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美国环保局 EPA 试验方法 EPA 3550c

METHOD 3550C

ULTRASONIC EXTRACTION

SW-846 is not intended to be an analytical training manual. Therefore, method procedures are written based on the assumption that they will be performed by analysts who are formally trained in at least the basic principles of chemical analysis and in the use of the subject technology.

In addition, SW-846 methods, with the exception of required method use for the analysis of method-defined parameters, are intended to be guidance methods which contain general information on how to perform an analytical procedure or technique which a laboratory can use as a basic starting point for generating its own detailed Standard Operating Procedure (SOP), either for its own general use or for a specific project application. The performance data included in this method are for guidance purposes only, and are not intended to be and must not be used as absolute QC acceptance criteria for purposes of laboratory accreditation.

1.0SCOPE AND APPLICATION

1.1This method describes a procedure for extracting nonvolatile and semivolatile organic compounds from solids such as soils, sludges, and wastes. The ultrasonic process ensures intimate contact of the sample matrix with the extraction solvent.

1.2This method is divided into two procedures, based on the expected concentration of organic compounds. The low concentration procedure (Sec. 11.3) is for individual organic components expected at less than or equal to 20 mg/kg and uses the larger sample size and three serial extractions (lower concentrations are more difficult to extract). The medium/high concentration procedure (Sec. 11.4) is for individual organic components expected at greater than 20 mg/kg and uses the smaller sample and a single extraction.

1.3It is highly recommended that the extracts be subject to some form of cleanup

(e.g., using a method from the 3600 series) prior to analysis.

1.4Because of the limited contact time between the solvent and the sample, ultrasonic extraction may not be as rigorous as other extraction methods for soils/solids. Therefore, it is critical that the method (including the manufacturer's instructions) be followed explicitly, in order to achieve the maximum extraction efficiency. See Sec. 11.0 for a discussion of the critical aspects of the extraction procedure. Consult the manufacturer's instructions regarding specific operational settings.

1.5This method describes at least three extraction solvent systems that may be employed for different groups of analytes (see Sec. 7.4). Other solvent systems may be employed, provided that adequate performance can be demonstrated for the analytes of interest. The choice of extraction solvent will depend on the analytes of interest and no single solvent is universally applicable to all analyte groups. As a result of concerns about the efficiency of ultrasonic extraction, particularly at concentrations near or below about 10 μg/kg, it is imperative that the analyst demonstrate the performance of the specific solvent system and operating conditions for the analytes of interest and the concentrations of interest. This demonstration applies to any solvent system that is employed, including those specifically listed in this method. At a minimum, such a demonstration will encompass the initial demonstration of proficiency described in Method 3500, using a clean reference matrix. Method 8000 describes

procedures that may be used to develop performance criteria for such demonstrations as well as for matrix spike and laboratory control sample results.

1.6EPA notes that there are limited published data on the efficiency of ultrasonic extraction with regard to organophosphorus pesticides at low part-per-billion (ppb) concentrations and below. As a result, use of this method for these compounds in particular should be supported by performance data such as those discussed above and in Method 3500.

1.7Prior to employing this method, analysts are advised to consult the base method for each type of procedure that may be employed in the overall analysis (e.g., Methods 3500, 3600, 5000, and 8000) for additional information on quality control procedures, development of QC acceptance criteria, calculations, and general guidance. Analysts also should consult the disclaimer statement at the front of the manual and the information in Chapter Two for guidance on the intended flexibility in the choice of methods, apparatus, materials, reagents, and supplies, and on the responsibilities of the analyst for demonstrating that the techniques employed are appropriate for the analytes of interest, in the matrix of interest, and at the levels of concern.

In addition, analysts and data users are advised that, except where explicitly specified in a regulation, the use of SW-846 methods is not mandatory in response to Federal testing requirements. The information contained in this method is provided by EPA as guidance to be used by the analyst and the regulated community in making judgments necessary to generate results that meet the data quality objectives for the intended application.

1.8Use of this method is restricted to use by, or under the supervision of, appropriately experienced and trained analysts. Each analyst must demonstrate the ability to generate acceptable results with this method. As noted above, such demonstrations are specific to the analytes of interest and the solvent system used, as well as to the procedures for low and medium/high concentration samples.

2.0SUMMARY OF METHOD

2.1Low concentration procedure -- The sample is mixed with anhydrous sodium sulfate to form a free-flowing powder. The mixture is extracted with solvent three times, using ultrasonic extraction. The extract is separated from the sample by vacuum filtration or centrifugation. The extract is ready for final concentration, cleanup, and/or analysis.

2.2Medium/high concentration procedure -- The sample is mixed with anhydrous sodium sulfate to form a free-flowing powder. This is extracted with solvent once, using ultrasonic extraction. A portion of the extract is collected for cleanup and/or analysis.

3.0DEFINITIONS

Refer to Chapter One and the manufacturer's instructions for definitions that may be relevant to this method.

4.0INTERFERENCES

4.1Solvents, reagents, glassware, and other sample processing hardware may yield artifacts and/or interferences to sample analysis. All of these materials must be demonstrated to be free from interferences under the conditions of the analysis by analyzing method blanks.

Specific selection of reagents and purification of solvents by distillation in all-glass systems may be necessary. Refer to each method to be used for specific guidance on quality control procedures and to Chapter Four for general guidance on the cleaning of glassware.

4.2Interferences are usually specific to the analytes of interest. Therefore, refer to Method 3500 and the appropriate determinative methods for specific guidance on extraction interferences.

5.0SAFETY

This method does not address all safety issues associated with its use. The laboratory is responsible for maintaining a safe work environment and a current awareness file of OSHA regulations regarding the safe handling of the chemicals listed in this method. A reference file of material safety data sheets (MSDSs) should be available to all personnel involved in these analyses.

6.0EQUIPMENT AND SUPPLIES

The mention of trade names or commercial products in this manual is for illustrative purposes only, and does not constitute an EPA endorsement or exclusive recommendation for use. The products and instrument settings cited in SW-846 methods represent those products and settings used during method development or subsequently evaluated by the Agency. Glassware, reagents, supplies, equipment, and settings other than those listed in this manual may be employed provided that method performance appropriate for the intended application has been demonstrated and documented.

This section does not list common laboratory glassware (e.g., beakers and flasks).

6.1Apparatus for grinding dry waste samples.

6.2Ultrasonic preparation -- A horn-type device equipped with a titanium tip, or a device that will give appropriate performance, must be used.

6.2.1Ultrasonic disrupter -- The disrupter must have a minimum power wattage

of 300 watts, with pulsing capability. A device designed to reduce the cavitation sound is recommended. Follow the manufacturers instructions for preparing the disrupter for

extraction of samples with low and medium/high concentrations.

6.2.2Use a 3/4-inch horn for the low concentration method procedure and a

1/8-inch tapered microtip attached to a 1/2-inch horn for the medium/high concentration method procedure.

6.3Sonabox -- Recommended with the above disrupters for decreasing cavitation sound (Heat Systems - Ultrasonics, Inc., Model 432B or equivalent).

6.4Apparatus for determining percent dry weight

6.4.1Drying oven -- Capable of maintaining 105 E C.

6.4.2Desiccator.

6.4.3Crucibles -- Porcelain or disposable aluminum.

6.5Pasteur pipets -- 1-mL, glass, disposable.

6.7Vacuum or pressure filtration apparatus

6.7.1Buchner funnel

6.7.2Filter paper -- Whatman No. 41 or equivalent.

6.8Kuderna-Danish (K-D) apparatus

6.8.1Concentrator tube -- 10-mL, graduated (Kontes K-570050-1025 or

equivalent). A ground-glass stopper is used to prevent evaporation of extracts.

6.8.2Evaporation flask -- 500-mL (Kontes K-570001-500 or equivalent). Attach

the flask to the concentrator tube with springs, clamps, or equivalent.

6.8.3Snyder column -- Three-ball macro (Kontes K-503000-0121 or

equivalent).

6.8.4Snyder column -- Two-ball micro (Kontes K-569001-0219 or equivalent).

6.8.5Springs -- 1/2-inch (Kontes K-662750 or equivalent).

6.9Solvent vapor recovery system (Kontes K-545000-1006 or K-547300-0000, Ace Glass 6614-30, or equivalent).

NOTE:This glassware is recommended for the purpose of solvent recovery during the concentration procedures requiring the use of Kuderna-Danish evaporative

concentrators. Incorporation of this apparatus may be required by Federal, State or

local municipality regulations that govern air emissions of volatile organics. EPA

recommends the incorporation of this type of reclamation system as a method to

implement an emissions reduction program. Solvent recovery is a means to conform

with waste minimization and pollution prevention initiatives.

6.10Boiling chips -- Solvent-extracted, approximately 10/40 mesh (silicon carbide or equivalent).

6.11Water bath -- Heated, with a concentric ring cover, capable of temperature control to ± 5 E C. The bath should be used in a hood.

6.12Balance -- Top-loading, capable of accurately weighing to the nearest 0.01 g.

6.13Vials -- 2-mL, for GC autosampler, equipped with polytetrafluoroethylene (PTFE)-lined screw caps or crimp tops.

6.14Glass scintillation vials -- 20-mL, equipped with PTFE-lined screw caps.

6.15Spatula -- Stainless steel or PTFE.

6.16Drying column -- 20-mm ID borosilicate glass chromatographic column with glass wool at the bottom.

NOTE:Columns with fritted glass discs are difficult to decontaminate after they have been used to dry highly-contaminated extracts. Columns without frits may be purchased.

Use a small pad of glass wool to retain the adsorbent. Prewash the glass wool pad with 50 mL of acetone followed by 50 mL of the elution solvent prior to packing the column with adsorbent.

6.17Nitrogen evaporation apparatus (optional) -- N-Evap, 12- or 24-position (Organomation Model 112, or equivalent).

7.0

REAGENTS AND STANDARDS

7.1Reagent-grade chemicals must be used in all tests. Unless otherwise indicated, it is intended that all reagents 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. Reagents should be stored in glass to prevent the leaching of contaminants from plastic containers.

7.2Organic-free reagent water. All references to water in this method refer to organic-free reagent water, as defined in Chapter One.

7.3Sodium sulfate (granular, anhydrous), Na 2SO 4. Purify by heating at 400 E C for 4hrs 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 should be analyzed,demonstrating that there is no interference from the sodium sulfate.

7.4

Extraction solvents

Samples should be extracted using a solvent system that gives optimum, reproducible recovery of the analytes of interest from the sample matrix, at the concentrations of interest. The choice of extraction solvent will depend on the analytes of interest and no single solvent is universally applicable to all analyte groups. Whatever solvent system is employed, including those specifically listed in this method, the analyst must demonstrate adequate performance for the analytes of interest, at the levels of interest. At a minimum, such a demonstration will encompass the initial demonstration of proficiency described in Method 3500, using a clean

reference matrix. Method 8000 describes procedures that may be used to develop performance criteria for such demonstrations as well as for matrix spike and laboratory control sample results.

Many of the solvent systems described below include the combination of a water-miscible solvent, such as acetone, and a water-immiscible solvent, such as methylene chloride or

hexane. The purpose of the water-miscible solvent is to facilitate the extraction of wet solids by allowing the mixed solvent to penetrate the layer of water of the surface of the solid particles. The water-immiscible solvent extracts organic compounds with similar polarities. Thus, a non-polar solvent such as hexane is often used for non-polar analytes such as PCBs, while a polar solvent like methylene chloride may be used for polar analytes. The polarity of acetone may also help extract polar analytes in mixed solvent systems.

Table 1 provides example recovery data for selected semivolatile organic compounds extracted from an NIST SRM using various extraction solvent systems. The following sections provide guidance on the choice of solvents for various classes of analytes.

All solvents should be pesticide quality or equivalent. Solvents may be degassed prior to use.

7.4.1Semivolatile organics may be extracted with acetone/hexane (1:1, v/v

CH 3COCH 3/C 6H 14), or acetone/methylene chloride (1:1,v/v CH 3COCH 3/CH 2Cl 2).7.4.2Organochlorine pesticides may be extracted with acetone/hexane (1:1,

v/v CH 3COCH 3/C 6H 14), or acetone/methylene chloride (1:1,v/v CH 3COCH 3/CH 2Cl 2).7.4.3PCBs may be extracted with acetone/hexane (1:1, v/v CH 3COCH 3/C 6H 14),

acetone/methylene chloride (1:1, v/v CH 3COCH 3/CH 2Cl 2) or hexane (C 6H 14).

7.4.4Other solvent systems may be employed, provided that the analyst can

demonstrate adequate performance for the analytes of interest, at the concentrations of interest, in the sample matrix (see Method 3500).

7.5Exchange solvents -- With the use of some determinative methods, the extraction solvent will need to be exchanged to a solvent compatible with the instrumentation used in that determinative method. Refer to the determinative method to be used for selection of the

appropriate exchange solvent. All solvents must be pesticide quality or equivalent. Examples of exchange solvents are given below.

7.5.1Hexane, C 6H 14

7.5.22-Propanol, (CH 3)2CHOH 7.5.3Cyclohexane, C 6H 127.5.4Acetonitrile, CH 3CN 7.5.5

Methanol, CH 3OH

8.0

SAMPLE COLLECTION, PRESERVATION, AND STORAGE

8.1See the introductory material to Chapter Four, "Organic Analytes," Method 3500,and the specific determinative methods to be employed.

8.2Solid samples to be extracted by this procedure should be collected and stored like any other solid samples containing semivolatile organics.9.0

QUALITY CONTROL

9.1Refer to Chapter One for additional guidance on quality assurance (QA) and quality control (QC) protocols. When inconsistencies exist between QC guidelines, method-specific QC criteria take precedence over both technique-specific criteria and those criteria given in Chapter One, and technique-specific QC criteria take precedence over the criteria in Chapter One. Any effort involving the collection of analytical data should include development of a structured and systematic planning document, such as a Quality Assurance Project Plan (QAPP) or a Sampling and Analysis Plan (SAP), which translates project objectives and

specifications into directions for those that will implement the project and assess the results. Each laboratory should maintain a formal quality assurance program. The laboratory should also maintain records to document the quality of the data generated. All data sheets and quality control data should be maintained for reference or inspection.

9.2Initial demonstration of proficiency

Each laboratory must demonstrate initial proficiency with each sample preparation and determinative method combination it utilizes by generating data of acceptable accuracy and precision for target analytes in a clean matrix. The laboratory must also repeat the demonstration of proficiency whenever new staff members are trained or significant changes in instrumentation are made. See Method 8000 for information on how to accomplish a demonstration of proficiency.

9.3Initially, before processing any samples, the analyst should demonstrate that all parts of the equipment in contact with the sample and reagents are interference-free. This is accomplished through the analysis of a method blank. As a continuing check, each time samples are extracted, cleaned up, and analyzed, and when there is a change in reagents, a method blank should be extracted and analyzed for the compounds of interest as a safeguard against chronic laboratory contamination.

9.4Any method blanks, matrix spike samples, or replicate samples should be subjected to the same analytical procedures (Sec. 11.0) as those used on actual samples.

9.5Standard quality assurance practices should be used with this method as included in appropriate systematic planning documents and laboratory SOPs. All instrument operating conditions should be recorded.

9.6Also refer to Method 3500 for extraction and sample preparation quality control procedures and the determinative methods to be used for determinative QC procedures.

9.7When listed in the appropriate determinative method, surrogate standards should be added to all samples prior to extraction. See Methods 3500 and 8000, and the appropriate determinative methods for more information.

9.8As noted earlier, use of any extraction technique, including ultrasonic extraction, should be supported by data that demonstrate the performance of the specific solvent system and operating conditions for the analytes of interest, at the levels of interest, in the sample matrix.

10.0CALIBRATION AND STANDARDIZATION

There are no calibration or standardization steps directly associated with this sample extraction procedure.

11.0PROCEDURE

As noted in Sec. 1.4, ultrasonic extraction may not be as rigorous a method as other extraction methods for soils/solids. Therefore, it is critical that this method be followed explicitly (including the manufacturer's instructions) to achieve the maximum extraction efficiency. At a minimum, for successful use of this technique:

?The extraction device must have a minimum of 300 watts of power and be equipped with appropriate size disrupter horns (see Sec. 6.2).

?The horn must be properly maintained, including tuning according to the manufacturer's instructions prior to use, and inspection of the horn tip for excessive wear.

?The sample must be properly prepared by thoroughly mixing it with sodium sulfate, so that it forms a free-flowing powder prior to the addition of the solvent.

?The extraction horns used for the low concentration and high concentration protocols (Secs. 11.3 and 11.4, respectively) are not interchangeable. Results indicate that the use of the 3/4-inch horn is inappropriate for the high concentration procedure, particularly for extraction of very non-polar organic compounds such as PCBs, which are strongly

adsorbed to the soil matrix.

?For low concentration samples, three extractions are performed with the appropriate solvent, the extraction is performed in the designated pulse mode, and the horn tip is

positioned just below the surface of the solvent, yet above the sample. The same

approach is used for high concentration samples, except that only one extraction may be needed.

?Very active mixing of the sample and the solvent must occur when the ultrasonic pulse is activated. The analyst must observe such mixing at some point during the extraction

process.

11.1Sample handling

11.1.1Sediment/soil samples -- Decant and discard any water layer on a

sediment sample. Discard any foreign objects such as sticks, leaves, and rocks. Mix the sample thoroughly, especially composited samples.

11.1.2Waste samples -- Samples consisting of multiple phases must be

prepared before extraction by the phase separation procedure described in Chapter Two.

This extraction procedure is for solids only.

11.1.3Dry waste samples amenable to grinding -- Grind or otherwise subdivide

the waste so that it either passes through a 1-mm sieve or can be extruded through a 1-mm hole. Introduce sufficient sample into the grinding apparatus to yield at least 10 g

after grinding.

CAUTION:Drying and grinding should be performed in a hood, to avoid contamination of the laboratory.

11.1.4Gummy, fibrous, or oily materials not amenable to grinding -- Cut, shred,

or otherwise reduce in size these materials to allow mixing and maximum exposure of the sample surfaces for the extraction.

11.2Determination of percent dry weight -- When sample results are to be calculated on

a dry weight basis, a separate portion of sample should be weighed out at the same time as the portion used for analytical determination.

CAUTION:The drying oven should be contained in a hood or vented. Significant laboratory contamination may result from a heavily contaminated hazardous waste sample.

Immediately after weighing the sample aliquot to be extracted, weigh an additional 5- to

10-g aliquot of the sample into a tared crucible. Dry this aliquot overnight at 105 E C. Allow to cool in a desiccator before weighing.

Calculate the percent dry weight as follows:

%dry weight'g of dry sample

g of sample

×100

This oven-dried aliquot is not used for the extraction and should be appropriately disposed of once the dry weight is determined.

11.3Low concentration extraction procedure

This procedure applies to solid samples that are expected to contain less than or equal to 20 mg/kg of organic analytes.

NOTE:Add the surrogates and matrix spiking compounds to the sample aliquot prior to mixing the sample with the sodium sulfate drying agent. Spiking the sample first increases

the contact time of the spiked compounds and the actual sample matrix. It should also lead to better mixing of the spiking solution with the sample when the sodium sulfate

and sample are mixed to the point of free-flowing.

11.3.1The following steps should be performed rapidly to avoid loss of the more

volatile extractables.

11.3.1.1Weigh approximately 30 g of sample into a 400-mL beaker.

Record the weight to the nearest 0.1 g.

11.3.1.2For the sample in each batch selected for spiking, add 1.0 mL

of the matrix spiking solution. Consult Method 3500 for guidance on the

appropriate choice of matrix spiking compounds and concentrations. Also see the

note in Sec. 11.3.

11.3.1.3Add 1.0 mL of the surrogate standard solution to all samples,

spiked samples, QC samples, and blanks. Consult Method 3500 for guidance on

the appropriate choice of surrogate compounds and concentrations. Also see the

note in Sec. 11.3.

11.3.1.4If gel permeation cleanup (see Method 3640) is to be

employed, the analyst should either add twice the volume of the surrogate spiking

solution (and matrix spiking solution, where applicable), or concentrate the final

extract to half the normal volume, to compensate for the half of the extract that is

lost due to loading of the GPC column. Also see the note in Sec. 11.3.

11.3.1.5Nonporous or wet samples (gummy or clay type) that do not

have a free-flowing sandy texture must be mixed with 60 g of anhydrous sodium

sulfate, using a spatula. If needed, more sodium sulfate may be added. After

addition of sodium sulfate, the sample should be free flowing. Also see the note in

Sec. 11.3.

11.3.1.6Immediately add 100 mL of the extraction solvent or solvent

mixture (see Sec. 7.4 and Table 2 for information on the choice of solvents).

11.3.2Place the bottom surface of the tip of the 3/4-inch disrupter horn about

1/2-inch below the surface of the solvent, but above the sediment layer.

NOTE:Be sure that the horn is properly tuned according to the manufacturer's

instructions.

11.3.3Extract the sample ultrasonically for 3 min, with output control knob set at

10 (full power) or at the manufacturer’s recommended power setting, the mode switch on

Pulse (pulsing energy rather than continuous energy), and the percent-duty cycle knob set at 50% (energy on 50% of time and off 50% of time). Do not use the microtip probe.

11.3.4Decant the extract and filter it through Whatman No. 41 filter paper (or

equivalent) in a Buchner funnel that is attached to a clean 500-mL filtration flask.

Alternatively, decant the extract into a centrifuge bottle and centrifuge at low speed to

remove particles.

11.3.5Repeat the extraction two more times with two additional 100-mL portions

of clean solvent. Decant off the solvent after each ultrasonic extraction. After the final

ultrasonic extraction, pour the entire sample into the Buchner funnel, rinse the beaker with extraction solvent, and add the rinse to the funnel. Apply a vacuum to the filtration flask, and collect the solvent extract. Continue filtration until all visible solvent is removed from the funnel, but do not attempt to completely dry the sample, as the continued application of a vacuum may result in the loss of some analytes. Alternatively, if centrifugation is used in Sec. 11.3.4, transfer the entire sample to the centrifuge bottle. Centrifuge at low speed, and then decant the solvent from the bottle.

11.3.6If necessary, concentrate the extract prior to analysis following the

procedure in Sec. 11.5. Otherwise, proceed to Sec. 11.7.

11.4Medium/high concentration extraction procedure

This procedure applies to solid samples that are expected to contain more than 20 mg/kg of organic analytes.

11.4.1Transfer approximately 2 g of sample to a 20-mL vial. Wipe the mouth of

the vial with a tissue to remove any sample material. Cap the vial before proceeding with the next sample to avoid any cross-contamination. Record the weight to the nearest 0.1 g.

11.4.2For the sample in each batch selected for spiking, add 1.0 mL of the

matrix spiking solution. Consult Method 3500 for guidance on the appropriate choice of matrix spiking compounds and concentrations. Also see the note in Sec. 11.3.

11.4.3Add 1.0 mL of surrogate spiking solution to all samples, spiked samples,

QC samples, and blanks. Consult Method 3500 for guidance on the appropriate choice of matrix spiking compounds and concentrations. Also see the note in Sec. 11.3.

11.4.4If gel permeation cleanup (see Method 3640) is to be employed, the

analyst should either add twice the volume of the surrogate spiking solution (and matrix spiking solution, where applicable), or concentrate the final extract to half the normal

volume, to compensate for the half of the extract that is lost due to loading of the GPC

column.

11.4.5Nonporous or wet samples (gummy or clay type) that do not have a free-

flowing sandy texture must be mixed with 2 g of anhydrous sodium sulfate, using a

spatula. If needed, more sodium sulfate may be added. After addition of sodium sulfate, the sample should be free flowing (see the note in Sec. 11.3).

11.4.6Immediately add whatever volume of solvent is necessary to bring the

final volume to 10.0 mL, considering the added volume of surrogates and matrix spikes (see Sec. 7.4 and Table 2 for information on the choice of solvents).

11.4.7Extract the sample with the 1/8-inch tapered microtip ultrasonic probe for

2 min at output control setting 5 and with mode switch on pulse and percent duty cycle at

50%.

11.4.8Loosely pack a disposable Pasteur pipette with 2 to 3 cm of glass wool.

Filter the sample extract through the glass wool and collect the extract in a suitable

container. The entire 10 mL of extraction solvent cannot be recovered from the sample.

Therefore, the analyst should collect a volume appropriate for the sensitivity of the

determinative method to be used. For instance, for methods that do not need the extract to be concentrated further (e.g., Method 8081 typically employs a final extract volume of

10 mL), the extract may be collected in a scintillation vial or other sealable container. For

extracts that will need further concentration, it is advisable to collect a standard volume for all such samples in order to simplify the calculation of the final sample results. For

instance, collect 5.0 mL of extract in a clean concentrator tube. This volume represents exactly half of the total volume of the original sample extract. As necessary, account for the "loss" of half of the extract in the final sample calculations, or concentrate the final

extract to one-half the nominal final volume (e.g., 0.5 mL vs. 1.0 mL) to compensate for the loss.

11.4.9If necessary, concentrate the extract prior to analysis following the

procedure in Sec. 11.5 or Sec. 11.6. Otherwise, proceed to Sec. 11.7.

11.5K-D concentration technique

Where necessary to meet the sensitivity criteria, sample extracts from either the low concentration or medium/high concentration extraction procedure may be concentrated to the final volume necessary for the determinative method and specific application to be used, using either the K-D technique or nitrogen evaporation.

11.5.1Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-mL

concentrator tube to an appropriately sized evaporation flask.

11.5.2Dry the extract by passing it through a drying column containing about 10

g of anhydrous sodium sulfate. Collect the dried extract in the K-D concentrator.

11.5.3Rinse the collection tube and drying column into the K-D flask with an

additional 20-mL portion of solvent in order to achieve a quantitative transfer.

11.5.4Add one or two clean boiling chips to the flask and attach a three-ball

Snyder column. Attach the solvent vapor recovery glassware (condenser and collection device, see Sec. 6.9) to the Snyder column of the K-D apparatus, following the

manufacturer's instructions. Pre-wet the Snyder column by adding about 1 mL of

methylene chloride (or other suitable solvent) to the top of the column. Place the K-D

apparatus on a hot water bath (15 - 20 E C above the boiling point of the solvent) so that the concentrator tube is partially immersed in the hot water and the entire lower rounded surface of the flask is bathed with hot vapor. Adjust the vertical position of the apparatus and the water temperature as needed to complete the concentration in 10 - 20 min. At the proper rate of distillation, the balls of the column will actively chatter, but the chambers will not flood. When the apparent volume of liquid reaches 1 mL, remove the K-D apparatus from the water bath and allow it to drain and cool for at least 10 min.

CAUTION: Do not let the extract go to dryness, as this will result in severe loss of some analytes. Organophosphorus pesticides are particularly susceptible to such

losses.

11.5.4.1If a solvent exchange is necessary (as indicated in Table 2 or

the appropriate determinative method), momentarily remove the Snyder column,

add 50 mL of the exchange solvent and a new boiling chip.

11.5.4.2Reattach the Snyder column. Concentrate the extract, raising

the temperature of the water bath, if necessary, to maintain a proper distillation

rate.

11.5.5Remove the Snyder column. Rinse the K-D flask and the lower joints of

the Snyder column into the concentrator tube with 1 - 2 mL of solvent. The extract may be further concentrated by using one of the techniques outlined in Sec. 11.6, or adjusted to a final volume of 5.0 - 10.0 mL using an appropriate solvent (see Table 2 or the appropriate determinative method). If sulfur crystals are present, proceed to Method 3660 for cleanup.

11.6If further concentration is necessary, use either the micro-Snyder column technique (see Sec. 11.6.1) or nitrogen evaporation technique (see Sec. 11.6.2).

11.6.1Micro-Snyder column technique

11.6.1.1Add a fresh clean boiling chip to the concentrator tube and

attach a two-ball micro-Snyder column directly to the concentrator tube. Attach the

solvent vapor recovery glassware (condenser and collection device) to the micro-

Snyder column of the K-D apparatus, following the manufacturer's instructions.

Pre-wet the Snyder column by adding 0.5 mL of methylene chloride or the

exchange solvent to the top of the column. Place the micro-concentration

apparatus in a hot water bath so that the concentrator tube is partially immersed in

the hot water. Adjust the vertical position of the apparatus and the water

temperature, as necessary, to complete the concentration in 5 - 10 min. At the

proper rate of distillation the balls of the column will actively chatter, but the

chambers will not flood.

11.6.1.2When the apparent volume of liquid reaches 0.5 mL, remove

the apparatus from the water bath and allow it to drain and cool for at least 10 min.

Remove the Snyder column and rinse its lower joints into the concentrator tube

with 0.2 mL of solvent. Adjust the final extract volume to 1.0 - 2.0 mL.

CAUTION:Do not let the extract go to dryness, as this will result in severe loss

of some analytes. Organophosphorus pesticides are particularly

susceptible to such losses.

11.6.2Nitrogen evaporation technique

11.6.2.1Place the concentrator tube in a warm bath (30 E C) and

evaporate the solvent volume to 0.5 mL using a gentle stream of clean, dry

nitrogen (filtered through a column of activated carbon).

CAUTION:New plastic tubing must not be used between the carbon trap and the

sample, since it may introduce phthalate interferences.

11.6.2.2Rinse down the internal wall of the concentrator tube several

times with solvent during the concentration. During evaporation, position the

concentrator tube to avoid condensing water into the extract. Under normal

procedures, the extract must not be allowed to become dry.

CAUTION:Do not let the extract go to dryness, as this will result in severe loss

of some analytes. Organophosphorus pesticides are particularly

susceptible to such losses.

11.7The extract may now be subjected to cleanup procedures or analyzed for the target analytes using the appropriate determinative technique(s). If further handling of the extract will not be performed immediately, stopper the concentrator tube and store in a refrigerator. If the extract will be stored longer than 2 days, it should be transferred to a vial equipped with a PTFE-lined screw-cap, and labeled appropriately.

12.0DATA ANALYSIS AND CALCULATIONS

There are no calculations explicitly associated with this extraction procedure. See the appropriate determinative method for the calculation of final sample results.

13.0METHOD PERFORMANCE

Refer to the appropriate determinative methods for performance data examples and guidance. Performance data and related information are provided in SW-846 methods only as examples and guidance. The data do not represent required performance criteria for users of the methods. Instead, performance criteria should be developed on a project-specific basis, and the laboratory should establish in-house QC performance criteria for the application of this method. These performance data are not intended to be and must not be used as absolute QC acceptance criteria for purposes of laboratory accreditation.

14.0POLLUTION PREVENTION

14.1Pollution prevention encompasses any technique that reduces or eliminates the quantity and/or toxicity of waste at the point of generation. Numerous opportunities for pollution prevention exist in laboratory operation. The EPA has established a preferred hierarchy of environmental management techniques that places pollution prevention as the management option of first choice. Whenever feasible, laboratory personnel should use pollution prevention techniques to address their waste generation. When wastes cannot be feasibly reduced at the source, the Agency recommends recycling as the next best option.

14.2For information about pollution prevention that may be applicable to laboratories and research institutions consult Less is Better: Laboratory Chemical Management for Waste Reduction available from the American Chemical Society's Department of Government Relations and Science Policy, 1155 16th St., N.W. Washington, D.C. 20036, https://www.docsj.com/doc/f9129011.html,.

15.0WASTE MANAGEMENT

The Environmental Protection Agency requires that laboratory waste management practices be conducted consistent with all applicable rules and regulations. The Agency urges laboratories to protect the air, water, and land by minimizing and controlling all releases from

hoods and bench operations, complying with the letter and spirit of any sewer discharge permits and regulations, and by complying with all solid and hazardous waste regulations, particularly the hazardous waste identification rules and land disposal restrictions. For further information on waste management, consult The Waste Management Manual for Laboratory Personnel available from the American Chemical Society at the address listed in Sec. 14.2.

16.0REFERENCES

1.U.S. EPA, "Interlaboratory Comparison Study: Methods for Volatile and Semi-Volatile

Compounds," Environmental Monitoring Systems Laboratory, Office of Research and

Development, Las Vegas, NV, EPA 600/4-84-027, 1984.

2. C. S. Hein, P. J. Marsden, A. S. Shurtleff, "Evaluation of Methods 3540 (Soxhlet) and 3550

(Sonication) for Evaluation of Appendix IX Analytes from Solid Samples," S-CUBED,

Report for EPA Contract 68-03-33-75, Work Assignment No. 03, Document No. SSS-R-88-9436, October, 1988.

17.0TABLES, DIAGRAMS, FLOW CHARTS, AND VALIDATION DATA

The following pages contain the tables referenced by this method.

患者知情同意书-中国临床试验注册中心

研究标题：单纯调强放疗与调强放疗联合同期化疗治疗II、III期鼻咽癌的非劣效性II期临床试验研究申办方：中山大学附属肿瘤医院 --------------------------------------------------------------------- 研究者姓名：....................... 电话 ................... 地址：.............................................................. ................................................................... ＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿患者姓名：....................... 出生日期：...... 年......月......日＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿＿ 1.简介您的医生已经告知您，目前您所患疾病的最主要治疗方法是放疗。您正受邀参加一项临床研究，其目的是比较单纯调强放疗与调强放疗联合同时期化疗治疗 AJCC分期II、III期鼻咽癌患者的疗效、副反应与生活质量。目前同时期放化疗是目前Ⅱ～Ⅳb期鼻咽癌的标准治疗方案。在这些确定同时期化疗地位的临床研究中，放射治疗技术采用的均为二维的常规放疗技术。在常规放疗技术条件下，同期放化疗确实可以提高局部中晚期的生存，然而同期放化疗的生存获益主要是通过提高局部控制率实现的。10余年来，调强放射治疗技术的物理学优势以及鼻咽癌的临床解剖和生物学特点，使得调强放射治疗在鼻咽癌治疗中得到广泛应用，众多临床实验结果也表明调强放射治疗技术使鼻咽癌的治疗疗效达到一个新的高度，调强放射治疗技术的应用，削弱了同期放化疗+/- 辅组化疗在局部晚期鼻咽癌中的作用。并且同时期化疗加重了鼻咽癌患者近期和远期副反应的发生率，如血液毒性、体重下降及耳毒性等毒副反应。在众多化疗药物中，顺铂是治疗中晚期鼻咽癌的经典一线药物。但是，由于顺铂引起的胃肠道反应较重，例如剧烈的恶心、呕吐等，导致部分患者不能耐受化疗；而顺铂直接损害肾实质，治疗时需要水化和利尿；顺铂的神经毒性和放疗后的远期毒性放射性听神经损伤叠加，严重影响了患者的生活质量。因此，根据现有的调强放射治疗结果和同期化疗的疗效，以及常规放射

美国环保局 EPA 试验方法 3541

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

研究方案10-中国临床试验注册中心

颅内血管磁共振管壁成像注册登记研究方案一、研究背景 1. 研究目的与意义颅内动脉狭窄是缺血性卒中的重要原因。由于缺乏可靠影像学手段及病理学证据，颅内动脉粥样硬化斑块（ICAD）易损性特征一直是研究难点。基于前期高分辨磁共振（HR-MRI）管壁成像研究工作，我们提出：症状性ICAD斑块强化是斑块易损性的重要标志，其强化程度与卒中复发密切相关。我们拟通过建立的颅内动脉狭窄研究队列，采用HR-MRI技术前瞻性比较症状性与无症状ICAD斑块组成、形态结构、强化程度等定量指标，探索①HR-MRI技术在脑卒中病因学诊断，治疗方案决策方面的价值；②建立包含斑块强化特性的ICAD易损斑块评价标准，明确及其在药物治疗效果评估中的价值，为ICAD的个体化治疗提供重要的客观依据。 2. 国内外研究现状颅内动脉粥样硬化性狭窄是引起脑梗死的重要原因颅内动脉粥样硬化性狭窄发生率存在种族差异[1]。亚洲黄种人及非洲、美洲黑人的颅内动脉狭窄的发生率较美洲白人高。基于我国的两项研究发现年龄超过60岁的正常人群中颅内动脉狭窄发生率为5.9%～6.9%[2, 3]。我国卒中患者中颅内动脉狭窄约占33%～50%，TIA患者中颅内动脉狭窄所占比例更高（＞50%）。症状性ICAD年卒中复发率较无症状ICAD年发生率显著增高。脑梗死后患者存在再卒中风险，而伴有颅内动脉狭窄患者的卒中复发率明显增加。我国国家卒中注册调查的数据显示伴有颅内动脉狭窄1年内卒中复发率随动脉狭窄程度而增加，其1年复发率从3.34％增至7.40％[4]。在WASID研究中症状性ICAD者应用阿司匹林组1年内卒中复发率为19%，而狭窄率≥70%的患者年卒中复发率高达23%；无症状颅内动脉粥样硬化性狭窄发生率为18.9%-27.3%，而其相关卒中年发生率平均3.5%。因此，ICAD导致卒中发生的风险存在显著差异，进一步的危险分层研究对于临床干预决策具有重要指导意义。颅内动脉粥样硬化引起卒中的机制复杂，包括：血栓形成、动脉-动脉栓塞、低灌注、穿支动脉闭塞等。其中血栓形成、动脉-动脉栓塞在卒中事件的发生中占有重要地位。而二者多由于局部斑块

主要发达国家环保产业发展概况

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

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

美国环境保护制度

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

ICF - 中国临床试验注册中心

一项评价西达本胺联合联合泼尼松、环磷酰胺、依托泊苷及甲氨蝶呤治疗复发或难治性外周T细胞淋巴瘤的多中心、单臂、开放性II期临床试验知情同意书受试者姓名：受试者姓名缩写：受试者编号：联系电话：联系地址：

受试者须知尊敬的患者：您好！首先感谢您有意参加本项临床试验。在您同意参加本项临床试验之前，请您仔细阅读这份知情同意书，如果您愿意也可以和您的亲人或朋友商量，或向您的医生或研究人员提出任何您需要了解的问题，直至得到满意的答复。参加本临床试验是自愿的，如果您同意参加，请您签署此知情同意书，并且保存该份经您和研究者双方签字的知情同意书副本。本临床试验遵循《药物临床试验质量管理规范》和《赫尔辛基宣言》，并获得国家食品药品监督管理局和医院伦理委员会的批准，这将会保证您的权益在本试验中不受侵犯。签署知情同意书不会改变您的合法权益，仅表示您已经理解了这些信息并愿意参加本试验。【试验目的和背景】针对外周T细胞淋巴瘤（PTCL）目前尚无标准的治疗方案，一线治疗包括CHOP 方案（环磷酰胺、阿霉素、长春新碱和强的松四药联合）或CHOP类似方案，虽然可获得较高缓解率，但维持时间短，患者生存获益差。对于难治患者或缓解后再复发的患者，特别是对于因各种原因不能进行自体干细胞移植患者，二线治疗难度更大，因此治疗指南首选临床试验。西达本胺（Chidamide，爱谱沙）是我国自主研发的亚型选择性组蛋白去乙酰化酶（HDAC）抑制剂，为 1.1类新药。在全国多家中心完成的西达本胺片治疗复发或难治性外周T细胞淋巴瘤的II期临床试验结果显示，西达本胺单药有效率为29.1%，常见不良事件为血液学毒性、胃肠道反应、食欲不振等，超过半数患者发生的不良事件为1-2级。这些结果显示，西达本胺安全性较好，主要不良反应为可控的血液毒性，并显示了较好的综合获益，口服给药方便。2014年12月23日国家食品药品监督管理总局（CFDA）批准西达本胺单药治疗复发或难治性PTCL。本项临床试验的主要目的是在前期相同适应症的单药临床试验基础上，对西达本胺联合泼尼松、环磷酰胺、依托泊苷及甲氨蝶呤治疗复发或难治性PTCL的疗效和安全性进行评价，为西达本胺联合用药的临床应用进一步提供依据。【试验设计和步骤】试验将选择合适的患者参加，计划共计入选36例受试者。在入组筛选期间，为了确定您是否适合参加本项临床试验，您的医生将询问并记录您的病史、全身健康状况以及进行相关的检查。您将被要求抽血（约5~8毫升）以及留取尿标本进行血常规、血生化、电解质和尿常规等检查，同时进行皮肤病灶拍照评估、放射学和其他必要的检查，以便了解您的疾病情况是否符合参加本项临床试验的入选标准。本研究包括联合治疗期和维持治疗期。在联合治疗期，您将接受西达本胺联合泼尼松、环磷酰胺、依托泊苷及甲氨蝶呤的治疗：西达本胺片每次30mg，每周服用2次

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

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 .

那些临床试验需要注册

注册指南请仔细阅读本指南，如有疑问，请与我们联系。一、什么样的临床研究需要注册？所有在人体进行的研究，包括各种干预措施的疗效和安全性的有对照或无对照试验（如随机对照试验、病例-对照研究、队列研究及非对照研究）、预后研究、病因学研究、和包括各种诊断技术、试剂、设备的诊断性试验，均需注册并公告。二、中、英文双语注册在完成中文注册申请表后，必须于两周内完成英文注册申请表。如果两周内不能完成英文版，请与我们联系采用英文翻译服务。在完成中、英文注册资料的上传后15天内可获得注册号，一个月内可在世界卫生组织国际临床试验注册平台检索入口(WHO ICTRP search portal)检索到已注册试验。未完成英文注册申请表者不算完成注册。三、注册是否需要费用？中国临床试验注册中心为非赢利机构，一律免费注册。四、哪些项目需要收费？ 1、只有那些需要我们指导设计的试验才收取一定的服务费用，仅仅用于维持机构运转。参考目前国际注册机构收费标准，任何类型的单个研究设计指导费用均为1500元； 2、翻译服务：500元。五、伦理审查及其费用中国临床试验注册中心组建的中国注册临床试验伦理审查委员会由资深各专业临床医学家、临床试验专家、医疗卫生服务用户代表、WHO患者安全保护联盟中国区代表、律师及药物公司代表组成，宗旨是保障受试者权益，审查临床试验的合理性，评估安全性，凡未经其他伦理委员会审查的临床试验均需在中国临床试验注册中心临床试验伦理委员会接受审查。临床试验伦理审查费用标准为每项2000元。六、申请注册程序 1. 全部注册程序均为在线申报； 2. 首先在中国临床试验注册中心网站上建立申请者账户：点击ChiCTR首页右侧的“用户登陆”区的“注册”； 3. 弹出个人信息注册表，请将你的信息录入此表后点击“注册”，则您的账户就建立起来了；

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

美国环保局 EPA 试验方法 3520c

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

临床研究方案-中国临床试验注册中心

临床研究方案放疗同步替吉奥胶囊治疗鼻咽癌临床研究研究者放射肿瘤科医院海军总医院申办者：海军总医院放射肿瘤科

一：前言鼻咽癌是我国常见恶性肿瘤之一，在头颈部恶性肿瘤中占首位。发病率有明显的地区分布。据估计，世界上80%的鼻咽癌病例发生在我国。治疗首选放射治疗，放疗后年生存率约为34-53%。到目前为止，其标准的治疗方案仍为以铂类药物为基础的联合化疗。由于铂类显著的肾毒性、消化道反应、血液学毒性，以及对生活质量的影响，在临床使用上受到限制。替吉奥为抗代谢药物，有替加氟、吉美嘧啶、奥替拉西钾按1:0.4:1摩尔比组成。吉美嘧啶和奥替拉西钾通过对酶的抑制作用，使替加氟在体内生成５-氟尿嘧啶（５-ＦＵ）的有效浓度持续更长的时间，同时减少５-ＦＵ胃肠道副反应。适用于头颈部肿瘤及晚期胃癌、胰腺癌、结直肠癌、非小细胞肺癌等患者。临床荟萃分析显示，在晚期胃癌、胰腺癌、结直肠癌、非小细胞肺癌中使用替吉奥可以在提高疗效的同时，还能降低患者的不良反应的发生率。替吉奥联合同步放疗既能使肿瘤细胞的增殖周期发生改变，增加放疗的敏感性，同时不增加患者严重的不良反应发生率。现进行放疗联合替吉奥胶囊治疗鼻咽癌的临床研究，以探讨该方案的疗效和不良反应。二：研究目的 ◆主要研究终点：疗效(无进展生存期PFS，总生存期OS) ◆次要研究终点：不良反应（早期，晚期）三：研究设计本研究采用单中心、随机、平行对照试验设计，拟纳入病人50例。研究采用随机分组方法：组别1（25例）为替吉奥胶囊同步放化疗，组别2（25例）为氟尿嘧啶+顺铂（PF方案）同步放化疗，在放疗结束后维持化疗3周期治疗结束时评价疗效。任何时间发现病情进展均可停止治疗。

美国EPA200种潜在致癌物的危害等级

潜在致癌剂的危害等级致癌性是筛选优先污染物的重要依据之一，下表列出了美国EPA公布的200种致癌剂的危害等级。其中的参数含义为： 1、证据的充分程度（Degree of Evidence）化学品对人体的致癌性证据之充分程度可以分为下列几类。（1）证据充分，指致癌剂和人体癌症之间有因果关系。（2）证据有限，指能提供一些可信的致癌性证据，但证据尚有限，还需作进一步补充。（3）证据不充分，可能有3种情况，①能获取的致癌性数据很少；②与证据有关的研究尚不能排除偶然性、误差及混淆等情况；③研究结果无致癌性证据。根据动物实验取得的致癌性证据的充分程度可分4级。 1级，致癌性证据充分。 2级，致癌性证据有限。 3级，致癌性证据不充分。 4级，无致癌性证据。 2、IARC标准分组国际癌症研究所（International Agency for research on cancer，简称IARC）将人类的肿瘤风险分为3组。 1组：列在此组内的化学品属致癌物，流行病学和暴露实验均已肯定，基致癌证据是充分的。 2组：化学品可能对人体有致癌性。其中有的对人体的致癌性证据几乎是“充分的”，另一类的证据不够充分。证据程度较高的为A组，较低的为B 组。例如，2A指对人体的致癌性至少存在着有限证据。当动物证据充分而人体数据不充分时，归入2B。 3组：列在本组中的化学品对人类没有致癌性。

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。

美国环保局 EPA 试验 方法 EPA 3550c