4-TCDD and 1312C -1,2,3,7,8,9-HxCDD (Table 2). The former is used to determine the percent 1312recoveries of tetra- and pentachlorinated PCDD/PCDF congeners, while the latter is used to determine the percent recoveries of the hexa-, hepta- and octachlorinated PCDD/PCDF congeners.
2.6Two μL of the concentrated extract are injected into an HRGC/HRMS system capable of performing selected ion monitoring at resolving powers of at least 10,000 (10 percent valley definition).
2.7The identification of OCDD and nine of the fifteen 2,3,7,8-substituted congeners (Table 3), for which a C-labeled standard is available 13in the sample fortification and recovery standard solutions (Table 2), is based on their elution at their exact retention time (within 0.005 retention time units measured in the routine calibration) and the simultaneous detection of the two most abundant ions in the molecular ion region. The remaining six 2,3,7,8-substituted congeners (i.e., 2,3,4,7,8-PeCDF; 1,2,3,4,7,8-HxCDD; 1,2,3,6,7,8-HxCDF; 1,2,3,7,8,9-HxCDF; 2,3,4,6,7,8-HxCDF, and 1,2,3,4,7,8,9-HpCDF), for which no carbon-labeled internal standards are available in the sample fortification solution, and all other PCDD/PCDF congeners are identified when their relative retention times fall within their respective PCDD/PCDF retention time windows,as established from the routine calibration data, and the simultaneous detection of the two most abundant ions in the molecular ion region. The identification of OCDF is based on its retention time relative to C -OCDD and the simultaneous 1312detection of the two most abundant ions in the molecular ion region.Identification also is based on a comparison of the ratios of the integrated ion abundance of the molecular ion species to their theoretical abundance ratios.
2.8Quantitation of the individual congeners, total PCDDs and total PCDFs is achieved in conjunction with the establishment of a multipoint (five points)
calibration curve for each homologue, during which each calibration solution is analyzed once.
3.0INTERFERENCES
3.1Solvents, reagents, glassware and other sample processing hardware may yield discrete artifacts or elevated baselines that may cause misinter-pretation of the chromatographic data (see references 1 and 2.) All of these materials must be demonstrated to be free from interferants under the conditions of analysis by performing laboratory method blanks. Analysts should avoid using PVC gloves.
3.2The use of high purity reagents and solvents helps minimize interference problems. Purification of solvents by distillation in all-glass systems may be necessary.
3.3Interferants coextracted from the sample will vary considerably from matrix to matrix. PCDDs and PCDFs are often associated with other interfering chlorinated substances such as polychlorinated biphenyls (PCBs), polychlorinated diphenyl ethers (PCDPEs), polychlorinated naphthalenes, and polychlorinated alkyldibenzofurans, that may be found at concentrations several orders of magnitude higher than the analytes of interest. Retention times of target analytes must be verified using reference standards. These values must correspond to the retention time windows established in Sec. 8.1.1.3. While cleanup techniques are provided as part of this method, unique samples may require additional cleanup steps to achieve lower detection limits.
3.4 A high-resolution capillary column (60 m DB-5, J&W Scientific, or equivalent) is used in this method. However, no single column is known to resolve all isomers. The 60 m DB-5 GC column is capable of 2,3,7,8-TCDD isomer specificity (Sec. 8.1.1). In order to determine the concentration of the 2,3,7,8-TCDF (if detected on the DB-5 column), the sample extract must be reanalyzed on a column capable of 2,3,7,8-TCDF isomer specificity (e.g., DB-225, SP-2330, SP-2331, or equivalent).
4.0APPARATUS AND MATERIALS
4.1High-Resolution Gas Chromatograph/High-Resolution Mass Spectrometer/Data System (HRGC/HRMS/DS) - The GC must be equipped for temperature programming, and all required accessories must be available, such as syringes, gases, and capillary columns.
4.1.1GC Injection Port - The GC injection port must be designed for
capillary columns. The use of splitless injection techniques is recommended. On column 1 μL injections can be used on the 60 m DB-5 column. The use of a moving needle injection port is also acceptable.
When using the method described in this protocol, a 2 μL injection volume is used consistently (i.e., the injection volumes for all extracts, blanks, calibration solutions and the performance check samples are 2 μL).
One μL injections are allowed; however, laboratories must remain
consistent throughout the analyses by using the same injection volume at all times.
4.1.2Gas Chromatograph/Mass Spectrometer (GC/MS) Interface - The
o
GC/MS interface components should withstand 350C. The interface must be designed so that the separation of 2,3,7,8-TCDD from the other TCDD isomers achieved in the gas chromatographic column is not appreciably degraded. Cold spots or active surfaces (adsorption sites) in the GC/MS interface can cause peak tailing and peak broadening. It is recommended that the GC column be fitted directly into the mass spectrometer ion source without being exposed to the ionizing electron beam. Graphite ferrules should be avoided in the injection port because they may adsorb
TM
the PCDDs and PCDFs. Vespel, or equivalent, ferrules are recommended.
4.1.3Mass Spectrometer - The static resolving power of the instrument must be maintained at a minimum of 10,000 (10 percent valley).
4.1.4Data System - A dedicated data system is employed to control the rapid multiple-ion monitoring process and to acquire the data. Quantitation data (peak areas or peak heights) and SIM traces (displays of intensities of each ion signal being monitored including the lock-mass ion as a function of time) must be acquired during the analyses and stored. Quantitations may be reported based upon computer generated peak areas or upon measured peak heights (chart recording). The data system must be capable of acquiring data at a minimum of 10 ions in a single scan. It is also recommended to have a data system capable of switching to different sets of ions (descriptors) at specified times during an HRGC/HRMS acquisition. The data system should be able to provide hard copies of individual ion chromatograms for selected gas chromatographic time intervals. It should also be able to acquire mass spectral peak profiles (Sec. 8.1.2.3) and provide hard copies of peak profiles to demonstrate the required resolving power. The data system should permit the measurement of noise on the base line.
NOTE:The detector ADC zero setting must allow peak-to-peak measure-ment of the noise on the base line of every monitored channel
and allow for good estimation of the instrument resolving
power. In Figure 2, the effect of different zero settings on
the measured resolving power is shown.
4.2GC Columns
4.2.1In order to have an isomer specific determination for 2,3,7,8-TCDD and to allow the detection of OCDD/OCDF within a reasonable time interval in one HRGC/HRMS analysis, use of the 60 m DB-5 fused silica capillary column is recommended. Minimum acceptance criteria must be demonstrated and documented (Sec. 8.2.2). At the beginning of each 12 hour period (after mass resolution and GC resolution are demonstrated) during which sample extracts or concentration calibration solutions will be analyzed, column operating conditions must be attained for the required separation on the column to be used for samples. Operating conditions known to produce acceptable results with the recommended column are shown in Sec. 7.6.
4.2.2Isomer specificity for all 2,3,7,8-substituted PCDDs/PCDFs
cannot be achieved on the 60 m DB-5 GC column alone. In order to determine the proper concentrations of the individual 2,3,7,8-substituted congeners, the sample extract must be reanalyzed on another GC column that resolves the isomers.
4.2.330 m DB-225 fused silica capillary column, (J&W Scientific) or
equivalent.
4.3Miscellaneous Equipment and Materials - The following list of items does not necessarily constitute an exhaustive compendium of the equipment needed for this analytical method.
4.3.1Nitrogen evaporation apparatus with variable flow rate.
4.3.2Balances capable of accurately weighing to 0.01 g and
0.0001 g.
4.3.3Centrifuge.
4.3.4Water bath, equipped with concentric ring covers and capable
o
of being temperature controlled within + 2C.
4.3.5Stainless steel or glass container large enough to hold
contents of one pint sample containers.
4.3.6Glove box.
4.3.7Drying oven.
4.3.8Stainless steel spoons and spatulas.
4.3.9Laboratory hoods.
4.3.10Pipets, disposable, Pasteur, 150 mm long x 5 mm ID.
4.3.11Pipets, disposable, serological, 10 mL, for the
preparation of the carbon columns specified in Sec. 7.5.3.
4.3.12Reaction vial, 2 mL, silanized amber glass (Reacti-vial,
or equivalent).
4.3.13Stainless steel meat grinder with a 3 to 5 mm hole size
inner plate.
4.3.14Separatory funnels, 125 mL and 2000 mL.
4.3.15Kuderna-Danish concentrator, 500 mL, fitted with 10 mL
concentrator tube and three ball Snyder column.
TM
4.3.16Teflon or carborundum (silicon carbide) boiling chips
(or equivalent), washed with hexane before use.
TM
NOTE:Teflon boiling chips may float in methylene chloride, may not work in the presence of any water phase, and may be penetrated
by nonpolar organic compounds.
4.3.17Chromatographic columns, glass, 300 mm x 10.5 mm, fitted
TM
with Teflon stopcock.
4.3.18Adapters for concentrator tubes.
4.3.19Glass fiber filters, 0.70 μm, Whatman GFF, or equivalent.
4.3.20Dean-Stark trap, 5 or 10 mL, with T-joints, condenser and 125 mL flask.
4.3.21Continuous liquid-liquid extractor.
4.3.22All glass Soxhlet apparatus, 500 mL flask.
4.3.23Soxhlet/Dean Stark extractor (optional), all glass, 500 mL flask.
4.3.24Glass funnels, sized to hold 170 mL of liquid.
4.3.25Desiccator.
4.3.26Solvent reservoir (125 mL), Kontes; 12.35 cm diameter (special order item), compatible with gravity carbon column.
4.3.27Rotary evaporator with a temperature controlled water bath.
4.3.28High speed tissue homogenizer, equipped with an EN-8 probe, or equivalent.
4.3.29Glass wool, extracted with methylene chloride, dried and stored in a clean glass jar.
4.3.30Extraction jars, glass, 250 mL, with teflon lined screw cap.
4.3.31Volumetric flasks, Class A - 10 mL to 1000 mL.
4.3.32Glass vials, 1 dram (or metric equivalent).
NOTE:Reuse of glassware should be minimized to avoid the risk of contamination. All glassware that is reused must be
scrupulously cleaned as soon as possible after use, according
to the following procedure: Rinse glassware with the last
solvent used in it. Wash with hot detergent water, then rinse
with copious amounts of tap water and several portions of
organic-free reagent water. Rinse with high purity acetone
and hexane and store it inverted or capped with solvent rinsed
aluminum foil in a clean environment.
5.0REAGENTS AND STANDARD SOLUTIONS
5.1Organic-free reagent water - All references to water in this method refer to organic-free reagent water, as defined in Chapter One.
5.2Column Chromatography Reagents
5.2.1Alumina, neutral, 80/200 mesh (Super 1, Woelm?, or
equivalent). Store in a sealed container at room temperature, in a desiccator, over self-indicating silica gel.
5.2.2Alumina, acidic AG4, (Bio Rad Laboratories catalog #132-1240,
or equivalent). Soxhlet extract with methylene chloride for 24 hours if blanks show contamination, and activate by heating in a foil covered glass
o
container for 24 hours at 190C. Store in a glass bottle sealed with a TM
Teflon lined screw cap.
5.2.3Silica gel, high purity grade, type 60, 70-230 mesh; Soxhlet
extract with methylene chloride for 24 hours if blanks show contamination, and activate by heating in a foil covered glass container for 24 hours at o TM
190C. Store in a glass bottle sealed with a Teflon lined screw cap.
5.2.4Silica gel impregnated with sodium hydroxide. Add one part
(by weight) of 1 M NaOH solution to two parts (by weight) silica gel (extracted and activated) in a screw cap bottle and mix with a glass rod
TM until free of lumps. Store in a glass bottle sealed with a Teflon lined screw cap.
5.2.5Silica gel impregnated with 40 percent (by weight) sulfuric
acid. Add two parts (by weight) concentrated sulfuric acid to three parts (by weight) silica gel (extracted and activated), mix with a glass rod until free of lumps, and store in a screw capped glass bottle. Store in
TM
a glass bottle sealed with a Teflon lined screw cap.
5.2.6Celite 545? (Supelco), or equivalent.
5.2.7Active carbon AX-21 (Anderson Development Co., Adrian, MI), or
o equivalent, prewashed with methanol and dried in vacuo at 110C. Store in
TM
a glass bottle sealed with a Teflon lined screw cap.
5.3Reagents
5.3.1Sulfuric acid, H SO, concentrated, ACS grade, specific gravity
24
1.84.
5.3.2Potassium hydroxide, KOH, ACS grade, 20 percent (w/v) in
organic-free reagent water.
5.3.3Sodium chloride, NaCl, analytical reagent, 5 percent (w/v) in
organic-free reagent water.
5.3.4Potassium carbonate, K CO, anhydrous, analytical reagent.
23
5.4Desiccating agent
5.4.1Sodium sulfate (powder, anhydrous), Na SO. Purify by heating
24
o
at 400C for 4 hours in a shallow tray, or by precleaning the sodium sulfate with methylene chloride. If the sodium sulfate is precleaned with methylene chloride, a method blank must be analyzed, demonstrating that there is no interference from the sodium sulfate.
5.5Solvents
5.5.1Methylene chloride, CH Cl. High purity, distilled in glass
22
or highest available purity.
5.5.2Hexane, C H. High purity, distilled in glass or highest
614
available purity.
5.5.3Methanol, CH OH. High purity, distilled in glass or highest
3
available purity.
5.5.4Nonane, C H. High purity, distilled in glass or highest
920
available purity.
5.5.5Toluene, C H CH. High purity, distilled in glass or highest
653
available purity.
5.5.6Cyclohexane, C H. High purity, distilled in glass or highest
612
available purity.
5.5.7Acetone, CH C0CH. High purity, distilled in glass or highest
33
available purity.
5.6High-Resolution Concentration Calibration Solutions (Table 5) - Five nonane solutions containing unlabeled (totaling 17) and carbon-labeled (totaling 11) PCDDs and PCDFs at known concentrations are used to calibrate the instrument. The concentration ranges are homologue dependent, with the lowest values for the tetrachlorinated dioxin and furan (1.0 pg/μL) and the highest values for the octachlorinated congeners (1000 pg/μL).
5.6.1Depending on the availability of materials, these high-
resolution concentration calibration solutions may be obtained from the Environmental Monitoring Systems Laboratory, U.S. EPA, Cincinnati, Ohio.
However, additional secondary standards must be obtained from commercial sources, and solutions should be prepared in the analyst's laboratory. It is the responsibility of the laboratory to ascertain that the calibration solutions received (or prepared) are indeed at the appropriate concentrations before they are used to analyze samples.
5.6.2Store the concentration calibration solutions in 1 mL
minivials at room temperature in the dark.
5.7GC Column Performance Check Solution - This solution contains the first and last eluting isomers for each homologous series from tetra- through heptachlorinated congeners. The solution also contains a series of other TCDD isomers for the purpose of documenting the chromatographic resolution. The C -2,3,7,8-TCDD is also present. The laboratory is required to use nonane as 1312the solvent and adjust the volume so that the final concentration does not exceed 100 pg/μL per congener. Table 7 summarizes the qualitative composition (minimum requirement) of this performance evaluation solution.
5.8Sample Fortification Solution - This nonane solution contains the nine internal standards at the nominal concentrations that are listed in Table 2.The solution contains at least one carbon-labeled standard for each homologous series, and it is used to measure the concentrations of the native substances.(Note that C -OCDF is not present in the solution.)
13125.9Recovery Standard Solution - This nonane solution contains two
recovery standards, C -1,2,3,4-TCDD and C -1,2,3,7,8,9-HxCDD, at a nominal
13131212concentration of 50 pg/μL per compound. 10 to 50 μL of this solution will be spiked into each sample extract before the final concentration step and HRGC/HRMS analysis.
5.10Matrix Spike Fortification Solution - Solution used to prepare the MS and MSD samples. It contains all unlabeled analytes listed in Table 5 at con-centrations corresponding to the HRCC 3.
6.0SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6.1
See the introductory material to this chapter, Organic Analytes,Sec. 4.1.
6.2Sample Collection
6.2.1Sample collection personnel should, to the extent possible,
homogenize samples in the field before filling the sample containers.This should minimize or eliminate the necessity for sample homogenization in the laboratory. The analyst should make a judgment, based on the appearance of the sample, regarding the necessity for additional mixing.If the sample is clearly not homogeneous, the entire contents should be transferred to a glass or stainless steel pan for mixing with a stainless steel spoon or spatula before removal of a sample portion for analysis.
6.2.2Grab and composite samples must be collected in glass
containers. Conventional sampling practices must be followed. The bottle must not be prewashed with sample before collection. Sampling equipment must be free of potential sources of contamination.
6.3Grinding or Blending of Fish Samples - If not otherwise specified by the U.S. EPA, the whole fish (frozen) should be blended or ground to provide a homogeneous sample. The use of a stainless steel meat grinder with a 3 to 5 mm
hole size inner plate is recommended. In some circumstances, analysis of fillet or specific organs of fish may be requested by the U.S. EPA. If so requested, the above whole fish requirement is superseded.
6.4Storage and Holding Times - All samples, except fish and adipose
o
tissue samples, must be stored at 4C in the dark, extracted within 30 days and completely analyzed within 45 days of extraction. Fish and adipose tissue
o
samples must be stored at -20C in the dark,extracted within 30 days and completely analyzed within 45 days of collection. Whenever samples are analyzed after the holding time expiration date, the results should be considered to be minimum concentrations and should be identified as such.
NOTE:The holding times listed in Sec. 6.4 are recommendations. PCDDs and PCDFs are very stable in a variety of matrices, and holding times
under the conditions listed in Sec. 6.4 may be as high as a year for
certain matrices. Sample extracts, however, should always be
analyzed within 45 days of extraction.
6.5Phase Separation - This is a guideline for phase separation for very wet (>25 percent water) soil, sediment and paper pulp samples. Place a 50 g portion in a suitable centrifuge bottle and centrifuge for 30 minutes at 2,000 rpm. Remove the bottle and mark the interface level on the bottle. Estimate the relative volume of each phase. With a disposable pipet, transfer the liquid layer into a clean bottle. Mix the solid with a stainless steel spatula and remove a portion to be weighed and analyzed (percent dry weight determination, extraction). Return the remaining solid portion to the original sample bottle (empty) or to a clean sample bottle that is properly labeled, and store it as appropriate. Analyze the solid phase by using only the soil, sediment and paper pulp method. Take note of, and report, the estimated volume of liquid before disposing of the liquid as a liquid waste.
6.6Soil, Sediment, or Paper Sludge (Pulp) Percent Dry Weight Determination - The percent dry weight of soil, sediment or paper pulp samples showing detectable levels (see note below) of at least one 2,3,7,8-substituted PCDD/PCDF congener is determined according to the following procedure. Weigh a 10 g portion of the soil or sediment sample (+ 0.5 g) to three significant
o
figures. Dry it to constant weight at 110C in an adequately ventilated oven. Allow the sample to cool in a desiccator. Weigh the dried solid to three significant figures. Calculate and report the percent dry weight. Do not use this solid portion of the sample for extraction, but instead dispose of it as hazardous waste.
NOTE:Until detection limits have been established (Sec. 1.3), the lower MCLs (Table 1) may be used to estimate the minimum detectable
levels.
% dry weight = g of dry sample x 100
g of sample
CAUTION:Finely divided soils and sediments contaminated with PCDDs/PCDFs are hazardous because of the potential for
inhalation or ingestion of particles containing PCDDs/PCDFs
(including 2,3,7,8-TCDD). Such samples should be handled in
a confined environment (i.e., a closed hood or a glove box).
6.7Lipid Content Determination
6.7.1Fish Tissue - To determine the lipid content of fish tissue,
concentrate 125 mL of the fish tissue extract (Sec. 7.2.2), in a tared 200mL round bottom flask, on a rotary evaporator until a constant weight (W)is achieved.
100 (W) Percent lipid =
10
Dispose of the lipid residue as a hazardous waste if the results of
the analysis indicate the presence of PCDDs or PCDFs.
6.7.2Adipose Tissue - Details for the determination of the adipose
tissue lipid content are provided in Sec. 7.3.3.
7.0PROCEDURE
7.1Internal standard addition
7.1.1Use a portion of 1 g to 1000 g (+ 5 percent) of the sample to
be analyzed. Typical sample size requirements for different matrices are given in Sec. 7.4 and in Table 1. Transfer the sample portion to a tared flask and determine its weight.
7.1.2Except for adipose tissue, add an appropriate quantity of the
sample fortification mixture (Sec. 5.8) to the sample. All samples should be spiked with 100 μL of the sample fortification mixture to give internal standard concentrations as indicated in Table 1. As an example, for C -13122,3,7,8-TCDD, a 10 g soil sample requires the addition of 1000 pg of C -13122,3,7,8-TCDD to give the required 100 ppt fortification level. The fish tissue sample (20 g) must be spiked with 200 μL of the internal standard solution, because half of the extract will be used to determine the lipid content (Sec. 6.7.1).
7.1.2.1For the fortification of soil, sediment, fly ash,
water, fish tissue, paper pulp and wet sludge samples, mix the
sample fortification solution with 1.0 mL acetone.
7.1.2.2
Do not dilute the nonane solution for the other
matrices.7.1.2.3The fortification of adipose tissue is carried out
at the time of homogenization (Sec. 7.3.2.3).
7.2Extraction and Purification of Fish and Paper Pulp Samples
7.2.1Add 60 g anhydrous sodium sulfate to a 20 g portion of a
homogeneous fish sample (Sec. 6.3) and mix thoroughly with a stainless
steel spatula. After breaking up any lumps, place the fish/sodium sulfate mixture in the Soxhlet apparatus on top of a glass wool plug. Add 250 mL methylene chloride or hexane/methylene chloride (1:1) to the Soxhlet apparatus and reflux for 16 hours. The solvent must cycle completely through the system five times per hour. Follow the same procedure for the partially dewatered paper pulp sample (using a 10 g sample, 30 g of anhydrous sodium sulfate and 200 mL of toluene).
NOTE:As an option, a Soxhlet/Dean Stark extractor system may be used, with toluene as the solvent. No sodium sulfate is added
when using this option.
7.2.2Transfer the fish extract from Sec. 7.2.1 to a 250 mL volumetric flask and fill to the mark with methylene chloride. Mix well, then remove 125 mL for the determination of the lipid content (Sec.
6.7.1). Transfer the remaining 125 mL of the extract, plus two 15 mL hexane/methylene chloride rinses of the volumetric flask, to a KD apparatus equipped with a Snyder column. Quantitatively transfer all of the paper pulp extract to a KD apparatus equipped with a Snyder column.
NOTE:As an option, a rotary evaporator may be used in place of the KD apparatus for the concentration of the extracts.
TM
7.2.3Add a Teflon, or equivalent, boiling chip. Concentrate the extract in a water bath to an apparent volume of 10 mL. Remove the apparatus from the water bath and allow to cool for 5 minutes.
7.2.4Add 50 mL hexane and a new boiling chip to the KD flask. Concentrate in a water bath to an apparent volume of 5 mL. Remove the apparatus from the water bath and allow to cool for 5 minutes.
NOTE:The methylene chloride must have been completely removed before proceeding with the next step.
7.2.5Remove and invert the Snyder column and rinse it into the KD apparatus with two 1 mL portions of hexane. Decant the contents of the KD apparatus and concentrator tube into a 125 mL separatory funnel. Rinse the KD apparatus with two additional 5 mL portions of hexane and add the rinses to the funnel. Proceed with the cleanup according to the instructions starting in Sec. 7.5.1.1, but omit the procedures described in Secs. 7.5.1.2 and 7.5.1.3.
7.3Extraction and Purification of Human Adipose Tissue
7.3.1Human adipose tissue samples must be stored at a temperature
o
of -20C or lower from the time of collection until the time of analysis. The use of chlorinated materials during the collection of the samples must be avoided. Samples are handled with stainless steel forceps, spatulas, or scissors. All sample bottles (glass) are cleaned as specified in the
TM
note at the end of Sec. 4.3. Teflon lined caps should be used.
o
NOTE:The specified storage temperature of -20C is the maximum storage temperature permissible for adipose tissue samples.
Lower storage temperatures are recommended.
7.3.2Adipose Tissue Extraction
7.3.2.1Weigh, to the nearest 0.01 g, a 10 g portion of a frozen adipose tissue sample into a culture tube (2.2 x 15 cm).
NOTE:The sample size may be smaller, depending on availability. In such a situation, the analyst is
required to adjust the volume of the internal standard
solution added to the sample to meet the fortification
level stipulated in Table 1.
7.3.2.2Allow the adipose tissue specimen to reach room temperature (up to 2 hours).
7.3.2.3Add 10 mL methylene chloride and 100 μL of the sample fortification solution. Homogenize the mixture for approximately 1 minute with a tissue homogenizer.
7.3.2.4Allow the mixture to separate, then remove the methylene chloride extract from the residual solid material with a disposable pipet. Percolate the methylene chloride through a filter funnel containing a clean glass wool plug and 10 g anhydrous sodium sulfate. Collect the dried extract in a graduated 100 mL volumetric flask.
7.3.2.5Add a second 10 mL portion of methylene chloride to the sample and homogenize for 1 minute. Decant the solvent, dry it, and transfer it to the 100 mL volumetric flask (Sec. 7.3.2.4).
7.3.2.6Rinse the culture tube with at least two additional portions of methylene chloride (10 mL each), and transfer the entire contents to the filter funnel containing the anhydrous sodium sulfate. Rinse the filter funnel and the anhydrous sodium sulfate contents with additional methylene chloride (20 to 40 mL) into the 100 mL flask. Discard the sodium sulfate.
7.3.2.7Adjust the volume to the 100 mL mark with methylene chloride.
7.3.3Adipose Tissue Lipid Content Determination
7.3.3.1Preweigh a clean 1 dram (or metric equivalent) glass vial to the nearest 0.0001 g on an analytical balance tared to zero.
7.3.3.2Accurately transfer 1.0 mL of the final extract (100 mL) from Sec. 7.3.2.7 to the vial. Reduce the volume of the
o
extract on a water bath (50-60C) by a gentle stream of purified
nitrogen until an oily residue remains. Nitrogen blowdown is continued until a constant weight is achieved.
NOTE:When the sample size of the adipose tissue is smaller than 10 g, then the analyst may use a larger portion (up
to 10 percent) of the extract defined in Sec. 7.3.2.7
for the lipid determination.
7.3.3.3Accurately weigh the vial with the residue to the nearest 0.0001 g and calculate the weight of the lipid present in the vial based on the difference of the weights.
7.3.3.4Calculate the percent lipid content of the original sample to the nearest 0.1 percent as shown below:
W x V
lr ext
Lipid content, LC (%) = x 100
W x V
at al
where:
W=weight of the lipid residue to the nearest 0.0001
lr
g calculated from Sec. 7.3.3.3,
V=total volume (100 mL) of the extract in mL from
ext
Sec. 7.3.2.7,
W=weight of the original adipose tissue sample to
at
the nearest 0.01 g from Sec. 7.3.2.1, and
V=volume of the aliquot of the final extract in mL
al
used for the quantitative measure of the lipid
residue (1.0 mL) from Sec. 7.3.3.2.
7.3.3.5Record the lipid residue measured in Sec. 7.3.3.3 and the percent lipid content from Sec. 7.3.3.4.
7.3.4Adipose Tissue Extract Concentration
7.3.4.1Quantitatively transfer the remaining extract from Sec. 7.3.3.2 (99.0 mL) to a 500 mL Erlenmeyer flask. Rinse the volumetric flask with 20 to 30 mL of additional methylene chloride to ensure quantitative transfer.
7.3.4.2Concentrate the extract on a rotary evaporator and
o
a water bath at 40C until an oily residue remains.
7.3.5Adipose Tissue Extract Cleanup
7.3.5.1Add 200 mL hexane to the lipid residue in the 500 mL Erlenmeyer flask and swirl the flask to dissolve the residue.
7.3.5.2Slowly add, with stirring, 100 g of 40 percent
(w/w) sulfuric acid-impregnated silica gel. Stir with a magnetic stirrer for two hours at room temperature.
7.3.5.3Allow the solid phase to settle, and decant the
liquid through a filter funnel containing 10 g anhydrous sodium sulfate on a glass wool plug, into another 500 mL Erlenmeyer flask.
7.3.5.4Rinse the solid phase with two 50 mL portions of
hexane. Stir each rinse for 15 minutes, decant, and dry as described under Sec. 7.3.5.3. Combine the hexane extracts from Sec.
7.3.5.3 with the rinses.
7.3.5.5Rinse the sodium sulfate in the filter funnel with
an additional 25 mL hexane and combine this rinse with the hexane extracts from Sec. 7.3.5.4.
7.3.5.6Prepare an acidic silica column as follows: Pack
a 2 cm x 10 cm chromatographic column with a glass wool plug, add
approximately 20 mL hexane, add 1 g silica gel and allow to settle, then add 4 g of 40 percent (w/w) sulfuric acid-impregnated silica gel and allow to settle. Elute the excess hexane from the column until the solvent level reaches the top of the chromatographic packing. Verify that the column does not have any air bubbles and channels.
7.3.5.7Quantitatively transfer the hexane extract from
the Erlenmeyer flask (Secs. 7.3.5.3 through 7.3.5.5) to the silica gel column reservoir. Allow the hexane extract to percolate through the column and collect the eluate in a 500 mL KD apparatus.
7.3.5.8Complete the elution by percolating 50 mL hexane
through the column into the KD apparatus. Concentrate the eluate on
a steam bath to approximately 5 mL. Use nitrogen blowdown to bring
the final volume to about 100 μL.
NOTE:If the silica gel impregnated with 40 percent sulfuric
acid is highly discolored throughout the length of the
adsorbent bed, the cleaning procedure must be repeated
beginning with Sec. 7.3.5.1.
7.3.5.9The extract is ready for the column cleanups
described in Secs. 7.5.2 through 7.5.3.6.
7.4Extraction and Purification of Environmental and Waste Samples
7.4.1Sludge/Wet Fuel Oil
7.4.1.1Extract aqueous sludge or wet fuel oil samples by
refluxing a sample (e.g., 2 g) with 50 mL toluene in a 125 mL flask fitted with a Dean-Stark water separator. Continue refluxing the sample until all the water is removed.
NOTE:If the sludge or fuel oil sample dissolves in toluene, treat it according to the instructions in Sec. 7.4.2
below. If the labeled sludge sample originates from
pulp (paper mills), treat it according to the
instructions starting in Sec. 7.2, but without the
addition of sodium sulfate.
7.4.1.2Cool the sample, filter the toluene extract through a glass fiber filter, or equivalent, into a 100 mL round bottom flask.
7.4.1.3Rinse the filter with 10 mL toluene and combine the extract with the rinse.
7.4.1.4Concentrate the combined solutions to near dryness
o
on a rotary evaporator at 50C. Use of an inert gas to concentrate the extract is also permitted. Proceed with Sec. 7.4.4.
7.4.2Still Bottom/Oil
7.4.2.1Extract still bottom or oil samples by mixing a sample portion (e.g., 1.0 g) with 10 mL toluene in a small beaker and filtering the solution through a glass fiber filter (or equivalent) into a 50 mL round bottom flask. Rinse the beaker and filter with 10 mL toluene.
7.4.2.2Concentrate the combined toluene solutions to near
o
dryness on a rotary evaporator at 50C. Proceed with Sec. 7.4.4.
7.4.3Fly Ash
NOTE:Because of the tendency of fly ash to "fly", all handling steps should be performed in a hood in order to minimize contamination.
7.4.3.1Weigh about 10 g fly ash to two decimal places and transfer to an extraction jar. Add 100 μL sample fortification solution (Sec. 5.8), diluted to 1 mL with acetone, to the sample. Add 150 mL of 1 M HCl to the fly ash sample. Seal the jar with the TM
Teflon lined screw cap and shake for 3 hours at room temperature.
7.4.3.2Rinse a glass fiber filter with toluene, and filter the sample through the filter paper, placed in a Buchner funnel, into a 1 L flask. Wash the fly ash cake with approximately 500 mL organic-free reagent water and dry the filter cake overnight at room temperature in a desiccator.
7.4.3.3Add 10 g anhydrous powdered sodium sulfate, mix thoroughly, let sit in a closed container for one hour, mix again, let sit for another hour, and mix again.
7.4.3.4Place the sample and the filter paper into an extraction thimble, and extract in a Soxhlet extraction apparatus
charged with 200 mL toluene for 16 hours using a five cycle/hour schedule.
NOTE:As an option, a Soxhlet/Dean Stark extractor system may
be used, with toluene as the solvent. No sodium sulfate
is added when using this option.
7.4.3.5Cool and filter the toluene extract through a
glass fiber filter into a 500 mL round bottom flask. Rinse the filter with 10 mL toluene. Add the rinse to the extract and concentrate the combined toluene solutions to near dryness on a
o
rotary evaporator at 50C. Proceed with Sec. 7.4.4.
7.4.4Transfer the concentrate to a 125 mL separatory funnel using 15 mL hexane. Rinse the flask with two 5 mL portions of hexane and add the rinses to the funnel. Shake the combined solutions in the separatory funnel for two minutes with 50 mL of 5 percent sodium chloride solution, discard the aqueous layer, and proceed with Sec. 7.5.
7.4.5Aqueous samples
7.4.5.1Allow the sample to come to ambient temperature,
then mark the water meniscus on the side of the 1 L sample bottle for later determination of the exact sample volume. Add the required acetone diluted sample fortification solution (Sec. 5.8).
7.4.5.2When the sample is judged to contain 1 percent or
more solids, the sample must be filtered through a glass fiber filter that has been rinsed with toluene. If the suspended solids content is too great to filter through the 0.45 μm filter, centrifuge the sample, decant, and then filter the aqueous phase.
NOTE:Paper mill effluent samples normally contain 0.02%-0.2%
solids, and would not require filtration. However, for
optimum analytical results, all paper mill effluent
samples should be filtered, the isolated solids and
filtrate extracted separately, and the extracts
recombined.
7.4.5.3Combine the solids from the centrifuge bottle(s)
with the particulates on the filter and with the filter itself and proceed with the Soxhlet extraction as specified in Secs. 7.4.6.1 through 7.4.6.4. Remove and invert the Snyder column and rinse it down into the KD apparatus with two 1 mL portions of hexane.
7.4.5.4Pour the aqueous filtrate into a 2 L separatory
funnel. Add 60 mL methylene chloride to the sample bottle, seal and shake for 30 seconds to rinse the inner surface. Transfer the solvent to the separatory funnel and extract the sample by shaking the funnel for two minutes with periodic venting.
7.4.5.5Allow the organic layer to separate from the water
phase for a minimum of 10 minutes. If the emulsion interface
between layers is more than one third the volume of the solvent layer, the analyst must employ mechanical techniques to complete the phase separation (e.g., glass stirring rod).
7.4.5.6Collect the methylene chloride into a KD apparatus (mounted with a 10 mL concentrator tube) by passing the sample extracts through a filter funnel packed with a glass wool plug and 5 g anhydrous sodium sulfate.
NOTE:As an option, a rotary evaporator may be used in place of the KD apparatus for the concentration of the
extracts.
7.4.5.7Repeat the extraction twice with fresh 60 mL portions of methylene chloride. After the third extraction, rinse the sodium sulfate with an additional 30 mL methylene chloride to ensure quantitative transfer. Combine all extracts and the rinse in the KD apparatus.
NOTE: A continuous liquid-liquid extractor may be used in place of a separatory funnel when experience with a
sample from a given source indicates that a serious
emulsion problem will result or an emulsion is
encountered when using a separatory funnel. Add 60 mL
methylene chloride to the sample bottle, seal, and shake
for 30 seconds to rinse the inner surface. Transfer the
solvent to the extractor. Repeat the rinse of the
sample bottle with an additional 50 to 100 mL portion of
methylene chloride and add the rinse to the extractor.
Add 200 to 500 mL methylene chloride to the distilling
flask, add sufficient organic-free reagent water (Sec.
5.1) to ensure proper operation, and extract for
24 hours. Allow to cool, then detach the distilling
flask. Dry and concentrate the extract as described in
Secs. 7.4.5.6 and 7.4.5.8 through 7.4.5.10. Proceed
with Sec. 7.4.5.11.
7.4.5.8Attach a Snyder column and concentrate the extract on a water bath until the apparent volume of the liquid is 5 mL. Remove the KD apparatus and allow it to drain and cool for at least 10 minutes.
7.4.5.9Remove the Snyder column, add 50 mL hexane, add the concentrate obtained from the Soxhlet extraction of the suspended solids (Sec. 7.4.5.3), if applicable, re-attach the Snyder column, and concentrate to approximately 5 mL. Add a new boiling chip to the KD apparatus before proceeding with the second concentration step.
7.4.5.10Rinse the flask and the lower joint with two 5 mL portions of hexane and combine the rinses with the extract to give a final volume of about 15 mL.
7.4.5.11Determine the original sample volume by filling
the sample bottle to the mark with water and transferring the water to a 1000 mL graduated cylinder. Record the sample volume to the nearest 5 mL. Proceed with Sec. 7.5.
7.4.6Soil/Sediment
7.4.6.1Add 10 g anhydrous powdered sodium sulfate to the
sample portion (e.g., 10 g) and mix thoroughly with a stainless steel spatula. After breaking up any lumps, place the soil/sodium sulfate mixture in the Soxhlet apparatus on top of a glass wool plug (the use of an extraction thimble is optional).
NOTE:As an option, a Soxhlet/Dean Stark extractor system may
be used, with toluene as the solvent. No sodium sulfate
is added when using this option.
7.4.6.2Add 200 to 250 mL toluene to the Soxhlet apparatus
and reflux for 16 hours. The solvent must cycle completely through the system five times per hour.
NOTE:If the dried sample is not of free flowing consistency,
more sodium sulfate must be added.
7.4.6.3Cool and filter the extract through a glass fiber
filter into a 500 mL round bottom flask for evaporation of the toluene. Rinse the filter with 10 mL of toluene, and concentrate the combined fractions to near dryness on a rotary evaporator at o
50C. Remove the flask from the water bath and allow to cool for
5 minutes.
7.4.6.4Transfer the residue to a 125 mL separatory
funnel, using 15 mL of hexane. Rinse the flask with two additional portions of hexane, and add the rinses to the funnel. Proceed with Sec. 7.5.
7.5Cleanup
7.5.1Partition
7.5.1.1Partition the hexane extract against 40 mL of
concentrated sulfuric acid. Shake for two minutes. Remove and discard the sulfuric acid layer (bottom). Repeat the acid washing until no color is visible in the acid layer (perform a maximum of four acid washings).
7.5.1.2Omit this step for the fish sample extract.
Partition the extract against 40 mL of 5 percent (w/v) aqueous sodium chloride. Shake for two minutes. Remove and discard the aqueous layer (bottom).
7.5.1.3Omit this step for the fish sample extract.
Partition the extract against 40 mL of 20 percent (w/v) aqueous
国家环境保护总局令第13号令 建设项目竣工环境保护验收管理办法 各省、自治区、直辖市环境保护局（厅）: 《建设项目竣工环境保护验收管理办法》，已于2001年12月11日经国家环境保护总局第12次局务会议通过，现予发布,自2002年2月1日起施行。 国家环境保护总局局长解振华 二〇〇一年十二月二十七日 抄送：解放军环境保护局，新疆生产建设兵团环境保护局，各直属单位，各派出机构 附件： 建设项目竣工环境保护验收管理办法 第一条为加强建设项目竣工环境保护验收管理，监督落实环境保护设施与建设项目主体工程同时投产或者使用，以及落实其他需配套采取的环境保护措施，防治环境污染和生态破坏，根据《建设项目环境保护管理条例》和其他有关法律、法规规定，制定本办法。 第二条本办法适用于环境保护行政主管部门负责审批环境影响报告书（表）或者环境影响登记表的建设项目竣工环境保护验收管理。 第三条建设项目竣工环境保护验收是指建设项目竣工后，环境保护行政主管部门根据本办法规定，依据环境保护验收监测或调查结果，并通过现场检查等手段，考核该建设项目是否达到环境保护要求的活动。 第四条建设项目竣工环境保护验收范围包括： （一）与建设项目有关的各项环境保护设施，包括为防治污染和保护环境所建成或配备的工程、设备、装置和监测手段，各项生态保护设施； （二）环境影响报告书（表）或者环境影响登记表和有关项目设计文件规定应采取的其他各项环境保护措施。 第五条国务院环境保护行政主管部门负责制定建设项目竣工环境保护验收管理规范，指导并监督地方人民政府环境保护行政主管部门的建设项目竣工环境保护验收工作，并负责对其审批的环境影响报告书（表）或者环境影响登记表的建设项目竣工环境保护验收工作。
METHOD 3541 AUTOMATED SOXHLET EXTRACTION 1.0SCOPE AND APPLICATION 1.1Method 3541 describes the extraction of organic analytes from soil, sediment, sludges, and waste solids. The method uses a commercially available, unique, three stage extraction system to achieve analyte recovery comparable to Method 3540, but in a much shorter time. There are two differences between this extraction method and Method 3540. In the initial extraction stage of Method 3541, the sample-loaded extraction thimble is immersed into the boiling solvent. This ensures very rapid intimate contact between the specimen and solvent and rapid extraction of the organic analytes. In the second stage the thimble is elevated above the solvent, and is rinse-extracted as in Method 3540. In the third stage, the solvent is evaporated, as would occur in the Kuderna-Danish (K-D) concentration step in Method 3540. The concentrated extract is then ready for cleanup (Method 3600) followed by measurement of the organic analytes. 1.2The method is applicable to the extraction and concentration of water insoluble or slightly water soluble polychlorinated biphenyls (PCBs) in preparation for gas chromatographic determination using either Method 8080 or 8081. This method is applicable to soils, clays, solid wastes and sediments containing from 1 to 50 μg of PCBs (measured as Arochlors) per gram of sample. It has been statistically evaluated at 5 and 50 μg/g of Arochlors 1254 and 1260, and found to be equivalent to Method 3540 (Soxhlet Extraction). Higher concentrations of PCBs are measured following volumetric dilution with hexane. 1.3The method is also applicable the extraction and concentration of semivolatile organics in preparation for GC/MS analysis by Method 8270 or by analysis using specific GC or HPLC methods. 2.0SUMMARY OF METHOD 2.1PCBs: Moist solid samples (e.g., soil/sediment samples) may be air-dried and ground prior to extraction or chemically dried with anhydrous sodium sulfate. The prepared sample is extracted using 1:1 (v/v) acetone:hexane in the automated Soxhlet following the same procedure as outlined for semivolatile organics in Sec. 2.1. The extract is then concentrated and exchanged into pure hexane prior to final gas chromatographic PCB measurement. 2.2Other semivolatile organics: A 10-g solid sample (the sample is pre-mixed with anhydrous sodium sulfate for certain matrices) is placed in an extraction thimble and usually extracted with 50 mL of 1:1 (v/v) acetone/hexane for 60 minutes in the boiling extraction solvent. The thimble with sample is then raised into the rinse position and extracted for an additional 60 minutes. Following the extraction steps, the extraction solvent is concentrated to 1 to 2 mL. CD-ROM3541 - 1Revision 0 September 1994
11.环境保护档案管理办法(国家环境保护局令第13号) 《环境保护档案管理办法》已于1994年9月27日经国家环境保护局局务会议通过，现予发布施行。 环境保护档案管理办法 第一章总则 第一条为加强环境保护档案管理，开发利用环境保护档案信息资源，根据《中华人民共和国档案法》及其实施办法，制定本办法。 第二条环境保护档案是指各级环境保护行政主管部门及其直属单位（以下简称“环保部门”），在环境保护活动中直接形成的、对国家和社会有保存价值的各种文字、图表、声像等不同形式和载体的历史记录。 第三条环境保护档案工作实行统一领导，分级管理。县级以上各级环保部门应当把环境档案工作纳人本部门的发展规划和年度计划，并保障档案业务经费。 第四条环境保护档案库(室)的建设和环境保护档案管理所需仪器、设备及装具的购置经费，按有关规定从相应的资金渠道解决，不足部分在环境保护补助资金的百分之二十部分中列支。 第五条县级以上各级环保部门应当加强对不同门类和不同载体的环境保护档案的综合管理，建立、健全档案管理制度，保证环境保护档案的安全和有效利用。 各级环保部门应当采用先进技术，逐步实现环境保护档案管理的现代化。 第二章档案管理机构及其职责 第六条环境保护档案工作在国家档案行政管理部门“统筹规划，组织协调，统一制度，监督和指导”下进行。国务院环境保护行政主管部门对全国环境保护档案工作实施监督管理。 县级以上地方各级环境保护行政主管部门对本辖区环境保护档案工作实施监督管理，并在业务上受上级环境行政主管部门和同级档案行政主管部门的监督、指导和检查。 第七条省辖市级以上环境保护行政主管部门，应根据实际情况，建立环保档案管理机构，并配备专职档案工作人员;县级环境保护行政主管部门应设立综合档案室，并配备专职或者兼职档案工作人员; 各级环境保护行政主管部门的直属单位应当根据实际情况，设立环保档案管理机构，并配备专职或者兼职档案工作人员。 第八条环保部门的档案管理机构履行下列职责: (一)贯彻执行国家档案工作的方针、政策和法规，结合本部门的实际情况，
主要发达国家环保产业发展概况 一、美国 （一）产业分类情况 美国环保产业分为环保服务、环保设备和环境资源三大类。 （二）产业发展概况 美国现在也在面临和处理一系列挑战，包括水方面、气候变化、细菌、污染、负氧，以及水供应。美国环保局现在也在动用自己的力量重整整个水资源系统，不管是学术界还是市民，都参与到了环保的行业当中。没有人能够再袖手旁观了。
美国环保技术和设备可以帮助解决水跟土壤的问题，其实最主要的是淤泥积土。每一次下雨的时候，空气当中的污染物都会进入到的水中，包括河流，包括大江，而随着水的流动，所有的这些分子，还有污染物都会流向其他地方，所以美国现在的环保部对于处理水污染方面的技术是的重点。要减排，减少能源的消耗，同时要解决这些水方面的问题。 美国技术和设备方面的优势。美国现在已经成为全球在环境保护技术和设备方面领先的国家，美国的研发工作做得非常到位，美国使用目前的研发成果来开发新的技术，例如水资源处理，还有其他诊断和探寻设备，还有在细菌、濒危物种、化肥、杀虫剂等方面的一些技术和设备。其实，目前中国的发展也非常快，在环境方面也解决了很多的问题。面临着新一代的环境系统，在基础设施建设方面也有着更多的优势，所以创新是一个很好的推动力量，只有创新才能推动经济的长远发展，中国和全球各个国家都已经意识到了这一点。 在现代经济当中，各个国家都在鼓励新技术的创新，新技术同时也推动了经济发展，新技术是经济发展的燃料剂和助推剂，可以影响到每个人，也会影响到每天的商业决策。目前有很多数据讲的都是一些新兴企业的产品、市场、知识产权的保护，这些议题是所有全球企业都面临的议题，而同时在这样的环境当中，美国有不断的技术、产品和服务推陈出新，同时美国有着新的体系、新的标准、新的数据，还有新的发现、分析的结果，这些能够更好的保护隐私和安全。关于气候变化和天气管理的政府机构都会对进行评估，对大气、水资源等去进行环评。另外很多企业和国家都面临着非常严峻的供应链的挑战，都会考虑所有的这些环境因素，未来发展的能力已经到了一个临界点，甚至现在天灾也会带来非常严重的后果，例如地震等，另外还有全球一些地区的冲突，所以货物在运输时所造成的损失也越来越频繁，每年因为这些因素导致的货物损失高达数亿美元，有
国家环境保护总局令第38号 环境行政复议与行政应诉办法 《环境行政复议与行政应诉办法》已于2006年12月19日国家环境保护总局2006年第七次局务会议通过，现予公布，自2007年2月1日起施行。 国家环境保护总局局长周生贤 二○○六年十二月二十七日 主题词: 环保行政复议行政应诉令 环境行政复议与行政应诉办法 第一条为防止和纠正违法或者不当的具体行政行为，保护公民、法人和其他组织的合法权益，规范环境保护行政主管部门的行政复议与行政应诉工作，依据《中华人民共和国行政复议法》、《中华人民共和国行政诉讼法》等法律法规制定本办法。 第二条公民、法人或者其他组织认为环境保护行政主管部门的具体行政行为侵犯其合法权益，向环境保护行政主管部门申请行政复议或者向人民法院提起行政诉讼，环境保护行政主管部门办理行政复议案件或者行政应诉案件，适用本办法。 第三条对重大、复杂的环境行政复议案件和行政应诉案件实行集体审议制度。集体审议由环境保护行政主管部门负责人主持，有关业务机构负责人参加。 第四条依法履行行政复议职责的环境保护行政主管部门为行政复议机关。 行政复议机关负责法制工作的机构，具体办理行政复议事项，履行下列职责： （一）受理行政复议申请；
（二）向有关组织和人员调查取证，查阅文件和资料； （三）组织审查行政复议案件，提出审查建议，拟订行政复议决定； （四）处理或转送本办法第十六条规定的审查申请； （五）送达行政复议法律文书； （六）对被申请人违反《行政复议法》及本办法的行为提出处理建议； （七）办理因不服行政复议决定提起行政诉讼的应诉事项； （八）对下级环境保护行政主管部门的行政复议工作进行指导、监督和检查； （九）法律、法规和规章规定的其他职责。 第五条有下列情形之一的，公民、法人或者其他组织可以依照本办法申请行政复议： （一）对环境保护行政主管部门作出的警告、罚款、没收违法所得、责令停止生产或者使用，暂扣、吊销许可证等行政处罚决定不服的； （二）认为符合法定条件，申请环境保护行政主管部门颁发许可证、资质证、资格证等证书，或者申请审批、登记等有关事项，环境保护行政主管部门没有依法办理的； （三）对环境保护行政主管部门有关许可证、资质证、资格证等证书的变更、中止、撤销、注销决定不服的； （四）认为环境保护行政主管部门违法征收排污费或者违法要求履行其他义务的； （五）申请环境保护行政主管部门履行法定职责，环境保护行政主管部门没有依法履行的； （六）认为环境保护行政主管部门的其他具体行政行为侵犯其合法权益的。 第六条有下列情形之一的，行政复议机关不予受理并说明理由： （一）申请行政复议的时间超过了法定申请期限又无法定正当理由的； （二）不服环境保护行政主管部门对环境污染损害赔偿责任和赔偿金额纠纷作出的调解或者其他处理决定的； （三）申请人在申请行政复议前已经向其他行政复议机关申请行政复议或者已向人民法院提起行政诉讼，其他行政复议机关或者人民法院已经依法受理的；
美国环境保护制度 篇一：环保：美国的垃圾管理机制 环境产业研究 第19期 20XX年7月27日全国工商联环境服务业商会 美国垃圾管理机制 ——商业模式下的系统化垃圾管理 作为经济大国的美国同样也是一个消费大国，持续增长的垃圾排放对其环境质量也造成了极大地威胁。据美国环境署最新公布数字显示，20XX年，美国城市固体垃圾产量达2.5亿吨，如果用卡车运送这些垃圾，组成的车队足以绕地球6圈。但是，在清晰的垃圾管理战略的指导下，美国垃圾处理产业得到了快速的发展，目前已经形成了系统化的垃圾管理商业模式，足以应对日益增长的垃圾排放量。 一、美国垃圾管理概况 （一）垃圾管理战略 美国确定的固体废弃物治理战略方针是实施源头控制政策，从生产阶段抑制废物的产生，减少使用成为污染源的物质；最大限度地实施废物资源回收，通过堆肥、焚烧热能回收利用实现废物资源、能源的再生利用，最后进行卫生填埋。 近年来，美国一直坚持垃圾减量、分流和再利用这个主题，以废物变
资源、废物变能源（焚烧和生物制肥）作为垃圾治理的主导方向，制定的20XX年的垃圾处理目标是：回收利用（包括直接回收、路边分类、堆肥、综合利用等）50%，填埋40%，焚烧10%。 为实现这些目标，美国各州普遍采取垃圾源头控制和减量措施，提出垃圾分流的概念，将食品垃圾、庭院垃圾和餐厨垃圾等按类别作为分流目标，直接进入适用的处理程序，既促进了不同成分垃圾的分类处理，也促进了资源的循环再生，垃圾处理已经形成了比较系统的模式。美国垃圾管理战略已取得了明显的成效：垃圾填埋已经从1980年的89%降为20XX年的54%，而垃圾资源回收再利用则从1980年的9.6%提高到了20XX年的33.4%，垃圾焚烧处理从1980年的1.8%上升到了20XX年的12.6%。 （二）垃圾处理方式的演变 全美国1988年共有垃圾填埋场7924个，1999年为2514个，20XX 年下降到1767个，20XX年又降为1654个，总体上呈下降趋势。垃圾焚烧厂数量从1997年的131座下降到20XX年的101座，包括焚烧和生物制能的废物变能源工厂。20XX年全美国共有废物定点回收场地12694个，路边资源垃圾分类回收项目也从1989年的1042个增长 到20XX年的7689个，成为废物资源回收的重要组成部分。 目前在美国的不同地区，垃圾处理方式的比例各不相同。如：新英格兰地区的填埋占36%，回收占33%，焚烧占31%。美国西部的填埋
9066 1 CD-ROM Revision 0 Date September 1986 METHOD 9066PHENOLICS (COLORIMETRIC, AUTOMATED 4-AAP WITH DISTILLATION) 1.0SCOPE AND APPLICATION 1.1This method is applicable to the analysis of ground water and of drinking, surface, and saline waters. 1.2The method is capable of measuring phenolic materials from 2 to 500ug/L in the aqueous phase using phenol as a standard. 2.0SUMMARY OF METHOD 2.1This automated method is based on the distillation of phenol and subsequent reaction of the distillate with alkaline ferricyanide (K Fe(CN)) and 364-amino-antipyrine (4-AAP) to form a red complex which is measured at 505 or 520 nm. 3.0INTERFERENCES 3.1Interferences from sulfur compounds are eliminated by acidifying the sample to a pH of < 4.0 with H SO and aerating briefly by stirring. 243.2Oxidizing agents such as chlorine, detected by the liberation of iodine upon acidification in the presence of potassium iodide, are removed immediately after sampling by the addition of an excess of ferrous ammonium sulfate (5.5). If chlorine is not removed, the phenolic compounds may be partially oxidized and the results may be low. 3.3Background contamination from plastic tubing and sample containers is eliminated by filling the wash receptacle by siphon (using Kel-F tubing) and using glass tubes for the samples and standards. 4.0APPARATUS AND MATERIALS 4.1Automated continuous-flow analytical instrument: 4.1.1 Sampler : Equipped with continuous mixer.4.1.2 Manifold .4.1.3 Proportioning pump II or III .4.1.4 Heating bath with distillation coil .4.1.5Distillation head .
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
15.电磁辐射环境保护管理办法（局令第18号）第一章总则 第一条为加强电磁辐射环境保护工作的管理，有效地保护环境，保障公众健康，根据《中华人民共和国环境保护法》及有关规定，制定本办法。 第二条本办法所称电磁辐射是指以电磁波形式通过空间传播的能量流，且限于非电离辐射，包括信息传递中的电磁波发射，工业、科学、医疗应用中的电磁辐射，高压送变电中产生的电磁辐射。 任何从事前款所列电磁辐射的活动，或进行伴有该电磁辐射的活动的单位和个人，都必须遵守本办法的规定。 第三条县级以上人民政府环境保护行政主管部门对本辖区电磁辐射环 境保护工作实施统一监督管理。 第四条从事电磁辐射活动的单位主管部门负责本系统、本行业电磁辐射环境保护工作的监督管理工作。 第五条任何单位和个人对违反本管理办法的行为有权检举和控告。第二章监督管理 第六条国务院环境保护行政主管部门负责下列建设项目环境保护申报 登记和环境影响报告书的审批，负责对该类项目执行环境保护设施与主体工程同时设计、同时施工、同时投产使用（以下简称“三同时”制度）的情况进行检查并负责该类项目的竣工验收： （一）总功率在200 千瓦以上的电视发射塔； （二）总功率在1000 千瓦以上的广播台、站； （三）跨省级行政区电磁辐射建设项目； （四）国家规定的限额以上电磁辐射建设项目。 第七条省、自治区、直辖市（以下简称“省级” ）环境保护行政主管部门负责除第六条规定所列项目以外、豁免水平以上的电磁辐射建设项目和设备的环境保护申报登记和环境影响报告书的审批；负责对该类项目和设备执行环境保护设施“三同时”制度的情况进行检查并负责竣工验收；参与辖区内由国务院环境保护行政主管部门负责的环境影响报告书的审批、环境保护设施“三同时”制度执行情况的检查和项目竣工验收以及项目建成后对环境影响的监督检查；负责辖区内电磁辐射环境保护管理队伍的建设；负责对辖区内因电磁辐射活动造成的环境影响实施监督管理和监督性监测。 第八条市级环境保护行政主管部门根据省级环境保护行政主管部门的 委托，可承担第七条所列全部或部分任务及本辖区内电磁辐射项目和设备的监督性监测和日常监督管理。 第九条从事电磁辐射活动的单位主管部门应督促其下属单位遵守国家
METHOD 3520C CONTINUOUS LIQUID-LIQUID EXTRACTION 1.0SCOPE AND APPLICATION 1.1This method describes a procedure for isolating organic compounds from aqueous samples. The method also describes concentration techniques suitable for preparing the extract for the appropriate determinative steps described in Sec. 4.3 of Chapter Four. 1.2This method is applicable to the isolation and concentration of water-insoluble and slightly soluble organics in preparation for a variety of chromatographic procedures. 1.3Method 3520 is designed for extraction solvents with greater density than the sample. Continuous extraction devices are available for extraction solvents that are less dense than the sample. The analyst must demonstrate the effectiveness of any such automatic extraction device before employing it in sample extraction. 1.4This method is restricted to use by or under the supervision of trained analysts. Each analyst must demonstrate the ability to generate acceptable results with this method. 2.0SUMMARY OF METHOD 2.1 A measured volume of sample, usually 1 liter, is placed into a continuous liquid-liquid extractor, adjusted, if necessary, to a specific pH (see Table 1), and extracted with organic solvent for 18 - 24 hours. 2.2The extract is dried, concentrated (if necessary), and, as necessary, exchanged into a solvent compatible with the cleanup or determinative method being employed (see Table 1 for appropriate exchange solvents). 3.0INTERFERENCES 3.1Refer to Method 3500. 3.2The decomposition of some analytes has been demonstrated under basic extraction conditions required to separate analytes. Organochlorine pesticides may dechlorinate, phthalate esters may exchange, and phenols may react to form tannates. These reactions increase with increasing pH, and are decreased by the shorter reaction times available in Method 3510. Method 3510 is preferred over Method 3520 for the analysis of these classes of compounds. However, the recovery of phenols may be optimized by using Method 3520 and performing the initial extraction at the acid pH. 4.0APPARATUS AND MATERIALS 4.1Continuous liquid-liquid extractor - Equipped with polytetrafluoroethylene (PTFE) or glass connecting joints and stopcocks requiring no lubrication (Kontes 584200-0000, 584500-0000, 583250-0000, or equivalent). CD-ROM3520C - 1Revision 3 December 1996
国家计委、财政部、建设部、国家环保总局关于实行城市生活垃圾处理收费制度促进垃圾处理产业化的通知 【法规类别】行政事业与服务收费管理行政事业性收费 【发文字号】计价格[2002]872号 【发布部门】国家发展和改革委员会(含原国家发展计划委员会、原国家计划委员会)财政部建设部(已撤销) 国家环境保护总局(已撤销) 【发布日期】2002.06.07 【实施日期】2002.06.07 【时效性】现行有效 【效力级别】部门规范性文件 国家计委、财政部、建设部、国家环保总局关于 实行城市生活垃圾处理收费制度促进垃圾处理产业化的通知 （计价格[2002]872号） 各省、自治区、直辖市人民政府： 随着我国城市化进程的加快，城市生活垃圾数量也在迅速增加。由于城市垃圾处理投资渠道单一，缺少必要的设施建设、运行和维护资金，处理设施严重不足，处理水平普遍不高，相当一部分城市的土壤、水体、大气受到生活垃圾的污染，使生态环境和人民群众生活受到影响。解决城市生活垃圾问题已成为全社会关注的热点问题。 为加快生活垃圾处理步伐，提高垃圾处理质量，改善城市生态环境，促进可持续发展，
根据《中华人民共和国国民经济和社会发展第十个五年计划》、《中华人民共和国固体废物污染环境防治法》的有关规定和党中央、国务院有关建立城市生活垃圾处理收费制度，实行垃圾处理产业化的决定，经国务院同意，现就实行城市生活垃圾处理收费制度，促进垃圾处理产业化的有关事项通知如下： 一、全面推行生活垃圾处理收费制度，促进垃圾处理的良性循环 城市生活垃圾是指城市人口在日常生活中产生或为城市日常生活提供服务的产生的固体废物，以及法律、行政法规规定，视为城市生活垃圾的固体废物（包括建筑垃圾和渣土，不包括工业固体废物和危险废物）。所有产生生活垃圾的国家机关、企事业单位（包括交通运输工具）、个体经营者、社会团体、城市居民和城市暂住人口等，均应按规定缴纳生活垃圾处理费。 实行生活垃圾处理收费制度，是适应社会主义市场经济体制的客观要求，促进垃处理体制改革，实行政事、政企分开，逐步实现垃圾处理产业化的重要措施。各地要充分发挥市场配置资源的基础作用，拓宽投融资渠道，改善投融资环境，鼓励国内外资金，包括私营企业资金投入垃圾处理设施的建设和运行，最终建立符合市场经济要求的垃圾处理运行机制，解决当前垃圾处理能力不足所造成的环境污染问题。
60.地方环境质量标准和污染物排放标准备案管理办法(环境保护部令第9号 《地方环境质量标准和污染物排放标准备案管理办法》已由环境保护部2009年第三次部务会议于2009年12月30日修订通过。现将修订后的《地方环境质量标准和污染物排放标准备案管理办法》公布,自2010年3月1日起施行。 2004年11月11日原国家环境保护总局发布的《地方环境质量标准和污染物排放标准备案管理办法》同时废止。 环境保护部部长周生贤 二○一○年一月二十八日地方环境质量标准和污染物排放标准备案管理办法 第一条 [立法目的] 为加强对地方环境质量标准和污染物排放标准的备案管理,根据《中华人民共和国环境保护法》、《中华人民共和国大气污染防治法》和《中华人民共和国水污染防治法》,制定本办法。 第二条 [适用范围] 本办法适用于环境保护部对省、自治区、直辖市人民政府依法制定的地方环境质量标准和污染物排放标准的备案管理。 地方机动车船大气污染物排放标准的管理,依照经国务院批准、原国家环境保护总局发布的《地方机动车大气污染物排放标准审批办法》执行。 第三条 [报备时限] 省、自治区、直辖市人民政府或者受其委托的环境保护行政主管部门应当在地方环境质量标准和污染物排放标准发布之日起45日内,向环境保护部备案。 第四条 [报备材料] 向环境保护部报送备案,应当提交下列材料(一式三份: (一报送备案的函; (二省、自治区、直辖市人民政府批准地方环境质量标准和污染物排放标准的文件,以及地方环境质量标准和污染物排放标准的发布文件;
(三地方环境质量标准和污染物排放标准文本的纸质文件和电子文件; (四地方环境质量标准和污染物排放标准编制说明的纸质文件和电子文件。 第五条 [审查和处理] 环境保护部在收到地方环境质量标准和污染物排放标准备案材料之日起45日内完成备案审查,并根据审查情况作如下处理: (一对符合本办法第七、八、九条规定的,予以备案,并在环境保护部网站公布备案信息。 (二对不符合本办法第七、八、九条规定的,不予备案,并函复报送备案的省、自治区、直辖市人民政府或者受其委托的环境保护行政主管部门,说明理由。 第六条 [暂缓备案] 地方污染物排放标准无法与国家污染物排放标准中 的项目限值、控制要求比较宽严关系的,环境保护部暂缓备案。 对暂缓备案的,环境保护部应当在收到备案材料之日起45日内书面说明理由,通知报送备案的省、自治区、直辖市人民政府或者受其委托的环境保护行政主管部门重新备案;重新备案的标准符合规定的,予以备案。 第七条 [质量标准备案要求] 报送备案的地方环境质量标准,应当符合下列要求: (一已经省、自治区、直辖市人民政府批准; (二对国家环境质量标准中未规定的污染物项目,补充制定地方环境质量标准。 第八条 [排放标准备案要求] 报送备案的地方污染物排放标准应当符合下列要求: (一已经省、自治区、直辖市人民政府批准; (二地方污染物排放标准应当参照国家污染物排放标准的体系结构制定,可以是行业型污染物排放标准和综合型污染物排放标准。行业型污染物排放标准适用于特
国家环境保护总局文件 环发〔2007〕56号 关于印发《全国环境监测站建设标准》的通知 各省、自治区、直辖市环境保护局（厅），新疆生产建设兵团环境保护局，中国环境监测总站： 为适应新时期环境监测能力建设的需要，加快建设先进的环境监测预警体系，我局组织制定了《全国环境监测站建设标准》，现印发给你们，请遵照执行。 附件：全国环境监测站建设标准 二○○七年四月二十三日 主题词：环保建设标准通知 抄送：财政部。
附件：全国环境监测站建设标准 全国环境监测站建设标准 为建设先进的环境监测预警体系，指导和规范全国各级环境监测机构能力建设，特制定本标准。有关辐射环境监测站的建设标准另行制定。本标准自发布之日起执行，原《环境监测站建设标准（试行）》同时废止。 本标准规定了省、市、县三级环境监测机构人员标准及机构、监测经费、监测用房、基本仪器配置、应急环境监测仪器配置和专项监测仪器配置。本标准为最低配置标准，有能力的地区可以适当提高标准。 本标准实行分级设置，分为一级、二级、三级。一级标准为各省（自治区、直辖市）设置的环境监测站、由国家环保总局批准的各专业环境监测站；二级标准为各地级市（自治州）、直辖市所辖区（县）设置的环境监测站执行；三级标准为各地级市（自治州）所辖区、县（自治县）设置的环境监测站执行。 每个级别（按照国务院确定的东部、中部、西部区域划分方法）划分为东部地区、中部地区、西部地区三档，处于不同区域的环境监测站执行不同的标准。直辖市及其所辖区（县）环境监测站分别执行东部地区一级、二级标准。 本标准规定了各级环境监测机构人员编制标准、环境监测技术人员占总人数的比例及高级、中级技术人员比例，详见表1。 表1 人员编制及人员结构 监测站 级别适用范围人员编制（人） 环境监测技术 人员比例 高、中级专业技术人员比例 一级东部地区不少于120 人 不低于85% 高级技术人员占技术人员总 数比例不低于25％，中级不低 于45％ 中部地区不少于100 人 西部地区不少于90 人 二级东部地区不少于150 人 不低于85% 高级技术人员占技术人员总 数比例不低于20％，中级不低 于50％ 中部地区不少于100 人 西部地区不少于70 人 三级东部地区不少于20 人 不低于75% 中级以上技术人员占技术人 员总数比例不低于50％ 中部地区不少于18 人 西部地区不少于10 人
国家环境保护总局令第29号 国家环境保护总局建设项目环境影响评价文件审批 程序规定 《国家环境保护总局建设项目环境影响评价文件审批程序规定》已于2005年10月27日由国家环境保护总局2005年第二十次局务会议通过，现予公布，自2006年1月1日起施行。 国家环境保护总局局长解振华二○○五年十一月二十三日 主题词：环保法规环境影响评价审批程序令 环境保护总局建设项目环境影响评价文件审批程序规定 第一章总则 第一条为规范国家环境保护总局（以下简称“环保总局”）建设项目环境影响评价文件审批行为，提高审批行为的科学性和民主性，保护公民、法人和其他组织的合法权益，根据《中华人民共和国行政许可法》、《中华人民共和国环境影响评价法》和《国务院关于投资体制改革的决定》，制定本规定。
第二条本规定所称建设项目环境影响评价文件，是指建设项目环境影响报告书、环境影响报告表和环境影响登记表的统称。 第三条本规定适用于环保总局负责审批的建设项目环境影响评价文件的审批。 第四条按照国家规定实行审批制的建设项目，建设单位应当在报送可行性研究报告前报批环境影响评价文件。 按照国家规定实行核准制的建设项目，建设单位应当在提交项目申请报告前报批环境影响评价文件。 按照国家规定实行备案制的建设项目，建设单位应当在办理备案手续后和开工前报批环境影响评价文件。 第五条环保总局审批建设项目环境影响评价文件，遵循公开、公平、公正原则，做到便民和高效。 第二章申请与受理 第六条建设单位按照环保总局公布的《建设项目环境保护分类管理名录》的规定，组织编制环境影响报告书、环境影响报告表或者填报环境影响登记表。