美国环保局 EPA 试验方法 9060aTotal Organic Carbon

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美国环保局 EPA 试验方法 550_1

Analyte Acenaphthene Acenaphthylene Anthracene Benzo(a)anthracene Benzo(a)pyrene Benzo(b)fluoranthene Benzo(g,h,i)perylene Benzo(k)fluoranthene Chrysene Dibenzo(a,h)anthracene Fluoranthene Fluorene Indeno(1,2,3-cd)pyrene Naphthalene Phenanthrene Pyrene 1.2
550.1-1
METHOD 550.1 DETERMINATION OF POLYCYCLIC AROMATIC HYDROCARBONS IN DRINKING WATER BY LIQUID-SOLID EXTRACTION AND HPLC WITH COUPLED ULTRAVIOLET AND FLUORESCENCE DETECTION
Hale Waihona Puke July 1990J.W. Hodgeson W.J. Bashe (Technology Applications Inc.) T.V. Baker (Technology Applications Inc.)
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY OFFICE OF RESEARCH AND DEVELOPMENT U.S. ENVIRONMENTAL PROTECTION AGENCY CINCINNATI, OHIO 45268
2.0
SUMMARY OF METHOD 2.1 Polycyclic aromatic hydrocarbons and internal standards, if used, are extracted from a water sample by passing 1 L of sample through a cartridge containing about 1 g of a solid inorganic matrix coated with a chemically bonded C-18 organic phase (liquid-solid extraction, LSE). The use of disks impregnated 550.1-2

EPA-测试 chap5

FIVE - 1Revision 5February 2007CHAPTER FIVE MISCELLANEOUS TEST METHODSPrior to employing the methods in this chapter, analysts are advised to consult thedisclaimer statement at the front of this manual and the information in Chapter Two for guidance on the allowed flexibility in the choice of apparatus, reagents, and supplies. In addition, unless specified in a regulation, the use of SW-846 methods is not mandatory in response to Federal testing requirements. The information contained in each procedure isprovided by EPA as guidance to be used by the analyst and the regulated community in making judgements necessary to meet the data quality objectives or needs for the intended use of the data.The following methods are found in Chapter Five:Method 5050:Bomb Preparation Method for Solid Waste Method 9000:Determination of Water in Waste Materials by Karl Fischer Titration Method 9001:Determination of Water in Waste Materials by Quantitative Calcium Hydride Reaction Method 9010B:Total and Amenable Cyanide: Distillation Method 9012A:Total and Amenable Cyanide (Automated Colorimetric, with Off-line Distillation)Method 9013:Cyanide Extraction Procedure for Solids and Oils Method 9014:Titrimetric and Manual Spectrophotometric Determinative Methods for Cyanide Method 9020B:Total Organic Halides (TOX)Method 9021:Purgeable Organic Halides (POX)Method 9022:Total Organic Halides (TOX) by Neutron Activation Analysis Method 9023:Extractable Organic Halides (EOX) in Solids Method 9030B:Acid-Soluble and Acid-Insoluble Sulfides: Distillation Method 9031:Extractable Sulfides Method 9034:Titrimetric Procedure for Acid-Soluble and Acid-Insoluble Sulfides Method 9035:Sulfate (Colorimetric, Automated, Chloranilate)Method 9036:Sulfate (Colorimetric, Automated, Methylthymol Blue, AA II)Method 9038:Sulfate (Turbidimetric)Method 9056A:Determination of Inorganic Anions by Ion Chromatography Method 9057:Determination of Chloride from HCl/Cl 2 Emission Sampling Train (Methods 0050 and 0051) by Anion Chromatography Method 9060A:Total Organic Carbon Method 9065:Phenolics (Spectrophotometric, Manual 4-AAP with Distillation)Method 9066:Phenolics (Colorimetric, Automated 4-AAP with Distillation)Method 9067:Phenolics (Spectrophotometric, MBTH with Distillation)Method 9070A:n -Hexane Extractable Material (HEM) for Aqueous SamplesMethod 9071B:n-Hexane Extractable Material (HEM) for Sludge, Sediment,and Solid SamplesMethod 9075:Test Method for Total Chlorine in New and Used PetroleumProducts by X-Ray Fluorescence Spectrometry (XRF) Method 9076:Test Method for Total Chlorine in New and Used PetroleumProducts by Oxidative Combustion and Microcoulometry Method 9077:Test Methods for Total Chlorine in New and Used PetroleumProducts (Field Test Kit Methods)Method A:Fixed End Point Test Kit MethodMethod B:Reverse Titration Quantitative End Point Test KitMethodMethod C:Direct Titration Quantitative End Point Test KitMethodMethod 9131:Total Coliform: Multiple Tube Fermentation Technique Method 9132:Total Coliform: Membrane-Filter TechniqueMethod 9210A:Potentiometric Determination of Nitrate in Aqueous Sampleswith an Ion-Selective ElectrodeMethod 9211:Potentiometric Determination of Bromide in Aqueous Sampleswith Ion-Selective ElectrodeMethod 9212:Potentiometric Determination of Chloride in Aqueous Sampleswith Ion-Selective ElectrodeMethod 9213:Potentiometric Determination of Cyanide in Aqueous Samplesand Distillates with Ion-Selective ElectrodeMethod 9214:Potentiometric Determination of Fluoride in Aqueous Sampleswith Ion-Selective ElectrodeMethod 9215:Potentiometric Determination of Sulfide in Aqueous Samplesand Distillates with Ion-Selective ElectrodeMethod 9216:Potentiometric Determination of Nitrate in Aqueous Sampleswith Ion-Selective ElectrodeMethod 9250:Chloride (Colorimetric, Automated Ferricyanide AAI)Method 9251:Chloride (Colorimetric, Automated Ferricyanide AAII)Method 9253:Chloride (Titrimetric, Silver Nitrate)Method 9320:Radium-228FIVE - 2Revision 5February 2007。

《固体废物挥发性有机物的测定顶空气相色谱法》

附件三:
《固体废物挥发性有机物的测定
顶空气相色谱法》(征求意见稿)
编制说明《固体废物挥发性有机物的测定顶空气相色谱法》标准编制组
二○一○年十月
项目名称:固体废物挥发性有机物的测定顶空气相色谱法
项目统一编号:1083
承担单位: 鞍山市环境监测中心站
编制组主要成员:田靖、孙华、杨洪彪、丁岚、王伟、钟岩、于亮、
3.2 国内相关分析方法研究..7
4 标准制订的基本原则和技术路线..9
4.1 标准制订的基本原则..9
4.2 标准制订的技术路线..9
5 方法研究报告..10
5.1 方法研究报告的目标10
5.2 方法适用范围11
5.3 规范性引用文件..11
5.4 术语和定义.11
5.5 方法原理..11
5.6 试剂和材料.11
9 四氯化碳 22 乙苯 35 1,2,4-三氯苯
10 1,2-二氯乙烷 23 对-二甲苯 36 六氯丁二烯
11 苯 24 间-二甲苯 37 萘
12 三氯乙烯 25 邻-二甲苯
13 1,2-二氯丙烷 26 苯乙烯3 环境危害
挥发性有机物在我们的日常生活中广泛存在,它们的主要释放来源是燃烧的燃料(汽油、
(1)固体废物的概念
《危险废物鉴别标准通则》GB5085.7-2007 中指出,固体废物 (solid waste)是指在
生产、生活和其它活动中产生的丧失原有利用价值或者虽未丧失利用价值但被抛弃或放弃的
固态、半固态和置于容器中的气态的物品、物质以及法律、行政法规规定纳入固体废物管理
的物品物质。
《工业固体废物采样制样技术规范》(HJ/T20-1998)中指出,工业固体废物是指在工

Fusion UV Persulfate TOC Analyzer 说明书

FusionUV/Persulfate TOC AnalyzerThe Fusion Total Organic Carbon (TOC) Analyzer utilizes powerful Ultra Violet (UV) Persulfateoxidation allowing superior carbon liberationfrom even the most challenging matrices. Byimplementing the patented Static PressureConcentration (SPC) technology, the Fusion TOC Analyzer is able to achieve unprecedented low-end sensitivity from a Non-Dispersive Infrared(NDIR) detector.The Fusion TOC Analyzer is designed to offerproductivity for a wide variety of applications. 1Advantages of the Fusion• Auto-calibration for unattended calibration monitoring• Intellidilution for automatically diluting a sample back into calibration range• 21 CFR Part 11 functionality• Turn-key method development• Exportable reports in user-definable formats including metadata • User friendly software• Pre-programmed method features for pharmaceutical, drinking water and waste water• Self-diagnostic capabilities including leak check• Mass flow controller for reduced gas consumption and enhanced flow controlUnparalleled Results The Fusion is designed to determine the carbon content in waterand other solutions. Using safe and proven UV promoted persulfateoxidation of carbonaceous material to carbon dioxide (CO2) followedby NDIR detection of the CO2 product, the Fusion is sensitive from0.2ppbC - 4,000ppmC. Varieties of carbon can be independently determined by selecting a pre-defined instrument method.These include:• Total Carbon (TC)• Inorganic Carbon (IC)• Total Organic Carbon (TOC = TC-IC)• Non-Purgeable Organic Carbon (NPOC or TOC by sparging)To determine TOC by the NPOC method, the Fusion uses a syringe driver and 7-port valve to accurately transfer samples and reagents to the reactor. It then uses carrier gas to transfer the reaction product(CO2) from the sample either to vent or to the NDIR detector in thefollowing sequence:1. Removal and venting of IC and POC by acidification and spargingin the IC sparger.2. Following IC removal, an aliquot of the sparged sample istransferred to the UV reactor and persulfate reagent is addedto oxidize the organic carbon, based on the following chemical reactions:a. Free radical oxidants formedb. Excitation of organicsc. Oxidation of organicsThe oxidation products in Step 2 are swept into the CO2 selectiveNDIR detector.The exit valve from the NDIR is closed to allow the detector to become pressurized. Once the gases in the detector have reached equilibrium, the concentration of the CO2is analyzed. The pressurization of the sample gas stream in the NDIR, Static Pressure Concentration, allows for increased sensitivity and precision. It measures all of the oxidation products in the sample in one reading, compared to flow-through technology. The output signal is proportional to the concentration of CO2in the carrier gas, from the oxidation of the sample.The PC workstation uses the TOC TekLink™ software to control the above sequence of operations, process the detector signal, and report the final concentration of the sample based on linearized, multi-point calibration data.Applications and Industries• Pharmaceutical• EnvironmentalMethodsEPA 415.1- 415.3, 9060A, Standard Method 5310C, ASTM D4779 and D4839, and prENV 13370, Cleaning Validation / USP TOC Method<643> / EP 2.2.44 / JPFeatures and BenefitsA. Autosampler - The Fusion has a standard 40mL vial, 75-position integrated autosampler with arobotic arm and carousel for position selection.B. UV Oxidation Reactor – The UV reactor is composed of a glass vessel and a UV light source. The Fusion introduces the sample and persulfate reagent into the UV reactor. The persulfate reagent, combined with UV light, oxidizes carbon in the sample. Tekmar’s improved UV reactor increases sample conservation and improves radiation interaction with water samples and oxidant.C. Halogen Scrubber - The detector, which measures CO2, can beaffected by halogens. To prevent analytical errors, the halogenscrubber removes chlorine and other halogens from the CO2 beforeit enters the detector.D. Septum Piercing Needle – allows for the use of vial caps with a septa thus eliminating sample exposure time to the atmosphere.E. Syringe and Valve - The syringe driver is a precision measuring Mass Flow Controller (MFC) - The patented MFC regulates either flow or pressure depending on the mode of operation. It allows for higher flows for clean up between samples and allows the user to optimize the sparge flow for each sample. Because of the MFC, the instrument automatically validates the system integrity by recording the pressure each time a sample is run. The MFC also performs pneumatic integrity tests on valves to make sure they are leak tight.Intellidilution – This intelligent feature detects when a sample is out of range and will dilute it back to within the calibration range. Additional FeaturesNote: Fusion with front door removed.Permeation DryerDTekmar TOC TekLink TM software allows the user to enter all analysis parameters and then once activated, will continuously monitor the system ensuring operating limits are not exceeded. TOC TekLink TM is capable of performing useful diagnostics such as leak and benchmark tests for validation. All instrument parameters, method scheduling, and editing can be programmed. TOC TekLink TM provides pre-developed methods, allowing startup with little or no modifications and also contains 21 CFR Part 11 compliance tools.TOC TekLink™Fully Optimized User InterfaceThe sample run screen shown here shows a blue status bar indicating that the current sample has exceeded the defined calibration range and the intellidilution feature has been initiated.Schedule Report Screen- The Schedule Report screen demonstrates flexibility in reporting which allows the user to define what is captured in the report.Diagnostics Screen - This screen demonstrates full control diagnostics, which allows for manipulation of all hardware components.5SpecificationsChemistry:Photochemical Oxidation via UV-Persulfate1Detector:Nondispersive Infrared (NDIR) with Static Pressure Concentration (SPC) - PatentedAnalytical Modes:TOC (NPOC), TC- IC, TC, ICAnalytical:Limit of Detection: 0.2 ppbMaximum Measurable Concentration: 4,000 ppm (sample volume and dilution dependent)Carryover: = 1.0% Cross ContaminationPrecision*: = 1.0% RSD,+/-2 ppb or +/- 0.02 µgC, typical of a mid-range standard(Whichever is greater over seven replicates).* Analytical performance affected by laboratory water, reagent and gas purity, as well as samplecontainer cleanliness, sample matrix, gas regulator cleanliness and precision, and operator skill.Complete Process andAnalysis Time:4-8 minutes typical for TOC analysis; Typically 12-22 minutes for Triplicate TOC Analysis Controller:PC, Interface through Windows® 7 Professional or greater21 CFR Part 11Software Control:TOC Teklink TM Software is a 21 CFR Part 11 tool for your laboratory complianceData Handling:• Pre-defined Industry Standard Methods and Customized User Defined Methods• Priority samples via schedule interrupt• Real-time and Historical graphical display of NDIR detector data• Reports exportable XML, CSV and HTML format• Recalculation of data, outlier deletions, and precision performance criteria controls• Ability to view historical results from multiple schedules on one graphical display Calibration:• Auto-Calibration from Single Stock Standards or User Calibration Standards• Multi-point (Linear or Quadratic) and auto-blanking• Ability to use one calibration curve and blank for entire instruments’ analytical range• Auto-Check Standards from Single Stock Standards or User Calibration Standards- Pass / Fail Criteria- Decision Control upon Failure (Halt, Re-Calibrate, or Continue)Other Features:• Auto-System Suitability with PerformanceMeasurements• Auto-dilution of samples/standards• Validation Support Package Available• Pre-programmed point and click method setup• Programmable flow rate and pressure controland monitoring • Auto-Leak Check• Automatic shutdown/standby• Self-cleaning sample handlingprocess that cleans reactor chambers on every repetition• IntellidilutionOfficial Methods:EPA 415.1- 415.3, 9060A, Standard Method 5310C, ASTM D4779 and D4839, and prENV 13370,Cleaning Validation / USP TOC Method <643> / EP 2.2.44 / JPDimensions:18 inches (45.7 cm) W x 24.5 inches (62.2 cm) D x 32 inches (81.3 cm) HCarrier Gas Supply:99.99% pure nitrogen cylinder or 99.9% pure nitrogen generatorInlet CarrierGas Pressure:65 to 100 psiWindows® is a registered trademark of Microsoft, TekLink™ is a registered trademark of Teledyne Tekmar Company. Covered by one or more of the following patents: 7,651,866; 8,128,874.1UV Lamp contains Mercury, Do Not Put In Trash. Recycle or Dispose as Hazardous Waste.6 To place an order: (800) 874-2004 • (513) 229-7000© 2022 Teledyne Technologies Incorporated4736 Socialville-Foster Rd. • Mason, OH 45040 USAPhone: (513) 229-700090023_6/22。

美国环保局 EPA 试验方法 3520c

METHOD 3520CCONTINUOUS LIQUID-LIQUID EXTRACTION1.0SCOPE AND APPLICATION1.1This 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 METHOD2.1 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).3.0INTERFERENCES3.1Refer 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 MATERIALS4.1Continuous 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 3December 19964.2Drying column - 20 mm ID Pyrex® chromatographic column with Pyrex® glass wool at bottom and a PTFE stopcock.NOTE:Fritted glass discs are difficult to decontaminate after highly contaminated extracts have been passed through. Columns without frits may be purchased.Use a small pad of Pyrex® glass wool to retain the adsorbent. Prewash theglass wool pad with 50 mL of acetone followed by 50 mL of elution solvent priorto packing the column with adsorbent.4.3Kuderna-Danish (K-D) apparatus4.3.1Concentrator tube - 10-mL graduated (Kontes K-570050-1025 or equivalent).A ground glass stopper is used to prevent evaporation of extracts.4.3.2Evaporation flask - 500-mL (Kontes K-570001-500 or equivalent). Attach toconcentrator tube with springs, clamps, or equivalent.4.3.3Snyder column - Three-ball macro (Kontes K-503000-0121 or equivalent).4.3.4Snyder column - Two-ball micro (Kontes K-569001-0219 or equivalent).4.3.5Springs - 1/2 inch (Kontes K-662750 or equivalent).NOTE:The following glassware is recommended for the purpose of solvent recovery during the concentration procedures requiring the use of Kuderna-Danishevaporative concentrators. Incorporation of this apparatus may be requiredby State or local municipality regulations that govern air emissions of volatileorganics. EPA recommends the incorporation of this type of reclamationsystem as a method to implement an emissions reduction program. Solventrecovery is a means to conform with waste minimization and pollutionprevention initiatives.4.4Solvent vapor recovery system (Kontes K-545000-1006 or K-547300-0000, Ace Glass 6614-30, or equivalent).4.5Boiling chips - Solvent-extracted, approximately 10/40 mesh (silicon carbide or equivalent).4.6Water bath - Heated, with concentric ring cover, capable of temperature control (± 5E C). The bath should be used in a hood.4.7Vials - 2-mL, glass with PTFE-lined screw-caps or crimp tops.4.8pH indicator paper - pH range including the desired extraction pH.4.9Heating mantle - Rheostat controlled.4.10Syringe - 5-mL.CD-ROM3520C - 2Revision 3December 1996CD-ROM 3520C - 3Revision 3December 19965.0REAGENTS5.1Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it isintended that all reagents shall conform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where such specifications are available. Other gradesmay be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit itsuse without lessening the accuracy of the determination. Reagents should be stored in glass toprevent the leaching of contaminants from plastic containers.5.2Organic-free reagent water - All references to water in this method refer to organic-freereagent water, as defined in Chapter One.5.3Sodium hydroxide solution (10N), NaOH. Dissolve 40 g NaOH in organic-free reagentwater and dilute to 100 mL. Other concentrations of hydroxide solutions may be used to adjustsample pH, provided that the volume added does not appreciably change (e.g., <1%) the totalsample volume.5.4Sodium sulfate (granular, anhydrous), Na SO . Purify by heating at 400E C for 4 hours24in a shallow tray, or by precleaning the sodium sulfate with methylene chloride. If the sodium sulfateis precleaned with methylene chloride, a method blank must be analyzed, demonstrating that thereis no interference from the sodium sulfate.5.5Sulfuric acid solution (1:1 v/v), H SO . Slowly add 50 mL of H SO (sp. gr. 1.84) to 5024 24mL of organic-free reagent water. Other concentrations of acid solutions may be used to adjustsample pH, provided that the volume added does not appreciably change (e.g., <1%) the totalsample volume.5.6Extraction/exchange solvents - All solvents must be pesticide quality or equivalent.5.6.1Methylene chloride, CH Cl , boiling point 39E C. 225.6.2Hexane, C H , boiling point 68.7E C.6145.6.32-Propanol, CH CH(OH)CH , boiling point 82.3E C. 335.6.4Cyclohexane, C H , boiling point 80.7E C. 6125.6.5Acetonitrile, CH CN, boiling point 81.6E C.36.0SAMPLE COLLECTION, PRESERVATION, AND HANDLINGSee the introductory material to this chapter, Organic Analytes, Sec. 4.1.7.0PROCEDURE7.1Using a 1-liter graduated cylinder, measure 1 liter (nominal) of sample. Alternatively, ifthe entire contents of sample bottle are to be extracted, mark the level of sample on the outside ofthe bottle. If high concentrations are anticipated, a smaller sample volume may be taken and dilutedto 1-L with organic-free reagent water. It is recommended that if high analyte concentrations areanticipated, samples should be collected in smaller sample bottles and the whole sample used.7.2Pipet 1.0 mL of the surrogate spiking solution into each sample in the graduated cylinder (or sample bottle) and mix well. (See Method 3500 and the determinative method to be used for details on the surrogate standard solution and matrix spiking solution).7.2.1For the sample in each batch (see Chapter One) selected for use as a matrixspike sample, add 1.0 mL of the matrix spiking standard.7.2.2If Method 3640, Gel-Permeation Cleanup, is to be employed, add twice thevolume of the surrogate spiking solution and the matrix spiking standard, since half of the extract is not recovered from the GPC apparatus. (Alternatively, use 1.0 mL of the spiking solutions and concentrate the final extract to half the normal volume, e.g., 0.5 mL instead of1.0 mL).7.3Check the pH of the sample with wide-range pH paper and adjust the pH, if necessary, to the pH indicated in Table 1, using 1:1 (v/v) sulfuric acid or 10 N sodium hydroxide. Lower concentrations of acid or base solution may be employed, provided that they do not result in a significant change (<1%) in the volume of sample extracted (see Secs. 5.3 and 5.5).7.4Add 300 - 500 mL of methylene chloride to the distilling flask of the extractor. Add several boiling chips to the flask.7.5Quantitatively transfer the sample from the graduated cylinder (or sample bottle) to the extractor. Use a small volume of methylene chloride to rinse the cylinder (or bottle) and transfer this rinse solvent to the extractor. Add organic-free reagent water to the extractor, if needed, to ensure proper operation and extract for 18-24 hours. If the sample was transferred directly from the sample bottle, refill the bottle to the mark made in Sec. 7.1 with water and then measure the volume of sample that was in the bottle.7.6Allow the extractor to cool, then detach the boiling flask. If extraction at a secondary pH is not required (see Table 1), the extract is dried and concentrated using one of the techniques described in Secs. 7.10 - 7.11.7.7If a pH adjustment and second extraction is required (see Table 1), carefully, while stirring, adjust the pH of the aqueous phase to the second pH indicated in Table 1. If the extracts are to be analyzed separately (see Sec. 7.8), attach a clean distilling flask containing 500 mL of methylene chloride to the continuous extractor. Extract for 18-24 hours, allow to cool, and detach the distilling flask. If the extracts are not to be analyzed separately, then the distilling flask and solvent need not be changed and may be used for the second pH extraction.7.8If performing GC/MS analysis (Method 8270), the acid/neutral and base extracts may be combined prior to concentration. However, in some situations, separate concentration and analysis of the acid/neutral and base extracts may be preferable (e.g., if for regulatory purposes the presence or absence of specific acid/neutral and base compounds at low concentrations must be determined, separate extract analyses may be warranted).7.9Perform concentration (if necessary) using the Kuderna-Danish technique (Secs. 7.10.1 through 7.10.6).7.10K-D technique7.10.1Assemble a Kuderna-Danish (K-D) concentrator (Sec. 4.3) by attaching a 10-mLconcentrator tube to a 500-mL evaporation flask.CD-ROM3520C - 4Revision 3December 19967.10.2Attach the solvent vapor recovery glassware (condenser and collection device)(Sec. 4.4) to the Snyder column of the K-D apparatus following manufacturer's instructions.7.10.3Dry the extract by passing it through a drying column containing about 10 cm ofanhydrous sodium sulfate. Collect the dried extract in a K-D concentrator. Rinse the Erlenmeyer flask, which contained the solvent extract, with 20 - 30 mL of methylene chloride and add it to the column to complete the quantitative transfer.7.10.4Add one or two clean boiling chips to the flask and attach a three-ball Snydercolumn. Prewet the Snyder column by adding about 1 mL of methylene chloride to the top of the column. Place the K-D apparatus on a hot water bath (15 - 20E 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 required, to complete the concentration in 10 -20 minutes. At the proper rate of distillation the balls of the column will actively chatter, butthe 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 minutes.7.10.5If a solvent exchange is required (as indicated in Table 1), momentarily removethe Snyder column, add 50 mL of the exchange solvent, a new boiling chip, and reattach the Snyder column. Alternatively, pour the exchange solvent into the top of the Snyder column while the concentrator remains on the water bath in Sec. 7.10.4. Concentrate the extract, as described in Sec. 7.10.4, raising the temperature of the water bath, if necessary, to maintain proper distillation.7.10.6Remove the Snyder column and rinse the flask and its lower joints into theconcentrator tube with 1 - 2 mL of methylene chloride or exchange solvent. If sulfur crystals are a problem, proceed to Method 3660 for cleanup. The extract may be further concentrated by using the techniques outlined in Sec. 7.11 or adjusted to 10.0 mL with the solvent last used.7.11If further concentration is indicated in Table 1, either the micro-Snyder column technique (7.11.1) or nitrogen blowdown technique (7.11.2) is used to adjust the extract to the final volume required.7.11.1Micro-Snyder column techniqueAdd another one or two clean boiling chips to the concentrator tube and attacha two-ball micro-Snyder column. Prewet the column by adding 0.5 mL of methylenechloride or exchange solvent to the top of the column. Place the K-D apparatus in a hotwater bath so that the concentrator tube is partially immersed in the hot water. Adjustthe vertical position of the apparatus and the water temperature, as required, to completethe concentration in 5 - 10 minutes. At the proper rate of distillation the balls of thecolumn will actively chatter, but the chambers will not flood. When the apparent volumeof liquid reaches 0.5 mL, remove the K-D apparatus from the water bath and allow it todrain and cool for at least 10 minutes. Remove the Snyder column, rinse the flask andits lower joints into the concentrator tube with 0.2 mL of methylene chloride or theexchange solvent, and adjust the final volume as indicated in Table 1, with solvent. CD-ROM3520C - 5Revision 3December 19967.11.2Nitrogen blowdown technique7.11.2.1Place the concentrator tube in a warm bath (35E C) and evaporate thesolvent to the final volume indicated in Table 1, using a gentle stream of clean, drynitrogen (filtered through a column of activated carbon).CAUTION:New plastic tubing must not be used between the carbon trap andthe sample, since it may introduce contaminants.7.11.2.2The internal wall of the tube must be rinsed several times withmethylene chloride or appropriate solvent during the operation. During evaporation, thetube must be positioned to avoid water condensation (i.e., the solvent level should bebelow the level of the water bath). Under normal procedures, the extract must not beallowed to become dry.CAUTION:When the volume of solvent is reduced below 1 mL, semivolatileanalytes may be lost.7.12The extract may now be analyzed for the target analytes using the appropriate determinative technique(s) (see Sec. 4.3 of this chapter). If analysis of the extract will not be performed immediately, stopper the concentrator tube and store refrigerated. If the extract will be stored longer than 2 days it should be transferred to a vial with a PTFE-lined screw-cap or crimp top, and labeled appropriately.8.0QUALITY CONTROL8.1Any reagent blanks, matrix spikes, or replicate samples should be subjected to exactly the same analytical procedures as those used on actual samples.8.2Refer to Chapter One for specific quality control procedures and Method 3500 for extraction and sample-preparation procedures.9.0METHOD PERFORMANCERefer to the determinative methods for performance data.10.0REFERENCESNone.CD-ROM3520C - 6Revision 3December 1996CD-ROM 3520C - 8Revision 3December 1996METHOD 3520CCONTINUOUS LIQUID-LIQUID EXTRACTION。

EPA方法索引

EPA方法索引EPA方法索引和相关标准品EPA 是美国国家环境保护局(U.S Environmental Protection Agency) 的英文缩写。

它的主要任务是保护人类健康和自然环境。

EPA 制定了一系列标准分析方法用于环境监测领域。

主要包括：EPA T01～T14 系列标准分析方法——空气中有毒有机物分析方法EPA IP1～IP10 系列标准分析方法——室内空气污染物的分析测定方法EPA 200 系列标准分析方法———金属的分析方法EPA 500 系列标准分析方法——饮用水中有机物的分析方法EPA 600 系列标准分析方法——城市和工业废水中有机化合物的分析方法SW -846 系列标准分析方法——固体废弃物试验分析评价手册1300 系列是毒性试验方法3000 系列是金属元素的提取方法3500 系列是半(非) 挥发性有机物的提取方法3600 系列是净化、分离方法5000 系列是挥发性有机物的提取方法6000 系列是测定金属的新方法7000 系列是原子吸收法测定金属元素8000 系列是有机物分析方法9000 系列是常规项目分析方法其中，500系列，600系列和8000系列是环境种有机物分析最常用的方法。

EPA 600系列方法是美国为贯彻“净水法”(CW A) 、“全国水体污染物排放消除制度”(NPDES) 和“许可证制度”,严格控制点源排放,保护地表水,使其免受城市和工业废水中有机物的污染而制定的。

EPA 500 系列方法是为执行“安全饮用水法”(SDW A) 和“国家一级饮用水法案”(National Primary Drinking Water Regulations) ,确保饮用水及饮用水源的质量而制订的。

EPA 500 系列是针对比较洁净的水样(饮用水、地下水、地表水) 开发的,有些方法仅用试剂水和饮用水验证过SW-846 系列集中贯彻了“资源保护回收法”和“陆地处置限制法规”的精神,包含了固体废弃物采样和分析试验的全部方法, 是在EPA200 ～EPA 600 系列的基础上发展起来的。

美国环保局 EPA 试验方法 3052

METHOD 3052MICROWAVE ASSISTED ACID DIGESTION OF SILICEOUS ANDORGANICALLY BASED MATRICES1.0 SCOPE AND APPLICATION1.1This method is applicable to the microwave assisted acid digestion of siliceous matrices, and organic matrices and other complex matrices. If a total decomposition analysis (relative to the target analyte list) is required, the following matrices can be digested: ashes, biological tissues, oils, oil contaminated soils, sediments, sludges, and soils. This method is applicable for the following elements:Aluminum Cadmium Iron Molybdenum SodiumAntimony Calcium Lead Nickel StrontiumArsenic Chromium Magnesium Potassium ThalliumBoron Cobalt Manganese Selenium VanadiumBarium Copper Mercury Silver ZincBerylliumOther elements and matrices may be analyzed by this method if performance is demonstrated for the analyte of interest, in the matrices of interest, at the concentration levels of interest (see Sec.8.0).Note: This technique is not appropriate for regulatory applications that require the use of leachate preparations (i.e., Method 3050, Method 3051, Method 1311, Method 1312, Method 1310, Method 1320, Method 1330, Method 3031, Method 3040). This method is appropriate for those applications requiring a total decomposition for research purposes (i.e., geological studies, mass balances, analysis of Standard Reference Materials) or in response to a regulation that requires total sample decomposition.1.2This method is provided as a rapid multi-element, microwave assisted acid digestion prior to analysis protocol so that decisions can be made about the site or material. Digests and alternative procedures produced by the method are suitable for analysis by flame atomic absorption spectrometry (FLAA), cold vapor atomic absorption spectrometry (CVAA), graphite furnace atomic absorption spectrometry (GFAA), inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS) and other analytical elemental analysis techniques where applicable. Due to the rapid advances in microwave technology, consult your manufacturer's recommended instructions for guidance on their microwave digestion system and refer to this manual’s "Disclaimer" when conducting analyses using Method 3052.1.3The goal of this method is total sample decomposition and with judicious choice of acid combinations this is achievable for most matrices (see Sec. 3.2). Selection of reagents which give the highest recoveries for the target analytes is considered the optimum method condition. CD-ROM3052 - 1Revision 0December 1996CD-ROM 3052 - 2Revision 0December 19962.0SUMMARY OF METHOD2.1 A representative sample of up to 0.5 g is digested in 9 mL of concentrated nitric acid and usually 3 mL hydrofluoric acid for 15 minutes using microwave heating with a suitable laboratory microwave system. The method has several additional alternative acid and reagent combinations including hydrochloric acid and hydrogen peroxide. The method has provisions for scaling up the sample size to a maximum of 1.0 g. The sample and acid are placed in suitably inert polymeric microwave vessels. The vessel is sealed and heated in the microwave system. The temperature profile is specified to permit specific reactions and incorporates reaching 180 ± 5 ºC in approximately less than 5.5 minutes and remaining at 180 ± 5 ºC for 9.5 minutes for the completion of specific reactions (Ref. 1, 2, 3, 4). After cooling, the vessel contents may be filtered, centrifuged, or allowed to settle and then decanted, diluted to volume, and analyzed by the appropriate SW-846 method.3.0INTERFERENCES3.1Gaseous digestion reaction products, very reactive, or volatile materials that may create high pressures when heated and may cause venting of the vessels with potential loss of sample and analytes. The complete decomposition of either carbonates, or carbon based samples,may cause enough pressure to vent the vessel if the sample size is greater than 0.25 g. Variations of the method due to very reactive materials are specifically addressed in sections 7.3.4 and 7.3.6.1.3.2Most samples will be totally dissolved by this method with judicious choice of the acid combinations. A few refractory sample matrix compounds, such as TiO 2, alumina, and other oxides may not be totally dissolved and in some cases may sequester target analyte elements.3.3The use of several digestion reagents that are necessary to either completely decompose the matrix or to stabilize specific elements may limit the use of specific analytical instrumentation methods. Hydrochloric acid is known to interfere with some instrumental analysis methods such as flame atomic absorption (FLAA) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The presence of hydrochloric acid may be problematic for graphite furnace atomic absorption (GFAA) and inductively coupled plasma mass spectrometry (ICP-MS).Hydrofluoric acid, which is capable of dissolving silicates, may require the removal of excess hydrofluoric acid or the use of specialized non-glass components during instrumental analysis.Method 3052 enables the analyst to select other decomposition reagents that may also cause problems with instrumental analyses necessitating matrix matching of standards to account for viscosity and chemical differences.4.0APPARATUS AND MATERIALS4.1Microwave apparatus requirements.4.1.1The temperature performance requirements necessitate the microwavedecomposition system sense the temperature to within ± 2.5E C and automatically adjust the microwave field output power within 2 seconds of sensing. Temperature sensors should be accurate to ± 2E C (including the final reaction temperature of 180E C). Temperature feedback control provides the primary control performance mechanism for the method. Due to the flexibility in the reagents used to achieve total analysis, tempertuare feedback control is necessary for reproducible microwave heating.Alternatively, for a specific set of reagent(s) combination(s), quantity, and specific vessel type, a calibration control mechanism can be developed similar to previous microwave methods (see Method 3051). Through calibration of the microwave power, vessel load and heat loss, the reaction temperature profile described in Section 7.3.6 can be reproduced.The calibration settings are specific for the number and type of vessel used and for the microwave system in addition to the variation in reagent combinations. Therefore no specific calibration settings are provided in this method. These settings may be developed by using temperature monitoring equipment for each specific set of equipment and reagent combination. They may only be used if not altered as previously described in other methods such as 3051 and 3015. In this circumstance, the microwave system provides programmable power which can be programmed to within ± 12 W of the required power.Typical systems provide a nominal 600 W to 1200 W of power (Ref. 1, 2, 5). Calibration control provides backward compatibility with older laboratory microwave systems without temperature monitoring or feedback control and with lower cost microwave systems for some repetitive analyses. Older lower pressure vessels may not be compatible.4.1.2The temperature measurement system should be periodically calibrated at anelevated temperature. Pour silicon oil (a high temperature oil into a beaker and adequately stirred to ensure a homogeneous temperature. Place the microwave temperature sensor and a calibrated external temperature measurement sensor into the beaker. Heat the beaker to a constant temperature of 180 ± 5°C. Measure the temperature with both sensors. If the measured temperatures vary by more than 1 - 2°C, the microwave temperature measurement system needs to be calibrated. Consult the microwave manufacturer’s instructions about the specific temperature sensor calibration procedure.CAUTION: The use of microwave equipment with temperature feedback control isrequired to control the unfamiliar reactions of unique or untested reagentcombinations of unknown samples. These tests may require additional vesselrequirements such as increased pressure capabilities.4.1.3The microwave unit cavity is corrosion resistant and well ventilated. Allelectronics are protected against corrosion for safe operation.CAUTION: There are many safety and operational recommendations specific to themodel and manufacturer of the microwave equipment used in individual laboratories.A listing of these specific suggestions is beyond the scope of this method and requirethe analyst to consult the specific equipment manual, manufacturer, and literature forproper and safe operation of the microwave equipment and vessels.4.1.4The method requires essentially microwave transparent and reagent resistantsuitably inert polymeric materials (examples are PFA or TFM suitably inert polymeric polymers) to contain acids and samples. For higher pressure capabilities the vessel may be contained within layers of different microwave transparent materials for strength, durability, and safety. The vessels internal volume should be at least 45 mL, capable of withstanding pressures of at least 30 atm (30 bar or 435 psi), and capable of controlled pressure relief.These specifications are to provide an appropriate, safe, and durable reaction vessel of which there are many adequate designs by many suppliers.CD-ROM3052 - 3Revision 0December 1996CAUTION: The outer layers of vessels are frequently not as acid or reagent resistantas the liner material and must not be chemically degraded or physically damaged toretain the performance and safety required. Routine examination of the vesselmaterials may be required to ensure their safe use.CAUTION: The second safety concern relates to the use of sealed containers withoutpressure relief devices. Temperature is the important variable controlling thereaction. Pressure is needed to attain elevated temperatures, but must be safelycontained. However, many digestion vessels constructed from certain suitably inertpolymerics may crack, burst, or explode in the unit under certain pressures. Onlysuitably inert polymeric (such as PFA or TFM and others) containers with pressurerelief mechanisms or containers with suitably inert polymeric liners and pressurerelief mechanisms are considered acceptable.Users are therefore advised not to use domestic (kitchen) type microwave ovens orto use inappropriate sealed containers without pressure relief for microwave aciddigestions by this method. Use of laboratory-grade microwave equipment is requiredto prevent safety hazards. For further details, consult Reference 3 and 6.4.1.5 A rotating turntable is employed to insure homogeneous distribution ofmicrowave radiation within most systems (Ref. 1). The speed of the turntable should be a minimum of 3 rpm.CAUTION: Laboratories should not use domestic (kitchen) type microwave ovens forthis method. There are several significant safety issues. First, when an acid such asnitric is used to effect sample digestion in microwave units in open vessel(s), orsealed vessels equipment, there is the potential for the acid gas vapor released tocorrode the safety devices that prevent the microwave magnetron from shutting offwhen the door is opened. This can result in operator exposure to microwave energy.Use of a system with isolated and corrosion resistant safety devices prevents thisfrom occurring.4.2Volumetric ware, volumetric flasks, and graduated cylinders, 50 and 100 mL capacity or equivalent.4.3 Filter paper, qualitative or equivalent.4.4 Filter funnel, polypropylene, polyethylene or equivalent.4.5Analytical balance, of appropriate capacity, with a ± 0.0001 g or appropriate precision for the weighing of the sample. Optionally, the vessel with sample and reagents may be weighed, with an appropriate precision balance, before and after microwave processing to evaluate the seal integrity in some vessel types.CD-ROM3052 - 4Revision 0December 1996CD-ROM 3052 - 5Revision 0December 19965.0REAGENTS5.1All reagents should be of appropriate purity or high purity (acids for example, should be sub-boiling distilled where possible) to minimize the blank levels due to elemental contamination.All references to water in the method refer to reagent water (Ref. 7). Other reagent grades may be used, provided it is first ascertained that the reagent is of sufficient purity to permit its use without lessening the accuracy of the determination. If the purity of a reagent is questionable, analyze the reagent to determine the level of impurities. The reagent blank must be less than the MDL in order to be used.6.0SAMPLE COLLECTION, PRESERVATION, AND HANDLING6.1All samples must have been collected using a sampling plan that addresses the considerations discussed in Chapter Nine of this manual.6.2All sample containers must be prewashed with detergents, acids, and water. Plastic and glass containers are both suitable. See Chapter Three, Sec. 3.1.3 of this manual, for further information.6.3Refer to Chapter Three for the appropriate holding times and storage conditions.7.0PROCEDURE7.1Temperature control of closed vessel microwave instruments provides the main feedback control performance mechanism for the method. Control requires a temperature sensor in one or more vessels during the entire decomposition. The microwave decomposition system should sense the temperature to within ± 2.5 C and permit adjustment of the microwave output o power within 2 seconds.7.2 All digestion vessels and volumetric ware must be carefully acid washed and rinsed with reagent water. When switching between high concentration samples and low concentration samples, all digestion vessels (fluoropolymer liners only) should be cleaned by leaching with hot (1:1)hydrochloric acid (greater than 80C, but less than boiling) for a minimum of two hours followed with o hot (1:1) nitric acid (greater than 80C, but less than boiling) for a minimum of two hours and rinsed o with reagent water and dried in a clean environment. This cleaning procedure should also be used whenever the prior use of the digestion vessels is unknown or cross contamination from vessels is suspected. Polymeric or glass volumetric ware (not used with HF) and storage containers should be cleaned by leaching with more dilute acids (approximately 10% V/V) appropriate for the specific plastics used and then rinsed with reagent water and dried in a clean environment. To avoid precipitation of silver, ensure that all HCl has been rinsed from the vessels.7.3Sample Digestion7.3.1Weigh a well-mixed sample to the nearest 0.001 g into an appropriate vesselequipped with a pressure relief mechanism. For soils, ash, sediments, sludges, and siliceous wastes, initially use no more than 0.5 g. For oil or oil contaminated soils, initially use no more than 0.25 g.7.3.2Add 9 ± 0.1 mL concentrated nitric acid and 3 ± 0.1 mL concentratedhydrofluoric acid to the vessel in a fume hood. If the approximate silicon dioxide content of the sample is known, the quantity of hydrofluoric acid may be varied from 0 to 5 mL for stoichiometric reasons. Samples with higher concentrations of silicon dioxide (> 70%) may require higher concentrations of hydrofluoric acid (>3 mL HF). Alternatively samples with lower concentrations of silicon dioxide (< 10% to 0%) may require much less hydrofluoric acid (0.5 mL to 0 mL). Examples are presented in Table 1, 2, 3, and 6. Acid digestion reagent combinations used in the analysis of several matrices, listed in Table 7, provide guidance for the development of new matrix decomposition procedures.7.3.3The addition of other reagents with the original acids prior to digestion maypermit more complete oxidation of organic sample constituents, address specific decomposition chemistry requirements, or address specific elemental stability and solubility problems.The addition of 2 ± 2 mL concentrated hydrochloric acid to the nitric and hydrofluoric acids is appropriate for the stabilization of Ag, Ba, and Sb and high concentrations of Fe and Al in solution. The amount of HCl needed will vary depending on the matrix and the concentration of the analytes. The addition of hydrochloric acid may; however, limit the techniques or increase the difficulties of analysis. Examples are presented in Table 4.The addition of hydrogen peroxide (30%) in small or catalytic quantities (such as 0.1 to 2 mL) may aid in the complete oxidation of organic matter.The addition of water (double deionized) may (0 to 5 mL) improve the solubility of minerals and prevent temperature spikes due to exothermic reactions.NOTE: Supporting documentation for the chemistry of this method has beenprepared in chapters 2 and 3 of reference 3. It provides additional guidance anddocumentation of appropriate reagent, matrix and analyte combinations that can beemployed in this method.CAUTION: Only one acid mixture or quantity may be used in a single batch in themicrowave to insure consistent reaction conditions between all vessels andmonitored conditions. This limitation is due to the current practice of monitoring arepresentative vessel and applying a uniform microwave field to reproduce thesereaction conditions within a group of vessels being simultaneously heated.CAUTION: Toxic nitrogen oxide(s), hydrogen fluoride, and toxic chlorine (from theaddition of hydrochloric acid) fumes are usually produced during digestion.Therefore, all steps involving open or the opening of microwave vessels must beperformed in a properly operating fume ventilation system.CAUTION: The analyst should wear protective gloves and face protection and mustnot at any time permit a solution containing hydrofluoric acid to come in contact withskin or lungs.CD-ROM3052 - 6Revision 0December 1996CAUTION: The addition of hydrochloric acid must be from concentrated hydrochloricacid and not from a premixed combination of acids as a buildup of toxic chlorine andpossibly other gases will result from a premixed acid solution. This will overpressurize the vessel due to the release of these gases from solution upon heating.The gas effect is greatly lessened by following this suggestion.CAUTION: When digesting samples containing volatile or easily oxidized organiccompounds, initially weigh no more than 0.10 g and observe the reaction beforecapping the vessel. If a vigorous reaction occurs, allow the reaction to cease beforecapping the vessel. If no appreciable reaction occurs, a sample weight up to 0.25g can be used.CAUTION: The addition of hydrogen peroxide should only be done when the reactivecomponents of the sample are known. Hydrogen peroxide may react rapidly andviolently on easily oxidizable materials and should not be added if the sample maycontain large quantities of easily oxidizable organic constituents.7.3.4The analyst should be aware of the potential for a vigorous reaction. If avigorous reaction occurs upon the initial addition of reagent or the sample is suspected of containing easily oxidizable materials, allow the sample to predigest in the uncapped digestion vessel. Heat may be added in this step for safety considerations (for example the rapid release of carbon dioxide from carbonates, easily oxidized organic matter, etc.). Once the initial reaction has ceased, the sample may continue through the digestion procedure.7.3.5Seal the vessel according to the manufacturer's directions. Properly placethe vessel in the microwave system according to the manufacturer's recommended specifications and connect appropriate temperature and pressure sensors to vessels according to manufacturer’s specifications.7.3.6This method is a performance based method, designed to achieve orapproach total decomposition of the sample through achieving specific reaction conditions.The temperature of each sample should rise to 180 ± 5 ºC in approximately 5.5 minutes and remain at 180 ± 5 ºC for 9.5 minutes. The temperature-time and pressure-time profile are given for a standard soil sample in Figure 1. The number of samples simultaneously digested is dependent on the analyst. The number may range from 1 to the maximum number of vessels that the microwave units magnetron can heat according to the manufacturer’s or literature specifications (the number will depend on the power of the unit, the quantity and combination of reagents, and the heat loss from the vessels).The pressure should peak between 5 and 15 minutes for most samples (Ref. 2, 3, 5). If the pressure exceeds the pressure limits of the vessel, the pressure will be reduced by the relief mechanism of the vessel.The total decomposition of some components of a matrix may require or the reaction kinetics are dramatically improved with higher reaction temperatures. If microwave digestion systems and/or vessels are capable of achieving higher temperatures and pressures, the minimum digestion time of 9.5 minutes at a temperature of at least 180 ± 5°C is an appropriate CD-ROM3052 - 7Revision 0December 1996alternative. This change will permit the use of pressure systems if the analysis verifies that 180°C is the minimum temperature maintained by these control systems.7.3.6.1For reactive substances, the heating profile may be altered forsafety purposes. The decomposition is primarily controlled by maintaining thereagents at 180 ± 5°C for 9.5 minutes, therefore the time it takes to heat the samplesto 180 ± 5°C is not critical. The samples may be heated at a slower rate to preventpotential uncontrollable exothermic reactions. The time to reach 180 ± 5 ºC may beincreased to 10 minutes provided that 180 ± 5 ºC is subsequently maintained for 9.5minutes. Decomposition profiles are presented in Figures 1 and 2. The extremedifference in pressure is due to the gaseous digestion products.7.3.6.2 Calibration control is applicable in reproducing this methodprovided the power in watts versus time parameters are determined to reproduce thespecifications listed in 7.3.6. The calibration settings will be specific to the quantityand combination of reagents, quantity of vessels, and heat loss characteristics of thevessels (Ref 1). If calibration control is being used, any vessels containing acids foranalytical blank purposes are counted as sample vessels and when fewer than therecommended number of samples are to be digested, the remaining vessels shouldbe filled with the same acid mixture to achieve the full complement of vessels. Thisprovides an energy balance, since the microwave power absorbed is proportional tothe total absorbed mass in the cavity (Ref. 1). Irradiate each group of vessels usingthe predetermined calibration settings. (Different vessel types should not be mixed).7.3.6.3Pressure control for a specific matrix is applicable if instrumentconditions are established using temperature control. Because each matrix will havea different reaction profile, performance using temperature control must bedeveloped for every specific matrix type prior to use of the pressure control system.7.3.7At the end of the microwave program, allow the vessels to cool for a minimumof 5 minutes before removing them from the microwave system. When the vessels have cooled to near room temperature, determine if the microwave vessels have maintained a seal throughout the digestion. Due to the wide variability of vessel designs, a single procedure is not appropriate. For vessels that are sealed as discrete separate entities, the vessel weight may be taken before and after digestion to evaluate seal integrity. If the weight loss of sample exceeds 1% of the weight of the sample and reagents, then the sample is considered compromised. For vessels with burst disks, a careful visual inspection of the disk may identify compromised vessels. For vessels with resealing pressure relief mechanisms, an auditory or sometimes a physical sign indicates a vessel has vented.7.3.8Complete the preparation of the sample by carefully uncapping and ventingeach vessel in a fume hood. Vent the vessels using the procedure recommended by the vessel manufacturer. Transfer the sample to an acid-cleaned bottle. If the digested sample contains particulates which may clog nebulizers or interfere with injection of the sample into the instrument, the sample may be centrifuged, allowed to settle, or filtered.CD-ROM3052 - 8Revision 0December 1996CD-ROM 3052 - 9Revision 0December 19967.3.8.1Centrifugation: Centrifugation at 2,000 - 3,000 rpm for 10minutes is usually sufficient to clear the supernatant.7.3.8.2Settling: If undissolved material remains such as TiO , or2other refractory oxides, allow the sample to stand until the supernatant is clear.Allowing a sample to stand overnight will usually accomplish this. If it does not,centrifuge or filter the sample.7.3.8.3 Filtering: If necessary, the filtering apparatus must bethoroughly cleaned and prerinsed with dilute (approximately 10% V/V) nitric acid.Filter the sample through qualitative filter paper into a second acid-cleanedcontainer.7.3.9If the hydrofluoric acid concentration is a consideration in the analysistechnique such as with ICP methods, boric acid may be added to permit the complexation of fluoride to protect the quartz plasma torch. The amount of acid added may be varied,depending on the equipment and the analysis procedure. If this option is used, alterations in the measurement procedure to adjust for the boric acid and any bias it may cause are necessary. This addition will prevent the measurement of boron as one of the elemental constituents in the sample. Alternatively, a hydrofluoric acid resistant ICP torch may be used and the addition of boric acid would be unnecessary for this analytical configuration. All major manufacturers have hydrofluoric resistant components available for the analysis of solutions containing hydrofluoric acid.CAUTION: The traditional use of concentrated solutions of boric acid can causeproblems by turning the digestion solution cloudy or result in a high salt contentsolution interfering with some analysis techniques. Dilute solutions of boric acid orother methods of neutralization or reagent elimination are appropriate to avoidproblems with HF and the glass sample introduction devices of analyticalinstrumentation. Gentle heating often serves to clear cloudy solutions. Matrixmatching of samples and standards will eliminate viscosity differences.7.3.10The removal or reduction of the quantity of the hydrochloric and hydrofluoricacids prior to analysis may be desirable. The chemistry and volatility of the analytes of interest should be considered and evaluated when using this alternative. Evaporation to near dryness in a controlled environment with controlled pure gas and neutralizing and collection of exhaust interactions is an alternative where appropriate. This manipulation may be performed in the microwave system, if the system is capable of this function, or external to the microwave system in more common apparatus(s). This option must be tested and validated to determine analyte retention and loss and should be accompanied by equipment validation possibly using the standard addition method and standard reference materials.This alternative may be used to alter either the acid concentration and/or acid composition.Note: The final solution typically requires nitric acid to maintain appropriate sample solution acidity and stability of the elements. Commonly, a 2% (v/v) nitric acid concentration is desirable. Examples of analysis performed with and without removal of the hydrofluoric acid are presented in Table 5. Waste minimization techniques should be used to capture reagent。

非甲烷总烃排放标准

非甲烷总烃排放标准非甲烷总烃（Non-Methane Total Hydrocarbons，NMTHC）是指除了甲烷以外的其他烃类物质的总量。

由于非甲烷总烃排放对于环境和人类健康具有潜在的危害，各国都制定了相应的排放标准。

非甲烷总烃可以由多种源头产生，包括工业过程、交通尾气、温室气体排放等。

这些非甲烷总烃物质在大气中进行化学反应，可能形成臭氧和其他有害物质，在一定的浓度下对人类和环境都产生不良影响。

因此，设定非甲烷总烃排放标准是为了限制和减少这些有害物质的释放。

国际上常用的非甲烷总烃排放标准是基于大气中臭氧的形成潜能来确定的。

一般而言，使用臭氧形成潜能（Ozone Formation Potential，OFP）和重活性（Reactivity）两个指标来评估非甲烷总烃的排放对于臭氧形成的贡献。

OFP是指非甲烷总烃与氮氧化物等反应形成臭氧的能力，而重活性则是用来表示非甲烷总烃在大气中的化学活性程度，两者一般情况下是正相关的。

各国的非甲烷总烃排放标准可以根据当地的环境状况、经济发展水平和科技进步情况进行调整和修订。

以下是一些国家关于非甲烷总烃排放标准的具体情况：1.美国：美国环保局（EPA）制定了大气易用计算程序（Atmospheric Release Estimation System）来评估各种工业过程和设备的非甲烷总烃排放。

根据《清洁空气法案》（Clean Air Act）的要求，EPA规定了不同行业和设备的非甲烷总烃排放限值。

2.欧洲：欧洲委员会制定了《大气中挥发性有机物排放限值指令》（Directive on the Limitation of Emissions of VolatileOrganic Compounds into the Air）。

该指令对各类工业设备和过程的非甲烷总烃排放限值进行了详细规定，以保护环境和人类健康。

3.中国：中国生态环境部发布了《VOCs排放标准》（HJ 890-2017），其中包括了非甲烷总烃的排放标准。

美国国家环保局EPA方法要点和推荐仪器

美国国家环保局EPA方法要点和推荐仪器EPA方法218.6离子色谱测定在饮用水、地下水和工业废水中的水溶性铬（1994年修订版3.3）应用范围测定饮用水、地下水和工业废水中的水溶性六价铬（如CrO2-4），这种方法的检测下限为0.4μg/L。

样品中如果含有大量的阴离子物质如硫酸或氯离子可能会引起色谱柱过载。

样品如果含有大量有机物或硫离子可能会引起可溶性的六价铬快速还原为三价铬。

样品贮存在4℃，在24小时内分析。

方法采用离子色谱法分析。

方法要点：水样经0.45μm滤膜过滤后，用浓缓冲溶液调节pH为9-9.5。

样品的测量体积为50-250μL进样到离子色谱。

保护柱去除样品中的有机物，六价铬以CrO2-4形式，在高容量的阴离子交换分离柱上分离，六价铬用双苯基苄巴脲柱后衍生，然后在530nm波长下检测有色络合物。

建议采用的仪器条件保护柱：Dionex IonPac NG1或与之相同的色谱柱分离柱：Dionex IonPac AS7或与之相同的色谱柱阴离子抑制器装置：Dionex Anion MicroMembrane Suppressor，其它抑制器必须有足够低的检测限和足够的基线稳定性。

色谱条件：色谱柱：保护柱-Dionex IonPac NG1, 分离柱-Dionex IonPac AS7淋洗液：250mM (NH4)2SO4, 100mM NH4OH, 流速=1.5 mL/min柱后试剂：2mM双苯基苄巴脲，10％ v/v甲醇，1N 硫酸，流速=0.5 mL/min 检测器：可见光530nm保留时间：3.8 分钟离子色谱测定无机阴离子(1993年八月，修订版2.2)应用范围1．可测定的阴离子包括A部分：溴离子，氯离子，氟离子，硝酸根，亚硝酸根，磷酸根，硫酸B部分：溴酸根，亚氯酸根，氯酸根2．基体包括：饮用水，地表水，民用水和工业废水，地下水，试剂用水，固体浸出液方法要点1．小量样品，一般2-3mL注入离子色谱，阴离子采用一个系统含有保护柱，分离柱，抑制器和电导检测器进行分离和检测。

美国EPA 关于空气自动监测系统性能指标的规定和测试方法

美国EPA关于大气自动监测系统性能指标的规定和测试方法引言环境空气污染的自动监测方法有多种，一般采用湿法和干法两种。

湿法是基于化学量理论的库仑法和电导法等测量原理，需使用大量试剂，存在试剂调整和废液处理等问题，操作比较繁琐，故障率较高，维护工作量较大；干法是基于物理光谱测量理论，使样品始终保持在气体状态，没有试剂的损耗，维护工作量较小。

比如SO2测量采用紫外荧光法，NOx测量采用化学发光法，O3测量采用紫外光度法，CO测量采用气体过滤相关分析法等，目前我国绝大部分空气自动监测采用的是该方法。

干法测量以欧美为主。

美国开展空气自动监测已有30年的历史，在空气自动监测方面积累了丰富的经验，并制定了详细的规范。

其中物理光谱法作为美国EPA的推荐方法,得到了广泛的应用。

湿法测量以日本为主,但自1996年起日本在法定的测量方法中增加了干式测量法。

利用物质的光谱特性进行污染物的分析已成为自动监测仪器发展的必然趋势。

我国在环境空气质量监测和质量保证方面的规定都参考了美国国家环保署（EPA）的规定。

目前，大气自动监测和空气质量日报工作在我国大部分省市已广泛开展，自动监测仪器监测数据的准确可靠是日报工作中的基础。

为使监测人员了解美国EPA关于空气自动监测的相关规定，特将其有关SO2、NO2、O3、CO自动监测仪器的性能指标规定和测试方法作简要说明，以供参考。

一、美国EPA对性能指标及判定原则的规定1、性能指标B-1自动监测仪器性能指标M/0.02447,M是该气体的摩尔质量。

2、判定原则对于每个性能指标（量程除外），测试程序从开始起要重复7次，得到7组测试结果。

每组结果要和表B-1中的规定指标相比较，高于或超出规定指标的值是一个超标值。

每个参数的7个结果说明如下：（1）0次超标：被测的参数合格；（2）3次或更多次超标：该参数不合格；（3）1次或2次超标：再重复测试该参数 8次，得到共15个测试结果。

将此15个测试结果说明如下：a：1次或2次超标：通过测试；b：3次以上：该参数不合格。

EPA测试方法-目录

目录---------------------------第一卷A 部分---------------------------免责声明摘要目录方法索引和换算表前言鸣谢第一部分分析测定方法第一章—质量控制1.0 引言2.0 质量保证计划3.0 室外操作4.0 实验室操作5.0 定义6.0 参考文献第二章—选择正确的步骤2.1 目的2.2 需要的信息2.3 使用指南2.4 特性2.5 地表水2.6 参考文献第三章—无机物分析3.1 采样注意事项3.2 样品准备方法方法3005A 用于火焰原子吸收光谱(FLAA)或电感偶合等离子发射光谱（ICP）进行总可回收或可溶性金属离子检测水样的酸性消化方法。

方法3010A 用于火焰原子吸收光谱(FLAA)或电感偶合等离子体原子发射光谱（ICP）进行全金属分析的水溶液或萃取物的酸性消化方法。

方法3015 水溶液或萃取物的微波辅助酸性消化方法。

方法3020A 用于无火焰原子吸收光谱法（GFAA）进行全金属分析的水溶液或萃取物的酸性消化方法。

方法3031 用于原子吸收光谱（AAS）或电感偶合等离子体原子发射光谱（ICP进行油脂中金属分析的油样的酸性消化方法。

方法3040A 油、脂和石蜡的溶解方法。

方法3050B 沉积物、污泥和土壤的酸性消化方法。

方法3051 沉积物、污泥和土壤的微波辅助酸性消化方法。

方法3052 硅酸盐和有机物质的微波酸性消化方法。

方法3060A 六价铬的碱性消化。

3.3 无机物的测定方法6010B 电感耦合等离子发射光谱（ICP-AES）方法6020 电感耦合等离子体质谱（ICP-MASS）方法7000A 原子吸收法方法7020 铝（原子吸收，直接进样）方法7040 锑（原子吸收，直接进样）方法7041 锑（原子吸收，石墨炉法）方法7060A 砷（原子吸收，石墨炉法）方法7061A 砷（原子吸收，氢火焰法）方法7062 锑和砷（原子吸收，氢硼化钠还原法）方法7063 砷水溶液和萃取物的阳极溶出伏安法（ASV）方法7080A 钡（原子吸收，直接进样）方法7081 钡（原子吸收，石墨炉法）方法7090 铍（原子吸收，直接进样）方法7091 铍（原子吸收，石墨炉法）方法7130 镉（原子吸收，直接进样）方法7131A 镉（原子吸收，石墨炉法）方法7140 钙（原子吸收，直接进样）方法7190 铬（原子吸收，直接进样）方法7191 铬（原子吸收，石墨炉法）方法7195 铬，六价（共沉淀法）方法7196A 铬，六价（比色法）方法7197 铬，六价（螯合/萃取）方法7198 铬，六价（微分脉冲极谱法DPP）方法7199 饮用水、地表水和工业排放废水中六价铬的测定-离子色谱法方法7200 钴（原子吸收，直接进样）方法7201 钴（原子吸收，石墨炉法）方法7210 铜（原子吸收，直接进样）方法7211 铜（原子吸收，石墨炉法）方法7380 铁（原子吸收，直接进样）方法7381 铁（原子吸收，石墨炉法）方法7420 铅（原子吸收，直接进样）方法7421 铅（原子吸收，石墨炉法）方法7430 锂（原子吸收，直接进样）方法7450 镁（原子吸收，直接进样）方法7460 锰（原子吸收，直接进样）方法7461 锰（原子吸收，石墨炉法）方法7470A 废液中的汞（冷蒸汽原子吸收光谱法）方法7471A 固体或半固体废弃物中的汞（冷蒸汽原子吸收光谱法）方法7472 阳极溶出伏安法测定水溶液和萃取物中的汞方法7480 钼（原子吸收，直接进样）方法7481 钼（原子吸收，石墨炉法）方法7520 镍（原子吸收，直接进样）方法7521 镍（原子吸收，石墨炉法）方法7550 锇（原子吸收，直接进样）方法7580 白磷（P4）的溶剂萃取-气相色谱法（GC）方法7610 钾（原子吸收，直接进样）方法7740 硒（原子吸收，石墨炉法）方法7741A 硒（原子吸收，氢火焰法）方法7742 硒（原子吸收，氢硼化钠还原法）方法7760A 硅（原子吸收，直接进样）方法7761 硅（原子吸收，石墨炉法）方法7770 钠（原子吸收，直接进样）方法7780 锶（原子吸收，直接进样）方法7840 铊（原子吸收，直接进样）方法7841 铊（原子吸收，石墨炉法）方法7870 锡（原子吸收，直接进样）方法7910 钒（原子吸收，直接进样）方法7911 钒（原子吸收，石墨炉法）方法7950 锌（原子吸收，直接进样）方法7951 锌（原子吸收，石墨炉法）附件—公司推荐---------------------------第一卷B 部分---------------------------免责声明摘要目录方法索引和换算表前言鸣谢第一章—质量控制1.0 引言2.0 质量保证计划3.0 室外操作4.0 实验室操作5.0 定义6.0 参考文献第四章—有机物分析4.1 采样注意事项4.2 样品准备方法4.2.1 萃取和准备方法3500B 有机物的萃取和样品准备方法3510C 分液漏斗液--液萃取方法3520C 连续液--液萃取方法3535 固相萃取（SPE）方法3540C 索氏萃取方法3541 自动索氏萃取方法3542 使用方法0010（改进后的采样教程方法5）萃取半挥发性有机物方法3545 加压液体萃取（PFE）方法3550B 超声波萃取方法3560 超临界流体萃取总可回收石油烃方法3561 超临界流体萃取多环芳烃方法3580A 固废分解方法3585 挥发性有机物固废样品的分解方法5000 挥发性有机物样品准备方法5021 用顶空法准备土壤中或其他固体物质中的挥发性有机物方法5030B 水溶液样品的吹扫捕集方法5031 共沸蒸馏法提取挥发性、不可吹出、水溶性有机化合物方法5032 挥发性有机物的真空蒸馏方法5035 封闭体系的吹扫捕集和萃取提取土壤和固废样品中的挥发性有机物方法5041A 挥发性有机物采样系统(VOST)吸附柱解吸物的分析4.2.2 净化方法3600C 净化方法3610B 铝氧土净化方法3611B 铝氧土柱的净化以及石油类废物的分离方法3620B Florisil柱的净化方法3630C 硅胶净化方法3640A 凝胶色谱柱净化方法3650B 酸性层析柱的净化方法3660B 硫的净化方法3665A 硫酸/高锰酸钾净化4.3 有机物的测定4.3.1 气相色谱法方法8000B 分析性的色谱分离方法8011 微萃取-气相色谱分析1，2-二溴乙烷和1，2-二溴-3-氯丙烷方法8015B 气相色谱-氢火焰离子检测器（GC-FID）测定非卤代有机物方法8021B 气相色谱法分析芳香族化合物和卤代挥发性有机物—使用光电离检测器（PID）和/或电导检测器（ELCD）方法8031 气相色谱分析丙烯腈方法8032A 气相色谱分析丙烯酰胺方法8033 气相色-氮磷检测器（GC-NPD）分析乙腈方法8041 气相色谱分析酚类方法8061A 气相色谱-电子捕获检测器（GC-ECD）分析邻苯二甲酸酯类方法8070A 气相色谱分析亚硝胺方法8081A 气相色谱分析有机氯杀虫剂方法8082 气相色谱分析多氯联苯方法8091 气相色谱分析硝基芳香烃和环酮方法8100 多核（多环）芳烃方法8111 气相色谱分析卤代醚类方法8121 气相色谱检测氯代烃：毛细管法方法8131 气相色谱法检测苯胺及其衍生物方法8141A 气相色谱分析有机磷化合物：毛细管法方法8151A 甲基化和氟代醇苯甲基化气相色谱法检测氯代除草剂4.3.2 气质联用法（GC-MASS）方法8260B 气质联用法测定挥发性有机物（VOCs）方法8270C 气质联用法测定半挥发性有机物方法8275A 热提取-气质联用法（TE/GC/MS）测定土壤、污泥和固废中的半挥发性有机物（多环芳烃PAHs和多氯联苯PCBs）方法8280A 高分辨率色谱/低分辨率质谱（HRGC/LRMS）法测定多氯二苯并对二英和多氯二苯并呋喃方法8290 高分辨率色谱/高分辨率质谱（HRGC/HRMS）法测定多氯二苯并二恶英（PCDDs）和多氯二苯并呋喃（PCDFs）附件A：实验室进行的擦拭实验的采集、处理、分析和报告步骤4.3.3 高效液相色谱法（HPLC）方法8310 多环芳烃方法8315A 高效液相色谱法测定碳酰（羰基）化合物附录A：2,4-二硝基苯肼的重结晶方法8316 丙烯酰胺、丙烯腈和丙烯醛的测定—高效液相色谱法方法8318 高效液相色谱分析N-氨基甲酸甲酯方法8321A 高效液相色谱/热喷雾/质谱法（HPLC/TS/MS）测定非挥发性有机物的可溶性提取物方法8325 高效液相色谱/粒子束/质谱法（HPLC/PB/MS）测定非挥发性有机物的可溶性提取物方法8330 硝基芳烃和硝胺的测定—高效液相色谱法方法8331 反相高效液相色谱法测定四氮烯方法8332 硝化甘油的测定—高效液相色谱法4.3.4 红外法方法8410 半挥发性有机物的测定—气相色谱/傅立叶变换红外光谱法（GC/FT-IR）：毛细管柱方法8430 水溶液直接进样气相色谱/傅立叶变换红外光谱法（GC/FT-IR）分析双氯甲醚及其水解产物方法8440 红外光谱法分析总可回收石油烃4.3.5 多光谱分析法方法8520 环境空气中甲醛的连续免疫测定4.4 免疫测定法方法4000 免疫测定方法4010A 用免疫测定法进行五氯苯酚的筛检方法4015 用免疫测定法进行2，4-二氯苯氧基乙酸的筛检方法4020 用免疫测定法进行多氯联苯的筛检方法4030 用免疫测定法对土壤中石油烃进行筛检方法4035 用免疫测定法对土壤中多环芳烃进行筛检方法4040 用免疫测定法对土壤中毒杀芬进行筛检方法4041 用免疫测定法对土壤中氯丹进行筛检方法4042 用免疫测定法对土壤中DDT进行筛检方法4050 用免疫测定法对土壤中TNT爆炸性物质进行筛检方法4051 用免疫测定法对土壤中黑索今(环三亚甲基三硝胺RDX)进行筛检4.5 多种筛选法方法3810 顶空法方法3820 可清除有机物的十六烷提取和筛检法方法8515 土壤中TNT物质的比色筛检法方法9078 土壤中多氯联苯的筛选法方法9079 变压器油中多氯联苯的筛选法附件—公司推荐---------------------------第一卷C 部分---------------------------免责声明摘要目录方法索引和换算表前言鸣谢第一章—质量控制1.0 引言2.0 质量保证计划3.0 室外操作4.0 实验室操作5.0 定义6.0 参考文献第五章—其它各种测试方法方法5050 固废爆炸的预防方法方法9010C 总可测定氰化物：蒸馏法方法9012B 总可测定氰化物（手动蒸馏，自动比色）方法9013 固废和土壤中氰化物的萃取方法方法9014 滴定和手动分光光度法测定氰化物方法9020B 总有机卤素（TOX）方法9021 挥发性有机卤素（POX）方法9022 中子活法分析法测定总有机卤素（TOX）方法9023 土壤中的可萃取有机卤素（EOX）方法9030B 酸溶性和非酸溶性硫化物：蒸馏法方法9031 可萃取硫化物方法9034 滴定法测定酸溶性和非酸溶性硫化物方法9035 硫酸盐（比色法，自动，氯冉酸盐）方法9036 硫酸盐（比色法，自动，甲基百里酚兰，）方法9038 硫酸盐（浊度计）方法9056 离子色谱法测定无机阴离子方法9057 阴离子色谱法测定HCl/Cl2排放源采集样品中的氯化物方法9060A 总有机碳（TOC）方法9065 酚醛塑料（分光光度法，手动4-氨基安替比林蒸馏）方法9066 酚醛塑料（比色法，自动4-氨基安替比林蒸馏）方法9067 酚醛塑料（分光光度法，酚试剂蒸馏）方法9070A 用于水溶液样品的正己烷可提取物方法9071B 用于污泥、沉积物、土壤样品的正己烷可提取物方法9075 X射线荧光光谱法分析新的或使用过的石油产品中的总氯方法9076 燃烧氧化和微库仑法分析新的或使用过的石油产品中的总氯方法9077 新的或使用过的石油产品中的总氯（现场测试套件）方法A：固定终点套件法方法B：反向滴定终点定量套件法方法C：直接滴定终点定量套件法方法9131 大肠杆菌：多管发酵法方法9132 大肠杆菌：膜过滤法方法9210 离子选择电极点位滴定法测定水溶液样品中的硝酸盐方法9211 离子选择电极点位滴定法测定水溶液样品中的溴化物方法9212 离子选择电极点位滴定法测定水溶液样品中的氯化物方法9213 蒸馏后离子选择电极点位滴定法测定水溶液样品中的氰化物方法9214 离子选择电极点位滴定法测定水溶液样品中的氟化物方法9215 蒸馏后离子选择电极点位滴定法测定水溶液样品中的硫化物方法9250 氯化物（比色法，自动铁氰化物，AAI）方法9251 氯化物（比色法，自动铁氰化物，AAII）方法9253 氯化物（滴定法，硝酸银）方法9320 镭-288第六章—性质分析方法1030 固体的可燃性方法1120 皮肤腐蚀性方法1312 人工凝结浸出方法方法1320 多次萃取法方法1330A 含油废弃物的提取方法9041A pH试纸制作方法方法9045D 土壤和废弃物pH方法9050A 电导率方法9080 土壤的阳离子交换性能（醋酸铵）方法9081 土壤的阳离子交换性能（醋酸钠）方法9090A 废弃物和膜沉淀的兼容性试验方法9095B 滤芯液体试验方法9096 液体泄露试验方法附件A：液体泄露试验预试验方法9100 饱和水溶液电导，饱和滤出液电导以及固有磁导率方法9310 总α、总β放射性水平方法9315 α放射性同位素第二部分性状第七章—性状说明和定义7.1 可燃性7.2 腐蚀性7.3 反应性7.4 毒性物质提取步骤第八章—性状测定方法8.1 可燃性方法1010A 潘-马氏闭杯分析仪测定闪点方法1020B 闪点的标准测定方法Setaflash闭杯分析仪法8.2 腐蚀性方法9040C pH电极测量方法1110A 钢铁腐蚀性测验8.3 毒性方法1310B 提取过程毒性测试方法和结构完整性试验方法1311 毒性物质提取步骤附件—公司推荐---------------------------第二卷---------------------------免责声明摘要目录方法索引和换算表前言鸣谢第一章—质量控制1.0 引言2.0 质量保证计划3.0 室外操作4.0 实验室操作5.0 定义6.0 参考文献第三部分采样第九章—采样计划9.1 规划和设计9.2 执行第十章—采样方法方法0010 改进后的Method 5 Sampling Train附件A：XAD-2吸附树脂的准备附件B：所有可用色谱分析物质的分析方法0011 固定醛酮类排放源的采样方法方法0020 源头评价采样方法方法0023A 固定多氯联苯并二恶英和多氯联苯并呋喃源的采样方法方法0030 挥发性有机物采样教程方法0031 挥发性有机化合物采样方法方法0040 塑料袋燃烧源头主要持久性危险有机物的采样方法方法0050 HCl/Cl2排放源的等动力采样教程方法0051 HCl/Cl2排放源的小型冲击吸收瓶采样教程方法0060 烟囱排放源的金属测定方法0061 固定排放源六价铬的测定方法0100 室内甲醛和其它羰基化合物的采样第四部分监测第十一章—地表水监测11.1 背景和目标11.2 与标准的关系和与其他文件的关系11.3 修订本和附录11.4 可以接受的设计和措施11.5 不可接受的设计和措施第十二章—土地处理（有害废物的）监测12.1 背景12.2 处理区域12.3 定义12.4 监测和采样策略12.5 分析12.6 参考文献和内容提要第十三章—灰化13.1 说明13.2 定义13.3 废物定性策略13.4 烟囱气体排放物定性策略13.5 附加排放物定性策略13.6 采样和分析方法的选择13.7 参考文献附件—公司推荐。

美国EPA农药登记残留试验样品储藏稳定性资料要求概述

美国EPA农药登记残留试验样品储藏稳定性资料要求概述
美国EPA农药登记残留试验样品储藏稳定性资料要求概述张宏军;李富根;姜文议
【期刊名称】《农药科学与管理》
【年(卷),期】2016(037)003
【摘要】本文概述了美国环保局关于农药登记残留储藏稳定性试验的有关要求,包括基本要求、残留储藏稳定性试验要求、试验结果的使用、试验报告的编写等.希望对我国制定相关技术规范有所借鉴.
【总页数】8页(16-23)
【关键词】农药;登记;残留;储藏稳定性;IR-4
【作者】张宏军;李富根;姜文议
【作者单位】农业部农药检定所,北京100125;农业部农药检定所,北京100125;美国密歇根州立大学昆虫学系,美国密歇根48824 【正文语种】中文
【中图分类】S482
【相关文献】
1.美国EPA农药登记残留试验样品储藏稳定性资料要求概述 [J],
2.美国EPA农药登记残留试验中样品储藏稳定性试验[J], 朱光艳; 张志勇
3.农药登记资料的审批程序、资料要求及注意事项 [C], 吴志凤
4.从农药登记资料新要求看农药发展趋势 [J], 沈迎春
5.美国修订对四种农药的残留限量要求 [J],
以上内容为文献基本信息，获取文献全文请下载。

美国EPA最新参考方法标准

特别规定的样品采集过滤器。
手动参考方法：配备 RAAS-10 PM10 进气口或
RFPS-0699-131 40 联邦法规（CFR）第 50 部分，
附录 L, 图 L-2 到 L-19 中特定的
联邦公告：卷 64，有通气孔的进口，作为 PM10
第 33481 页，参考方法配置，流量为 16.67 升
图 L-2 参考方法
第 33481 页，配置，流量为 16.67 升/分钟，24
BGI 公司 BGI 公司 DKK-TOA 公司 Ecotech 公司
PQ100 型空气采样器
PQ200 型空气采样器
FPM-222/222C,FPM223 /223C 及 DUB-222(S)型 PM10 监测器 3000 型 PM10 大容量空气采样器
或
12/01/87 及卷 53， GMW-IP-10-8000 中的任一型号
第 1062 页，大容量采样器，这些采样器含有
01/15/88
以下部件：带有丙烯腈-丁二烯-
苯乙烯塑胶过滤器托架和电机/
鼓风机外壳或不锈钢过滤器托
架和酚醛塑料电机/鼓风机外壳
的阳极氧化处理铝制大容量外
壳；0.6 大功率电机/鼓风机; 压
06/23/99
小时连续采样周期操作。符合
RAAS105-300 操作说明书，遵
循 40 CFR 第 50 部分，附录 J
或附录 M 中有关要求和特别规
定的样品采集过滤器。
手动参考方法：配备 BGI16.7 进气口装置或附
RFPS-0699-132 录 L，40 联邦法规（CFR）50，
图 L-2 到 L-19 中特定的有通气
7.0 说明书，适当的还带有特制

EPA方法索引范文

EPA方法索引范文EPA方法索引是指美国环境保护署（Environmental Protection Agency）使用的一种方法或指南的集合。

这些方法和指南被广泛应用于环境监测、控制和评估等领域，以确保环境和公共健康的保护。

以下是一些常见的EPA方法索引。

1.环境监测方法-EPA方法200.7：用于痕量金属分析的集中器分析方法。

-EPA方法353.2：用于水中氨氮的连续流动分析方法。

-EPA方法8010：挥发性有机化合物（VOCs）在土壤、固体废物和水样中的分析方法。

2.大气排放测量方法-EPA方法1：测量排放源气流量的方法。

-EPA方法3：使用热式测速计测量气流速度的方法。

-EPA方法25A：测量总有机气态污染物（TO-9A）的方法。

3.水质监测方法-EPA方法200.8：通过电感耦合等离子体发射光谱法（ICP-OES）测量地下水和饮用水中痕量金属的方法。

-EPA方法160.2：测量水和废水中总悬浮颗粒物（TSS）的方法。

-EPA方法300.0：用于汞浓度分析的氢化物发生-冷蒸汽原子吸收光谱法的方法。

4.土壤和固体废物分析方法-EPA方法3050B：提取土壤和固体废物中的金属的方法。

-EPA方法3540C：挥发性有机物在土壤、底泥和固体样品中的提取方法。

-EPA方法8260B：环境样品中挥发性有机物（VOCs）的气相色谱/质谱（GC/MS）分析法。

5.生物监测方法-EPA方法1605：用于大肠杆菌和菌落总数的微生物分析方法。

-EPA方法821-R-02-012：基于鱼类激素和特征蛋白的鱼类暴露评估方法。

-EPA方法821-R-02-013：用于粪臭强度测量的无尘试纸法。

需要注意的是，这只是EPA方法索引中的一小部分，并且每个方法都有详细的操作规程和分析步骤。

研究人员和环境监测单位可以根据需要，选择合适的方法来进行各种环境样品的分析和监测工作，以确保结果的准确性和可比性。

EPA方法索引

EPA方法索引EPA（Environmental Protection Agency，环境保护局）是美国联邦政府机构，负责制定环境保护政策和监督执行，旨在保护人类健康和自然环境。

EPA通过开发和更新一系列的方法和准则来评估和监测环境中的各种污染物。

以下是EPA方法的索引，其中包含了一些常用的方法。

1.水质分析方法：-EPA方法6010：使用电感耦合等离子体质谱仪对水样中的重金属进行测定。

-EPA方法160.2：测定饮用水中总溶解性氟化物的浓度。

-EPA方法200.7：使用火焰原子吸收光谱法测定水样中的金属。

-EPA方法365.2：测定地下水中40种有机化合物的浓度。

2.大气质量监测方法：-EPA方法305：测定大气中颗粒物（PM10）的质量浓度。

-EPA方法1664：对水和底泥中的油脂进行提取和测定。

-EPA方法321.8：通过气浓度梯度法测定大气中的苯系化合物。

-EPA方法327：使用红外光谱法测定大气中的多环芳烃。

3.土壤和底泥分析方法：-EPA方法3540：对土壤和底泥中的有机物进行提取。

-EPA方法8000：使用气相色谱质谱法分析土壤和底泥中的挥发性有机化合物。

-EPA方法3051：测定土壤样品中重金属的浓度。

-EPA方法8240：使用气相色谱质谱法分析土壤和底泥中的半挥发性有机化合物。

4.垃圾和固体废物分析方法：-EPA方法8015：使用气相色谱质谱法分析固体废物中的多环芳烃。

-EPA方法8082：使用气相色谱质谱法分析土壤、底泥和固体废物中的戴奥辛和类似化合物。

-EPA方法8260：使用气相色谱质谱法分析固体废物中的挥发性有机化合物。

-EPA方法8280：使用气相色谱质谱法分析固体废物中的多氯联苯。

5.生物监测方法：-EPA方法1600：测定饮用水和海水中的大肠杆菌和肠球菌数量。

-EPA方法1613：使用液相色谱质谱法测定鱼类组织中的多氯联苯和多溴联苯醚。

-EPA方法2050：测定水和生物体中蓝绿藻的数量和类群组成。

epa试验测试方法及计算方法

epa试验测试方法及计算方法English Answer:EPA Test Methods for Emissions.The Environmental Protection Agency (EPA) has developed a series of test methods to measure emissions from various sources, including stationary sources such as power plants and industrial facilities, and mobile sources such as vehicles and aircraft. These test methods are used to determine the levels of pollutants emitted into the atmosphere and to assess the effectiveness of pollution control technologies.Some of the most common EPA test methods include:Method 1: Sample and velocity traverses for stationary sources. This method describes the procedures for measuring the velocity and volumetric flow rate of gas streams in ducts, stacks, and chimneys.Method 2: Determination of stack gas velocity and volumetric flow rate (Type S pitot tube). This method is used to measure the velocity and volumetric flow rate of gas streams in stacks and ducts using a Type S pitot tube.Method 3: Gas analysis for the determination of dry molecular weight. This method is used to determine the dry molecular weight of a gas stream by measuring its density and composition.Method 4: Determination of moisture content in stack gases. This method is used to determine the moisture content of a gas stream by measuring the dew point or absolute humidity of the gas.Method 5: Determination of particulate matter emissions from stationary sources. This method is used to measure the concentration of particulate matter emissions from stationary sources by collecting the particles on a filter paper and measuring their mass.Method 10: Determination of carbon monoxide emissions from stationary sources. This method is used to measure the concentration of carbon monoxide emissions from stationary sources by using a continuous analyzer or a grab sample collection and analysis.Method 18: Measurement of gaseous organic compound emissions by gas chromatography. This method is used to measure the concentration of gaseous organic compound emissions from stationary sources by collecting a sample in a sorbent tube and analyzing it using gas chromatography.Calculation Methods.The EPA provides calculation methods for each test method to determine the concentration of pollutants emitted. The calculation methods typically involve using the measured data from the test method to calculate the mass or volume of the pollutant emitted per unit of time.For example, the calculation method for Method 5involves using the following equation to calculate theparticulate matter emission rate:ER = (C_s Q_sd) / (S t)。

EPA方法索引

EPA方法索引根据您的要求，以下是EPA（美国环保局）使用的一些常见的方法索引。

这些方法涵盖了环境监测、风险评估、废物管理、空气质量评估和水质评估等各个领域。

请注意，这只是一个简要的索引，详细的方法描述和操作程序可以在EPA的官方网站上找到。

1.环境监测方法：-EPA方法1：样品获取和保留方法-EPA方法2：采样口和尾气采集系统评估方法-EPA方法3：抽样方法-EPA方法4：大气沉降物的抽样和分析方法-EPA方法5：大气礁石沉积物中颗粒物的采样和分析方法-EPA方法6：大气颗粒物的测定方法-EPA方法7：废气流中氮氧化物的测定方法-EPA方法8：高温、高湿废气流中苯/甲苯浓度的测定方法2.风险评估方法：-EPA方法9：风险评估基础指南-EPA方法10：风险评估的质量保证3.废物管理方法：-EPA方法11：可回收物品处理-EPA方法12：生物治理/垃圾填埋申请-EPA方法13：废物水处理系统操作4.空气质量评估方法：-EPA方法14：大气污染源排放计算-EPA方法15：大气质量模型基础指南-EPA方法16：大气氨浓度的测定方法-EPA方法17：大气细颗粒物的测定方法-EPA方法18：大气湿沉降物的收集和分析方法5.水质评估方法：-EPA方法19：水质评估基础指南-EPA方法20：废水处理工艺-EPA方法21：水样处理和分析方法-EPA方法22：饮用水质量监测这些方法索引只是EPA使用的一小部分方法。

EPA还有其他方法用于地下水监测、土壤污染评估、生物毒性评估和生态风险评估等。

为了确保准确性和合规性，使用这些方法时应仔细阅读相关的方法说明和操作程序，以确保正确的实施和数据采集。

美国环保局 EPA 试验方法 EPA 3550c

METHOD 3550CULTRASONIC EXTRACTIONSW-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 APPLICATION1.1This 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 describesprocedures 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 METHOD2.1Low 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.3.0DEFINITIONSRefer to Chapter One and the manufacturer's instructions for definitions that may be relevant to this method.4.0INTERFERENCES4.1Solvents, 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.5.0SAFETYThis 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 SUPPLIESThe 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 wattageof 300 watts, with pulsing capability. A device designed to reduce the cavitation sound is recommended. Follow the manufacturers instructions for preparing the disrupter forextraction of samples with low and medium/high concentrations.6.2.2Use a 3/4-inch horn for the low concentration method procedure and a1/8-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 weight6.4.1Drying 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 apparatus6.7.1Buchner funnel6.7.2Filter paper -- Whatman No. 41 or equivalent.6.8Kuderna-Danish (K-D) apparatus6.8.1Concentrator tube -- 10-mL, graduated (Kontes K-570050-1025 orequivalent). A ground-glass stopper is used to prevent evaporation of extracts.6.8.2Evaporation flask -- 500-mL (Kontes K-570001-500 or equivalent). Attachthe flask to the concentrator tube with springs, clamps, or equivalent.6.8.3Snyder column -- Three-ball macro (Kontes K-503000-0121 orequivalent).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 evaporativeconcentrators. Incorporation of this apparatus may be required by Federal, State orlocal municipality regulations that govern air emissions of volatile organics. EPArecommends the incorporation of this type of reclamation system as a method toimplement an emissions reduction program. Solvent recovery is a means to conformwith 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 padwith 50 mL of acetone followed by 50 mL of the elution solvent prior to packing thecolumn with adsorbent.6.17Nitrogen evaporation apparatus (optional) -- N-Evap, 12- or 24-position(Organomation Model 112, or equivalent).7.0REAGENTS AND STANDARDS7.1Reagent-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.7.4Extraction solventsSamples 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 cleanreference 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 orhexane. 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/vCH 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 candemonstrate 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 theappropriate exchange solvent. All solvents must be pesticide quality or equivalent. Examples of exchange solvents are given below.7.5.1Hexane, C 6H 147.5.22-Propanol, (CH 3)2CHOH 7.5.3Cyclohexane, C 6H 127.5.4Acetonitrile, CH 3CN 7.5.5Methanol, CH 3OH 8.0SAMPLE COLLECTION, PRESERVATION, AND STORAGE8.1See 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.9.0QUALITY CONTROL9.1Refer to Chapter One for additional guidance on quality assurance (QA) andquality 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 andspecifications 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 proficiencyEach 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 STANDARDIZATIONThere are no calibration or standardization steps directly associated with this sample extraction procedure.11.0PROCEDUREAs 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 stronglyadsorbed 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 ispositioned just below the surface of the solvent, yet above the sample. The sameapproach 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 extractionprocess.11.1Sample handling11.1.1Sediment/soil samples -- Decant and discard any water layer on asediment 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 beprepared 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 subdividethe 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 gafter 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 ona 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- to10-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 sampleg of sample×100This 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 procedureThis 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 increasesthe 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 sulfateand sample are mixed to the point of free-flowing.11.3.1The following steps should be performed rapidly to avoid loss of the morevolatile 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 mLof the matrix spiking solution. Consult Method 3500 for guidance on theappropriate choice of matrix spiking compounds and concentrations. Also see thenote 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 onthe appropriate choice of surrogate compounds and concentrations. Also see thenote in Sec. 11.3.11.3.1.4If gel permeation cleanup (see Method 3640) is to beemployed, the analyst should either add twice the volume of the surrogate spikingsolution (and matrix spiking solution, where applicable), or concentrate the finalextract to half the normal volume, to compensate for the half of the extract that islost 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 nothave a free-flowing sandy texture must be mixed with 60 g of anhydrous sodiumsulfate, using a spatula. If needed, more sodium sulfate may be added. Afteraddition of sodium sulfate, the sample should be free flowing. Also see the note inSec. 11.3.11.3.1.6Immediately add 100 mL of the extraction solvent or solventmixture (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 about1/2-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'sinstructions.11.3.3Extract the sample ultrasonically for 3 min, with output control knob set at10 (full power) or at the manufacturer’s recommended power setting, the mode switch onPulse (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 (orequivalent) 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 toremove particles.11.3.5Repeat the extraction two more times with two additional 100-mL portionsof clean solvent. Decant off the solvent after each ultrasonic extraction. After the finalultrasonic 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 theprocedure in Sec. 11.5. Otherwise, proceed to Sec. 11.7.11.4Medium/high concentration extraction procedureThis 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 ofthe 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 thematrix 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, theanalyst 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 normalvolume, to compensate for the half of the extract that is lost due to loading of the GPCcolumn.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 aspatula. 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).。

美国环保局EPA试验方法美国环保局EPA试验方法9045dSoilandWastepH

美国环保局EPA试验方法美国环保局EPA试验方法9045dSoilandWastepHMETHOD 9045DSOIL AND WASTE pH1.0SCOPE AND APPLICATION1.1This method is an electrometric procedure for measuring pH in soils and waste samples. Wastes may be solids, sludges, or non-aqueous liquids. If water is present, it must constitute less than 20% of the total volume of the sample.2.0SUMMARY OF METHOD2.1The sample is mixed with reagent water, and the pH of the resulting aqueous solution is measured.3.0INTERFERENCES3.1Samples with very low or very high pH may give incorrect readings on the meter. For samples with a true pH of >10, the measured pH may be incorrectly low. This error can be minimized by using a low-sodium-error electrode. Strong acid solutions, with a true pH of <1, may give incorrectly high pH measurements.3.2Temperature fluctuations will cause measurement errors.3.3Errors will occur when the electrodes become coated. If an electrode becomes coated with an oily material that will not rinse free, the electrode can (1) be cleaned with an ultrasonic bath, or (2) be washed with detergent, rinsed several times with water, placed in 1:10 HCl so that the lower third of the electrode is submerged, and then thoroughly rinsed with water, or (3) be cleaned per the manufacturer's instructions.4.0APPARATUS AND MATERIALS4.1pH meter with means for temperature compensation.4.2Glass electrode.4.3Reference electrode -- A silver-silver chloride or other reference electrode of constant potential may be used.NOTE:Combination electrodes incorporating both measuring and referenced functions are convenient to use and are available with solid, gel-type filling materials that require minimal maintenance.4.4Beaker -- 50-mL.4.5Thermometer and/or temperature sensor for automatic compensation.4.6Analytical balance -- capable of weighing 0.1 g.5.0REAGENTS5.1Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.5.2Reagent water. All references to water in this method refer to reagent water, as defined in Chapter One.5.3Primary standard buffer salts are available from the National Institute of Standards and Technology (NIST) and should be used in situations where extreme accuracy is necessary. Preparation of reference solutions from these salts requires some special precautions and handling, such as low-conductivity dilution water, drying ovens, and carbon-dioxide-free purge gas. These solutions should be replaced at least once each month.5.4Secondary standard buffers may be prepared from NIST salts or purchased as solutions from commercial vendors. Thesecommercially available solutions, which have been validated by comparison with NIST standards, are recommended for routine use.6.0SAMPLE PRESERVATION AND HANDLINGSamples should be analyzed as soon as possible.7.0PROCEDURE7.1Calibration7.1.1Because of the wide variety of pH meters and accessories, detailedoperating procedures cannot be incorporated into this method. Each analyst must beacquainted with the operation of each system and familiar with all instrument functions.Special attention to care of the electrodes is recommended.7.1.2Each instrument/electrode system must be calibrated ata minimum oftwo points that bracket the expected pH of the samples and are approximately three pH units or more apart. Repeat adjustments on successive portions of the two buffer solutions until readings are within 0.05 pH units of the buffer solution value. If anaccurate pH reading based on the conventional pH scale [0 to 14 at 25 E C] is required, the analyst should control sample temperature at 25 ± 1 E C when sample pH approaches the alkaline end of the scale (e.g., a pH of 11 or above).7.2Sample preparation and pH measurement of soils:7.2.1To 20 g of soil in a 50-mL beaker, add 20 mL of reagent water, cover, andcontinuously stir the suspension for 5 min. Additional dilutions are allowed if working with hygroscopic soils and saltsor other problematic matrices.7.2.2Let the soil suspension stand for about 1 hr to allow most of thesuspended clay to settle out from the suspension or filter or centrifuge off the aqueousphase for pH measurement.7.2.3Adjust the electrodes in the clamps of the electrode holder so that, uponlowering the electrodes into the beaker, the glass electrode will be immersed just deep enough into the clear supernatant solution to establish a good electrical contact through the ground-glass joint or the fiber-capillary hole. Insert the electrodes into the samplesolution in this manner. For combination electrodes, immerse just below the suspension.7.2.4If the sample temperature differs by more than 2 E C from the buffersolution, the measured pH values must be corrected.7.2.5Report the results as "soil pH measured in water at E C" where " E C" isthe temperature at which the test was conducted.7.3Sample preparation and pH measurement of waste materials7.3.1To 20 g of waste sample in a 50-mL beaker, add 20 mL of reagent water,cover, and continuously stir the suspension for 5 min. Additional dilutions are allowed if working with hygroscopic wastes and salts or other problematic matrices.7.3.2Let the waste suspension stand for about 15 min to allow most of thesuspended waste to settle out from the suspension or filter or centrifuge off aqueousphase for pH measurement.NOTE:If the waste is hygroscopic and absorbs all the reagent water, begin theexperiment again using 20 g of waste and 40 mL of reagent water.NOTE:If the supernatant is multiphasic, decant the oily phase and measure the pH of the aqueous phase. The electrode may need to be cleaned (Step 3.3) if itbecomes coated with an oily material.7.3.3Adjust the electrodes in the clamps of the electrode holder so that, uponlowering the electrodes into the beaker, the glass electrode will be immersed just deep enough into the clear supernatant to establish good electrical contact through the ground-glass joint or the fiber-capillary hole. Insert the electrode into the sample solution in this manner. For combination electrodes, immerse just below the suspension.7.3.4If the sample temperature differs by more than 2 E C from the buffersolution, the measured pH values must be corrected.7.3.5Report the results as "waste pH measured in water at E C" where " E C"is the temperature at which the test was conducted.8.0QUALITY CONTROL8.1Refer to Chapter One for the appropriate QC protocols.8.2Electrodes must be thoroughly rinsed between samples.9.0METHOD PERFORMANCE9.1No data provided.10.0REFERENCES1.Black, Charles Allen; Methods of Soil Analysis; American Society of Agronomy:Madison, WI, 1973.2.National Bureau of Standards, Standard Reference Material Catalog, 1986-87, SpecialPublication 260.METHOD 9045D SOIL AND WASTE pH。

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矿产资源开发利用方案编写内容要求及审查大纲
矿产资源开发利用方案编写内容要求及《矿产资源开发利用方案》审查大纲一、概述
㈠矿区位置、隶属关系和企业性质。

如为改扩建矿山, 应说明矿山现状、
特点及存在的主要问题。

㈡编制依据
(1简述项目前期工作进展情况及与有关方面对项目的意向性协议情况。

(2 列出开发利用方案编制所依据的主要基础性资料的名称。

如经储量管理部门认定的矿区地质勘探报告、选矿试验报告、加工利用试验报告、工程地质初评资料、矿区水文资料和供水资料等。

对改、扩建矿山应有生产实际资料, 如矿山总平面现状图、矿床开拓系统图、采场现状图和主要采选设备清单等。

二、矿产品需求现状和预测
㈠该矿产在国内需求情况和市场供应情况
1、矿产品现状及加工利用趋向。

2、国内近、远期的需求量及主要销向预测。

㈡产品价格分析
1、国内矿产品价格现状。

2、矿产品价格稳定性及变化趋势。

三、矿产资源概况
㈠矿区总体概况
1、矿区总体规划情况。

2、矿区矿产资源概况。

3、该设计与矿区总体开发的关系。

㈡该设计项目的资源概况
1、矿床地质及构造特征。

2、矿床开采技术条件及水文地质条件。

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