Analytical Chemistry Methods Manuals _ Microbiological and Chemical Exposure

March 23, 2018 | Author: robby2105 | Category: Gas Chromatography, High Performance Liquid Chromatography, Volatile Organic Compound, Detection Limit, Chromatography
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Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPAAnalytical Chemistry Methods Manuals: Manual of Manuals Summaries and Ordering Information for Eight Laboratory Analytical Chemistry Methods Manuals Published by the EPA between 1988 and 1995. - Prepared by William L. Budde This document contains the titles, publication numbers, dates of publication, ordering information, abstracts, tables of contents, analyte-method cross reference lists, and Introductions to eight laboratory analytical chemistry methods manuals published between 1988 and 1995. The complete manuals may be ordered from the National Technical Information Service (NTIS) at the address or telephone numbers below: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Voice: 703-487-4650 or 800-553-6847 Fax: 703-321-8547 The shipping charge per order is $3.00. On this page: Organics Manual of 1988 Organics Supplement I of 1990 Organics Supplement II of 1992 Organic Supplement III of 1995 Metals Manual of 1991 Metals Supplement I of 1994 Inorganic Non-Metals of 1993 Marine & Estuarine of 1992 Methods for the Determination of Organic Compounds in Drinking Water Environmental Monitoring Systems Laboratory Office of Research and Development U.S. Environmental Protection Agency Cincinnati, Ohio 45268 EPA-600/4-88/039 December 1988 (Revised July 1991) This manual is available from NTIS and contains Methods 502.1, 502.2, 503.1, 504, 505, 507, 508, 508A, 515.1, 524.1, 524.2, 525.1 and 531.1. Note that all of these methods except 502.1, 503.1, 508A and 524.1 have been revised and published in one of the three organics supplements that are described in this document. Address your request for this manual to NTIS and ask for their order number PB91-231480; the cost is $61.50. Abstract Thirteen analytical methods for the identification and measurement of organic compounds in drinking water are described in detail. Six of the methods are for volatile organic compounds (VOCs) and certain disinfection by-products, and these methods were cited in the Federal Register of July 8, 1987, under the National Primary Drinking Water Regulations. The other seven methods are designed for the determination of a variety of synthetic organic compounds and pesticides, and these methods were cited in proposed drinking water regulations in the Federal Register of May 22, 1989. Five of the methods utilize the inert gas purge-and-trap extraction http://www.epa.gov/nerlcwww/methmans.html#organics_supp_ii[8.12.2010 19:05:46] Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA procedure for VOCs, six methods employ a classical liquid-liquid extraction, one method uses a new liquid-solid extraction technique, and one method is for direct aqueous analysis. Of the 13 methods, 12 use either packed or capillary gas chromatography column separations followed by detection with mass spectrometry or a selective gas chromatography detector. One method is based on a high performance liquid chromatography separation. Table of Contents Method Number 502.1 Foreword Abstract Analyte - Method Cross Reference Acknowledgement Introduction Volatile Halogenated Organic Compounds in Water by Purge and Trap Gas Chromatography Volatile Organic Compounds in Water By Purge and Trap Capillary Column Gas Chromatography with Photoionization and Electrolytic Conductivity Detectors in Series Title Revision Page 2.0 iii iv vii xii 1 5 502.2 2.0 31 503.1 Volatile Aromatic and Unsaturated Organic Compounds in Water by Purge and Trap Gas 2.0 Chromatography 1,2-Dibromoethane (EDB) and 1,2-Dibromo3-Chloropropane (DBCP) in Water by 2.0 Microextraction and Gas Chromatography Analysis of Organohalide Pesticides and Commerical Polychlorinated Biphenyl Products in Water by Micro-Extraction and Gas Chromatography 2.0 63 504 89 505 109 507 Determination of Nitrogen- and PhosphorusContaining Pesticides in Water by Gas 2.0 Chromatography with a Nitrogen-Phosphorus Detector Determination of Chlorinated Pesticides in Water by Gas Chromatography with An Electron Capture Detector Screening for Polychlorinated Biphenyls by Perchlorination and Gas Chromatography Determination of Chlorinated Acids in Water by Gas Chromatography with an Electron Capture Detector 3.0 1.0 4.0 143 508 508A 515.1 171 199 221 http://www.epa.gov/nerlcwww/methmans.html#organics_supp_ii[8.12.2010 19:05:46] Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 524.1 Measurement of Purgeable Organic Compounds in Water by Packed Column GasChromatography/Mass Spectrometry Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry Measurement of N-Methylcarbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post Column Derivatization Analyte-Method Cross Reference Analyte Acifluorfen Acenaphthylene Alachlor Aldicarb Aldicarb sulfone Aldicarb sulfoxide Aldrin Ametryn Anthracene Aroclor 1016 Aroclor 1221 Aroclor 1232 Aroclor 1242 Aroclor 1248 Aroclor 1254 Aroclor 1260 Aroclor (General screen) Atraton Atrazine Baygon 515.1 525.1 505, 507, 525.1 531.1 531.1 531.1 505, 508, 525.1 507 525.1 505, 508, 525.1 505, 508, 525.1 505, 508, 525.1 505, 508, 525.1 505, 508, 525.1 505, 508, 525.1 505, 508, 525.1 508A, 525.1 507 505, 507, 525.1 531.1 3.0 253 524.2 3.0 283 525.1 2.2 323 531.1 3.0 361 Method No. http://www.epa.gov/nerlcwww/methmans.html#organics_supp_ii[8.12.2010 19:05:46] 524. 508.2010 19:05:46] 515.2.1 502. 524. 524. 524.12.2 507 507 502.2.1.1 507 502. 502.1.2.1. 524.1.1 531. 503.gov/nerlcwww/methmans.2 502.1.2.2 525. 524. 524.2.1.1. 508.2 507 515.2 502. 502.1 502. 525. 524. 502. 524.1. 502.1 525. 502.1.2 502.2 502. 524.1 531. 502.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Bentazon Benz[a]anthracene Benzene Benzo[b]fluoranthene Benzo[k]fluorathene Benzo[g.epa. 524.1.1.2.2 502.1 505. 524.i]perylene Benzo[a]pyrene Bromacil Bromobenzene Bromochloromethane Bromodichloromethane Bromoform Bromomethane Butachlor Butylate n-Butylbenzene sec-Butylbenzene tert-Butylbenzene Butylbenzylphthalate Carbaryl Carbofuran Carbon tetrachloride Carboxin Chloramben Chlordane (Technical) Chlordane-alpha Chlordane-gamma Chlorneb http://www.1.1 525.2.1 525.2 502.2 525. 503.2. 524. 524. 524.1.1 525.2.1. 525.1 505.html#organics_supp_ii[8.1.1. 508 505.1.2. 524.1. 503.h. 503. 524.1 508 . 503. 1 508 515.4-D) 4-(2. 524. 502.4'-DDD[1. 502.1.2. 502. 503.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Chlorobenzene Chlorobenzilate 2-Chlorobiphenyl Chloroethane Chloroform Chloromethane Chlorothalonil 2-Chlorotoluene 4-Chlorotoluene Chlorpropham Chrysene Cycloate Dalapon Dimethyl-2. 502.1.1-trichloro2. 524. 524.1. 503.1.2-bis(pchlorophenyl)ethylene] 4.2-bis(pchlorophenyl)ethane] Diazinon http://www.1. 524.1.2.12.1 2.1.6tetrachloroterephthalate (DCPA) (Dacthal) DCPA mono and diacid metabolites 502.2 508 502.4-DB) 4.1-dichloro2.1 507 515.gov/nerlcwww/methmans. 524.1.1.2 502.1. 524.1 502.2 508 525.2.1. 524. 524. 502.1-dichloro2.5.1. 502.2010 19:05:46] 515.4'-DDT[1.html#organics_supp_ii[8.3. 524.2-bis(pchlorophenyl)ethane] 4. 524.4Dichlorophenoxy)butyric acid (2.4-Dichlorophenoxyacetic 515. 524.2.2.1.1.2.2 502. 503.1 acid (2.2 507 525.1 508 508 508 507 .1.2 502.1.4'-DDE[1.epa. 524. 3-Dichlorobenzene 1. 524. 524.1. 502.2 515. 502.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Dibenz[a.2.2.5-Dichlorobenzoic acid 2. 524.2 502.1.2.1. 502.3-Dichlorobiphenyl 1.2 502.1. 502.2-Dichloroethene trans-1.2.2-Dichlorobenzene 1.2-Dichloropropane 1.2010 19:05:46] 525.2. 502. .1. 502.2.1 502.1.1.1-Dichloropropene cis-1.1-Dichloroethane 1.3-Dichloropropene http://www.1. 524. 524. 524.2. 524. 502.2-Dichloroethane 1. 524.1 515.2 502. 524. 502.1-Dichloroethene cis-1.2 502.2.2 502.h]anthracene Dibromochloromethane 1.1.1.2.2.2. 524. 524.1. 504.2 502.2-Dibromoethane Di-n-butylphthalate Dicamba 1.1.2.2.2 502.2 502.2 502. 524.1.1.1. 524.1. 502. 524.1 502. 502.2 502.2-Dichloroethene 1.1. 504.1.2-Dichloropropane 1. 524.1. 524.1.1. 524. 524. 502.2 502.gov/nerlcwww/methmans.1. 524. 503. 524.2-Dibromo-3chloropropane Dibromomethane 1.3-Dichloropropane 2.2 525. 502. 524.2. 503.1. 524. 524. 524. 524.1.1. 503.2. 524.1.1. 524.1 502.1.1. 524.1 525. 524.2 502.4-Dichlorobenzene 3. 524.2.1.1. 502. 502. 524.12.2 502.2 502.1. 502.html#organics_supp_ii[8. 502.1.1.1. 524. 524.2.epa.1. 525.2.epa. 524. 524.1]5-heptene-2.2 525. 524.1 507 507 507 507 508 508 508 508 505.1 525.2.12.1.1.1 Etridiazole Fenamiphos Fenarimol 508 507 507 http://www.2 trans-1. 502.1.3-Dichloropropene Dichlorodifluoromethane Dichlorprop Dichlorvos Dieldrin Diethylphthalate Dimethylphthalate Dinoseb Diphenamid Disulfoton sulfoxide Disulfoton sulfone Disulfoton Endosulfan sulfate Endosulfan I Endosulfan II Endrin aldehyde Endrin S-Ethyl dipropylthiocarbamate (EPTC) n-(2Ethylhexyl)bicyclo[2. 508. 524.1 507 505.gov/nerlcwww/methmans.2010 19:05:46] .1 507 507 507 502.html#organics_supp_ii[8. 503.2.1. 524.1.1. 524.1 515.2 502.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 524. 508 525.1 bis(2-Ethylhexyl)phthalate 525.2 515.2. 502.3dicarboximide (MGK-264) Ethoprop Ethylbenzene bis(2-Ethylhexyl)adipate 502. 525. 508.1 505.1. 508.2.2010 19:05:46] . 525. 508.1 502.2'. 503.4.5.1 505.2.2.6Heptachlorobiphenyl Hexachlorobenzene 2.1 515. 524.1 525.html#organics_supp_ii[8.d]pyrene Isopropylbenzene 4-Isopropyltoluene Merphos Methiocarb Methomyl Methoxychlor Methyl paraoxon Methylene chloride 507 531.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Fluorene Fluridone alpha Hexachlorocyclohexane (alpha BHC)(HCH-alpha) beta Hexachlorocyclohexane (beta BHC)(HCH-beta) delta Hexachlorocyclohexane (delta BHC)(HCH-delta) gamma Hexachlorocyclohexane (Lindane)(gamma BHC)(HCH-gamma) Heptachlor Heptachlor Epoxide 2.4'. 525.1.2 Hexachlorocyclopentadiene 505.1 525.3. 524. 524.3'.1 531.1 507 508 508 508 505.2'.1 505.1. 524.4. 508. 525.3.1 502.gov/nerlcwww/methmans. 525.1 525.6'Hexachlorobiphenyl Hexachlorobutadiene 525.2 http://www.1 Hexazinone 3-Hydroxycarbofuran 5-Hydroxydicamba Indeno[1.2.2 507 531. 502. 524.1 505.1.1.2.12. 503. 503.epa.2 502.c. 525.1 507 502. 508.4'. 5'.2 503.1 505 505.2 525.2'.1 508A 507 507 507 508 507 502.1 531.1 515.524.3'.1. 525.6'Octachlorobiphenyl Oxamyl Pentachlorophenol (PCP) Pebulate 2.1 505.3.6Pentachlorobiphenyl cis-Permethrin trans-Permethrin Phenanthrene Picloram Polychlorobiphenyls (General screen) Prometon Prometryn Pronamide Propachlor Propazine Propylbenzene n-Propylbenzene Pyrene Simazine Simetryn 507 507 507 507 502.1. 525.4. 525.12.2010 19:05:46] .1 508 508 525. 507.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Metolachlor Metribuzin Mevinphos Molinate Naphthalene Napropamide 4-Nitrophenol cis-Nonachlor trans-nonachlor Norflurazon 2.epa. 503.2'.1 507 525.html#organics_supp_ii[8.1 515.2.gov/nerlcwww/methmans.3'.6. 524.2 507 515.1 507 525.4.1.1 507 http://www. 525.2.1-Trichloroethane 1. 524.2.2.1.1.1.2 502.1.1 507 502.2 525.2 502. 503.4-Trichlorobenzene 2. 524.2-Tetrachloroethane 1.5Trichlorophenoxy)propionic 515.1. 524.2. 524.2'. 524.1. 503. 524.1 2-(2.5-T) 507 502.gov/nerlcwww/methmans.2.2.1.1.5-Trichlorobiphenyl Trichloroethene 1.1.1.524.1.2 502.1.4. 524.5Trichlorophenoxyacetic acid (2.2.2 502. 503.1.1.1.html#organics_supp_ii[8. 524. 524.4.1 502.2.2.2.4. 502.1.1.4. 502.2 502.2 http://www.503.4.2.12.1.2 502. 524. 524. 508.4'Tetrachlorobiphenyl 2.epa.1. 524.3-Trichloropropane 507 507 507 507 502. 524.2 505. 502. 503.2 502.1 acid (2. 502.2.2.2 502.1. 524.1. 524. 502.1 515. 524.1.1.2.2. 502.2 525.2-Tetrachloroethane Toluene Toxaphene (Technical) Triademefon 1. 524.1.524.1.5-TP)(Silvex) Tebuthiuron Terbacil Terbufos Terbutryn Tetrachloroethene 1.1.1.2.2-Trichloroethane Trichlorofluoromethane 1.4. 524.1.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Stirofos Styrene 2.3-Trichlorobenzene 1.2010 19:05:46] . 524. 502.1. 524. 502. 503. Methods developed for drinking water include provisions for removal of free chlorine http://www. Therefore caution is needed when applying these methods to matrices other than relatively clean water. for example.1.1. 524. 524. 524. Some methods require relatively modest equipment. that is. General Method Features Each of the methods in the manual was written to stand-alone.2. This flexible approach should meet the needs and requirements of nearly all laboratories. 524. industrial wastewaters and beverages. Some methods have been tested only in reagent water and/or drinking water. 524.2.2.1.2 502. While some of these methods may provide reliable results with more complex water matrices. 524. drinking water and some ground and surface waters.2 502. This approach of multiple methods for many analytes was selected to provide the maximum flexibility to method users from small and large laboratories.1. The authors believe that the added bulk of the manual is a small price to pay for the flexibility of the format.html#organics_supp_ii[8.2.2 507 502.2. 502.2 502. Sample Matrices All methods were developed for relatively clean water matrices. 503.1. nearly 50 compounds are listed as analytes in four different methods.2010 19:05:46] .3. The names of authors of the methods are provided to assist users in obtaining direct telephone support when required. For example. and this feature is especially helpful in the quality control sections where standardized terminology is not yet available. Revisions of these methods will be made available in a similar stand-alone format to facilitate the replacement of existing methods as new technical developments occur.2. for example. inserted into another binder. This flexibility comes at the cost of some duplication of material.gov/nerlcwww/methmans. 524.2. 524.epa. that is. photocopied. the definitions of terms section of each method is nearly identical.2 Introduction William L.2 502. An important feature of the methods in this manual is the consistent use of terminology.1. 503.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Tricyclazole Trifluralin 1. and used without loss of information. and others require sophisticated instrumentation. 524. Environmental Protection Agency Many of the nearly 200 organic analytes included in this manual may be identified and measured in drinking water using two or more of the documented analytical methods.1.5-Trimethylbenzene Vernolate Vinyl chloride m-Xylene o-Xylene p-Xylene 507 508 502. 524. 503. each method may be removed from the manual. techniques for dealing with more complex matrices have not been included in the methods in order to keep them as simple and brief as possible. The terms were carefully selected to be meaningful without extensive definition. 503.12. Budde U.4-Trimethylbenzene 1.1.1. 503.1. and therefore should be easy to understand and use. S. 2. or a concentration of compound in a clean water matrix that gives a peak in the final extract with a signal-to-noise ratio of about 5. The MDL is calculated from the standard deviation of replicate measurements. 524.1. but they may not be of regulatory significance.2. In addition. Detection Limits Most methods include either a method detection limit (MDL) or an estimated detection limit (EDL) for each analyte. Methods for Volatile Organic Compounds (VOCS) Six of the methods in the manual are for the determination of VOCs and certain disinfection byproducts.gov/nerlcwww/methmans. and bring them up-todate. Solicited and unsolicited written and telephoned comments have been received from some of the laboratories using the VOC methods.epa. The other method (Method 504) is a microextraction procedure for two compounds of special interest. Ascorbic acid has been extensively tested as a dechlorinating http://www. or to prevent the formation of method interferences and analytes generated from chlorination of impurities in reagents and solvents.html#organics_supp_ii[8. depending on the specific method selected. 503. (b) to prevent acid or base catalyzed decomposition of analytes. If the replicate measurements needed to calculate an MDL are obtained under ideal conditions. and accurate calibration standards and quality control samples are needed to implement the methods. the resulting standard deviation may be small and give an unrealistically low MDL. Dechlorination is necessary to stop the formation of trichloromethanes and other disinfection by-products.2-dibromo-3-chloropropane (DBCP).Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA (dechlorination) which is assumed to be present in all samples. The revisions of the six VOC methods contained in the manual incorporate a few technical and many editorial changes which are summarized below. 502. 26 W. and some of these users suggested certain technical and editorial changes. These limits are intended to provide an indication of the capability of the method. Calibration Standards and Quality Control Samples The methods contain separate calibration and quality control sections. but. The six VOC methods have been distributed in the form of photocopied documents by EMSLCincinnati to several hundred laboratories in the last two years.Cincinnati. and the MDL will be more realistic.1. measured. 504. or may be available on a limited basis from the Quality Assurance Research Division. OH. and reported with 99% confidence that the analyte concentration is greater than zero. the staff of the Chemistry Research Division recognized that some changes were needed to make the methods easier to understand and use. The data acquired for measurement of an MDL should be obtained over a period of time (several days or more).1 and 524. during a short period of time within a work shift. and (c) to improve the extraction efficiency of certain analytes. Environmental Monitoring Systems Laboratory . Similarly. ethylene dibromide (EDB) and 1. Calibration standards and quality control samples may be available commercially. 1987 under the National Primary Drinking Water Regulations. Martin Luther King Drive. The EDL is either the MDL. 45268. Calibration standards and quality control samples should be obtained from different sources so that the quality control sample can provide an independent check on the calibration and the other method variables. The use of ascorbic acid as a dechlorinating agent is described. These methods were cited in the Federal Register of July 8.12. Cincinnati. the user has a choice of a packed or capillary column gas chromatography (GC) separation and a mass spectrometer (MS) or conventional GC detector. and is defined as the minimum concentration of a substance that can be identified. These are Methods 502. Obtained in this way. Few technical changes were made to the six VOC methods. pH adjustments are included in some of the methods for several reasons: (a) to retard growth in dechlorinated water of bacteria that can decompose some analytes. for example.2010 19:05:46] . Five of these methods utilize the same basic purge-and-trap extraction technique. the standard deviation includes normal day-to-day variations. 508. and measured with a high resolution capillary column GC/MS procedure. Methods for Synthetic Organic Compounds (SOCS) Four of the SOC methods were developed for a national pesticides survey conducted by EPA during 1987-1989. and detection limits.epa. consistent.12. Method 505. Data is presented in the method to show that the open split interface can provide acceptable precision.1. Method 505 provides a rapid procedure for chlorinated hydrocarbon pesticides and commercial PCB mixtures (Aroclors). but without the undesirable generation of sulfur dioxide at low pH. 515.2 allowed any interface that could meet the precision and accuracy requirements of the method. was developed to provide a rapid method for the determination of chlorinated hydrocarbon pesticides and commercial PCB mixtures (Aroclors) in drinking water. and a quality control procedure was developed to permit selection of cartridges with acceptable performance characteristics. This method uses a high resolution capillary column GC separation and detection with an electron capture detector.) plastic or glass tubes packed with reverse phase liquid chromatography packing materials. but the interfaces previously mentioned were retained.gov/nerlcwww/methmans. The LSE procedure is attractive because it greatly reduces the use and worker exposure to methylene chloride and similar solvents. The disks are made of Teflon containing silica which is coated with a chemically bonded C-18 organic phase. Changes were made in the recommended chromatographic conditions and internal standards in Method 502. a relatively simple microextraction procedure patterned after Method 504. polycyclic http://www. The disks are manufactured by a single company. so only one type was evaluated. 508. Many laboratories will find the open split interface to be the most economical for this method. One of the methods (531. Cartridges from six suppliers were used in the methods research. One screening method (Method 508A) for polychlorinated biphenyls (PCBs) was developed as a result of a specific request from the Office of Drinking Water (ODW). The addition of these details.5 in. Water samples are passed through the cartridges or disks and some organic compounds are sorbed on the solid phase. This allows the simultaneous determination of 42 SOCs including chlorinated hydrocarbon pesticides. x 3 in. and these are designated Methods 507.2.1) uses a liquid-solid extraction (LSE) procedure based on commercial LSE cartridges or disks. and has been found to be as effective as sodium thiosulfate.1 is a broad spectrum GC/MS method for a variety of compounds under consideration for regulation. The compounds in the cartridge extract are separated. and the uniform organization of all the methods should substantially reduce the number of questions received and provide the user community with the information needed to obtain high quality results. These changes allow the measurement of all 60 VOCs in a single calibration solution. These editorial changes were necessary to provide an organized. The method uses the powerful chlorinating agent antimony pentachloride to convert all the PCB congeners in a sample extract to decachlorobiphenyl which is separated with either packed or capillary column gas chromatography. After air drying. Three of the methods used in the national pesticides survey utilize a liquid-liquid extraction of the SOCs from water followed by a high resolution capillary column GC separation and detection with an electron capture or other selective detector (Methods 507. and much more complete presentation of the myriad details needed by laboratories to successfully implement the methods. the consistent use of terminology. accuracy. The broad spectrum GC/MS method (Method 525. the organic compounds are eluted using a very small volume of an organic solvent. and it was developed specifically to utilize the new liquid-solid extraction technology and minimize use of the solvent methylene chloride. and detected with an electron capture detector.1) employs the direct analysis of a water sample with a high performance liquid chromatography (HPLC) separation and post-column derivatization to a compound detected with a fluorescence detector. identified.1). and 531. Method 508A was designed as a screening procedure for polychlorinated biphenyls (PCBs).2010 19:05:46] . Extensive editorial changes were made in all six VOC methods.html#organics_supp_ii[8. and 515.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA agent. Method 525.2. The open split interface between the GC and the MS was incorporated into Method 524. The previous revision of Method 524.1. The cartridges are small (about 0. Please note that Methods 506. Ohio 45268 EPA-600/4-90/020 July 1990 This manual is available from NTIS and contains Methods 506. 551.epa.1.3. Seven of these methods cover compounds designated for regulation under the Safe Drinking Water Act Amendments of 1986. Regulations for this group are in the proposal stages with promulgation scheduled for June 1992.12. 550. Address your request for this manual to to NTIS and ask for their order number PB91-146027. The remainder employ capillary column gas chromatography. To the: Chemical Exposure Research Branch Top of page Methods for the Determination of Organic Compounds in Drinking Water Supplement Ik Environmental Monitoring Systems Laboratory Office of Research and Development U. and 552 have been revised and the revised versions are published in Supplement II or III. 548. 548. Labeled isotopes of this analyte are employed as tracers and high resolution mass spectrometry is required for detection and unambiguous identification. 547. Table of Contents Method Number 506 Foreword Abstract Acknowledgment Analyte . phthalate and adipate esters. Most of the analytes may be classified as non-volatile and three of the methods entail separations by high performance liquid chromatography. Laboratories will find this method attractive because of its potential economy of operation when a wide variety of analytes are to be determined.S. 2. individual PCB congeners. 550. 551 and 552.50. a trend which is likely to become even more pronounced in the future.2010 19:05:46] . Three of the methods herein offer new and simplified liquid-solid extraction procedures. several triazine pesticides. Abstract Nine analytical methods covering 54 organic contaminants which may be present in drinking water or drinking water sources are described in detail.Method Cross Reference Introduction Determination of Phthalate and Adipate Esters in Drinking Water by Liquid-Liquid Extraction or LiquidSolid Extraction and Gas Chromatography with Title Page iii iv vi vii 1 5 http://www.7. the cost is $51.8-tetrachlorodibenzop-dioxin. 549. at the low parts per trillion level.html#organics_supp_ii[8. The other two methods are for chlorination disinfection byproducts and may be regulated as part of EPA's disinfectants and disinfectant byproducts rule scheduled for proposal early in 1992. and pentachlorophenol. Environmental Protection Agency Cincinnati.gov/nerlcwww/methmans.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA aromatic hydrocarbons. One of these requires detection of a potentially very toxic contaminant. 549. 513. 1 550. 550.1 550. and Gas Chromatography with Electron Capture Detection Analyte-Method Cross Reference Analyte Acenaphthene Acenaphthylene Anthracene Benz(a)anthracene Benzo(b)fluoranthene Method No.1 143 551 169 552 201 .8-Tetrachloro-dibenzo-p-dioxin in Drinking Water by Liquid-Liquid Extraction and Gas Chromatography with High-Resolution Mass Spectrometry Determination of Glyphosate in Drinking Water by Direct-Aqueous-Injection HPLC. and Fluorescence Detection Determination of Endothall in Drinking Water by Aqueous Derivatization.1 550. http://www.3. 550. 550.epa. 550.1 550. Liquid-Solid Extraction.gov/nerlcwww/methmans.html#organics_supp_ii[8. 550.1 550.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Photoionization Detection 513 Determination of 2.2010 19:05:46] 33 547 63 548 81 549 101 550 121 550. and Gas Chromatography with Electron-Capture Detection Determination of Diquat and Paraquat in Drinking Water by Liquid-Solid Extraction and HPLC with Ultraviolet Detection Determination of Polycyclic Aromatic Hydrocarbons in Drinking Water by Liquid-Liquid Extraction and HPLC with Coupled Ultraviolet and Fluorescence Detection Determination of Polycyclic Aromatic Hydrocarbons in Drinking Water by Liquid-Solid Extraction and HPLC with Coupled Ultraviolet and Fluorescence Detection Determination of Chlorination Disinfection Byproducts and Chlorinated Solvents in Drinking Water by LiquidLiquid Extraction and Gas Chromatography with Electron-CaptureDetection Determination of Haloacetic Acids in Drinking Water by Liquid-Liquid Extraction.7. Post-Column Derivatization. Derivatization. 550.12. 1 550.html#organics_supp_ii[8.i)perylene Benzo(a)pyrene Bis(2-ethylhexyl)adipate Bis(2ethylhexyl)phthalate Bromochloroacetic Acid Bromochloroacetonitrile Bromodichloromethane Bromoform Butylbenzyl phthalate Carbon Tetrachloride Chloral Hydrate Chloroform Chloropicrin Chrysene Dibenz(a.1-Dichloropropanone-2 Diethyl phthalate Dimethyl phthalate Di-n-butyl phthalate 552 551 552 551 506 506 506 http://www.1 552 551 551 551 1.h)anthracene Dibromoacetic Acid Dibromoacetonitrile Dibromochloromethane 1. 550.4-Dichlorophenol 1. 550. 550.2010 19:05:46] .Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Benzo(k)fluoranthene Benzo(g.1 550.epa.h.2-Dibromo-3chloropropane(DBCP) 550.12.1 550. 550.1 506 506 552 551 551 551 506 551 551 551 551 550.gov/nerlcwww/methmans.2-Dibromoethane(EDB) 551 Dichloroacetic Acid Dichloroacetonitrile 2. Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Di-n-octyl phthalate Diquat Endothall Fluoranthene Fluorene Glyphosate Indeno(1,2,3-cd)pyrene Monobromoacetic Acid Monochloroacetic Acid Naphthalene Paraquat Phenanthrene Pyrene 2,3,7,8Tetrachlorodibenzo-pdioxin Tetrachloroethylene Trichloroacetic Acid Trichloroacetonitrile 1,1,1-Trichloroethane Trichloroethylene 2,4,6-Trichlorophenol 1,1,1Trichloropropanone-2 Introduction James W. Eichelberger 506 549 548 550, 550.1 550, 550.1 547 550, 550.1 552 552 550, 550.1 549 550, 550.1 550, 550.1 513 551 552 551 551 551 552 551 U. S. Environmental Protection Agency An integral component of the role of the Environmental Protection Agency (EPA) in protecting the quality of the Nation's water resources is the provision of means for monitoring water quality. In keeping with this role, EPA develops and disseminates analytical methods for measuring chemical and physical parameters affecting water quality, including chemical contaminants which may have http://www.epa.gov/nerlcwww/methmans.html#organics_supp_ii[8.12.2010 19:05:46] Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA potential adverse effects upon human health. This manual provides nine, analytical methods for 54 organic contaminants, which may be present in drinking water or drinking water sources. In December 1988, EPA published "METHODS FOR THE DETERMINATION OF ORGANIC COMPOUNDS IN DRINKING WATER", EPA/600/4-88/039, a manual containing 13 methods for approximately 200 potential drinking water contaminants. The current manual is a supplement to the earlier version, providing, for the most part, methods for analytes which appear at a later time in the regulatory framework. Efforts have been made herein to provide a manual and methods format, which is consistent with the earlier version. Regulatory Background Analytical methodology for monitoring water quality serves a number of related purposes, including occurrence studies in community water systems, health effects studies, and the determination of the efficacy of various water treatment approaches. These activities, in turn, form the supporting bases for water quality regulations, and the support of these regulations is the ultimate purpose of the analytical methods. Limitations on the levels of specific contaminants are codified in proposed and promulgated Federal regulations developed in response to the Safe Drinking Water Act (SDWA) of 1974 and the SDWA amendments of 1986. The Act requires EPA to promulgate regulations for contaminants in drinking water which may cause adverse health effects and which are known or anticipated to occur in public water systems. The 1986 amendments require regulations to include Maximum Contaminant Levels (MCL's) with compliance determined by regulatory monitoring or by the application of an appropriate treatment, when adequate analytical methodology is not available. In addition, the 1986 amendments specified 83 contaminants, originally scheduled for regulation by June 19, 1989. The amended Act also required EPA to develop a priority list of additional contaminants, to propose 25 more of these by January of 1988 for subsequent regulation and to continue this process by the addition of 25 from the priority list on a triennial basis thereafter. Of the original 83 pollutants, regulations for eight volatile organic chemicals (VOC) were promulgated in June 1987 (see 52 FR 25690 and 51 FR 11396). Analytical methods for these eight as well as other unregulated VOC's were published in the December 1988 manual (EPA Methods 502.1, 502.2, 503.1, 524.1 and 524.2). Regulations for thirty synthetic organic chemicals (SOC's) were proposed May 22, 1989 (54 FR 22062) and scheduled for promulgation by December 1990. Note that this group included six SOC's which, by authority of provisions in the 1986 amendments, were substituted into the original list of 83 in January 1988 (53 FR 1892) - namely aldicarb sulfoxide, aldicarb sulfone, ethylbenzene, heptachlor, heptachlor epoxide and styrene. With the exception of lindane, analytical methods for all thirty compounds are by the VOC methods above or SOC methods also included in the 1988 manual. The current manual provides analytical methods for many of the remaining contaminants on the original list of 83 - namely adipates, diquat, endothall, glyphosate, polycyclic aromatic hydrocarbons (PAH's), phthalates and dioxin. Phase V of EPA regulations for these and eleven other remaining SOC's from the list of 83 is scheduled for proposal in June 1990 and promulgation in March 1992. Analytical methods for the latter eleven were included in the December 1988 manual. Methods 551 and 552 of this manual cover the most important classes of organic chlorination disinfection byproducts. These contaminants were included in the first EPA priority list of additional substances, which may require regulation under the Act (see 53 FR 1892). At least some of these will be regulated by EPA's phase IV disinfectants and disinfectant byproducts rule scheduled for proposal early in 1992. General Comments The current manual provides methods, which are in the same format and cast in the same terminology as the December 1988 manual. The introduction to the earlier manual discusses general method features on format, sample matrices, method detection limits, and calibration and quality control samples. These same comments apply herein. In particular, these methods are written in standardized terminology in a stand-alone format, requiring no other source material for application. The methods are designed for drinking water and drinking water sources and not for more complex matrices such as waste water, hazardous waste effluents or biological fluids. The method detection limits provided were determined by replicate analyses of fortified reagent water over a relatively short period of time. As such, these are somewhat idealized limits, but nevertheless provide a useful index of method performance. Reporting limits for reliable quantitative data may be considerably higher. http://www.epa.gov/nerlcwww/methmans.html#organics_supp_ii[8.12.2010 19:05:46] Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA The quality assurance sections are uniform and contain minimum requirements for operating a reliable monitoring program - initial demonstration of performance, routine analyses of reagent blanks, analyses of fortified reagent blanks and fortified matrix samples, and analyses of quality control (QC) samples. Other quality control practices are recommended and may be adopted to meet the particular needs of monitoring programs - e. g., the analyses of field reagent blanks, instrument control samples and performance evaluation samples. Where feasible, surrogate analytes have been included in the methods as well as internal standards for calibration. Surrogate recoveries and the internal standard response should be routinely monitored as continuing checks on instrument performance, calibration curves and overall method performance. The Analytical Methods This manual includes seven methods for synthetic organic chemicals and two methods for chlorination disinfection byproducts. In general, the analytes may by classified as nonvolatile and three of the methods employ separation by high performance liquid chromatography (HPLC). The remainder utilize capillary column gas chromatography (GC). Two of the methods use convenient liquid-solid extraction (LSE) methods for analyte isolation, and two others offer LSE as an option. By contrast to the original manual, four of the methods are for single analytes - 2,3,7,8tetrachlorobenzo-p-dioxin, glyphosate, endothall and diquat. These analytes are not readily amenable to generic methods. Each method provides an adequate summary statement. Some additional comments are germane here. Method 506 for phthalates and adipates offers both liquid-liquid extraction (LLE) and LSE options. After capillary column GC separation, a photoionization detector is required for detection and MDL's are limited to approximately 10 g/L. Phthalates and adipates are among the most common contaminants encountered in the laboratory and extreme care must be taken to ensure clean reagent blanks. Dioxin may be an extremely toxic chemical and water concentrations of a few parts per trillion (pg/L) are of concern. In addition to extreme sensitivity, unambiguous identification is an analytical requirement. Thus, Method 513 is an inherently complex method, which employs LLE or LSE, extract cleanup, a sample concentration factor of 105, capillary column GC separation and analysis by high resolution mass spectrometry. In addition, labeled isotopes of dioxin are employed as surrogate analyte and internal standard to aid in identification and quantitation and to compensate for analyte losses during the complex sample handling procedure. Methods 547, 548 and 549 are single analyte procedures for glyphosate, endothall and diquat. Paraquat is a non-regulated ionic herbicide quite similar to diquat and may be analyzed simultaneously. These may be characterized as difficult analytes because of their high water solubility and low volatility. In addition, glyphosate and endothall require derivatization prior to detection. Glyphosate is analyzed by direct aqueous HPLC injection and undergoes post-column derivatization prior to fluorescence detection. Endothall must be transferred from the aqueous phase to an acetic acid matrix for derivatization, followed by analysis by GC with electron capture detection (ECD). As with glyphosate, no preconcentration factor is involved. Method 549 provides for the extraction and concentration of diquat and paraquat in the base forms by LSE with a C-8 cartridge, preconditioned to operate in the reverse phase mode. The analytes are eluted with an acidic solvent and, after addition of ion-pairing reagent, are separated by HPLC. The analytes are detected by ultraviolet absorption (UV) with confirmation provided by a photodiode array spectrometer. Methods 550 and 550.1 provide HPLC alternatives for polycyclic aromatic hydrocarbons. Method 550 employs a conventional serial LLE approach while 550.1 uses a LSE procedure similar to Method 525. Dual UV and fluorescence detectors are employed, with considerably lower MDL's reported for the latter. Halogenated organic byproducts, other than the regulated trihalomethanes, account for most of the total organic halogen formed by the chlorination of water supplies. The most important classes in terms of occurrence are the neutral analytes of Method 551 and the haloacetic acids of Method 552. Method 551 is quite similar to Method 504, employing a simple one step LLE and direct injection of the extract into a capillary GC with ECD detection. The haloacetic method is a serial LLE with analysis by GC-ECD and is quite similar to, but simpler than, Method 515.1 for acid herbicides. Both employ diazomethane for methylation with a micromolar generation procedure, which avoids the hazards associated with handling concentrated diazomethane. These two methods are unique in that significant background concentrations will always be present in chlorinated http://www.epa.gov/nerlcwww/methmans.html#organics_supp_ii[8.12.2010 19:05:46] 524. Environmental Protection Agency Cincinnati. Address your request for this manual to NTIS and ask for their order number PB92-207703.12. these background levels must be taken into account when deciding upon fortification concentrations. replace older versions of these methods. Five of the methods in this manual.2 and Method 552. 554 and 555. 524. or potential candidates for regulation.2. as called for in the quality assurance section. 549.00.1.2. Three are new methods for the determination of semivolatile compounds: Method 554 for ozonation disinfection by-products. and Method 553 for nonvolatile compounds using particle beam HPLC/MS. Ohio 45268 EPA-600/R-92/129 AUGUST 1992 This manual is available from NTIS and contains Methods 515. When determining fortified matrix recoveries as required in the quality assurance (QA) section. 524. 552. and appeared in either of two previous organic methods manuals. To the: Chemical Exposure Research Branch Top of page Methods for the Determination of Organic Compounds in Drinking Water Supplement II Environmental Monitoring Systems Laboratory Office of Research and Development U. respectively.1. The older versions were numbered 515.2 and 524. 548. to improve method performance and reduce the use of organic solvents.epa. designated for regulation by the Office of Ground Water and Drinking Water in the near future.html#organics_supp_ii[8.1.0 iii iv vi vii 1 5 http://www.2 Foreword Abstract Acknowledgment Analyte . 549.2 are published in Supplement III which is described below. In addition.0.0.gov/nerlcwww/methmans. Abstract Eight analytical methods covering 133 organic contaminants which may be present in drinking water or drinking water sources are described in detail. 548. and 552. Methods 515.2 Revision 4. the uncertainty in measuring the background level should be considered when establishing control limits. Table of Contents Method Number 524.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA supplies. and 552. These methods will give the laboratory analyst the capability to accurately and precisely determine organic compounds that are currently regulated in drinking water. Method 555 for phenoxyacid herbicides using the novel approach of in-line extraction/high performance liquid chromatography (HPLC). the cost is $55. such as liquid-solid extraction.1. Please note that revised versions of Methods 515.1.2.1. 548.Method Cross Reference Introduction Measurement of Purgeable Organic Compounds in Water by Capillary Column Title Revision Page 4. 549.1.S.2010 19:05:46] . The new versions employ new analytical techniques. 553.2 Revision 3. 2.0 With a Photodiode Array Ultraviolet Detector Analyte .gov/nerlcwww/methmans.0 213 555 Determination of Chlorinated Acids in Water by High Performance Liquid Chromatography 1.html#organics_supp_ii[8.0 143 553 1.0 Methylation Gas Chromatography/Mass Spectrometry Determination of Diquat and Paraquat in Drinking Water by Liquid-Solid Extraction and HPLC with Ultraviolet Detection Determination of Haloacetic Acids and Dalapon in Drinking Water by Ion Exchange Liquid-Solid Extraction and Gas Chromatography With Electron Capture Detection Determination of Benzidines and NitrogenContaining Pesticides in Water by LiquidLiquid Extraction or Liquid-Solid Extraction and Reverse Phase High Performance Liquid Chromatography/Particle Beam/Mass Spectrometry Determination of Carbonyl Compounds in Drinking Water by DNPH Derivatization and High Performance Liquid Chromatography 1.0 51 548.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Gas Chromatography/Mass Spectrometry 515.1 119 552.1 Determination of Endothall in Drinking Water by Ion Exchange Extraction. Acidic Methanol.2010 19:05:46] .2 515.12.2 Determination of Chlorinated Acids in Water Using Liquid-Solid Extraction and Gas Chromatography With an Electron Capture Detector 1.0 89 549.1 1.1 173 554 1. 555 524. 554 524.2.2 524.2 515.epa. 1. 555 237 http://www.Method Cross Reference Analyte Acetaldehyde Acetone Acifluorofen Acrylonitrile Allyl chloride Bentazon Method No. 2 524.2 553 524.2 524.2 524.2 524.1 515.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Benzene Benzidine Benzoylprop ethyl Bromobenzene Bromochloroacetic acid Bromochloromethane Bromodichlorobenzene Bromoform Bromomethane Butanal 2-Butanone n-Butylbenzene sec-Butylbenzene tert-Butylbenzene Carbaryl Carbon disulfide Carbon tetrachloride Chloramben Chloroacetonitrile Chlorobenzene 1-Chlorobutane Chloroethane Chloroform Chloromethane 2-Chlorotoluene 4-Chlorotoluene Crotonaldehyde Cyclohexanone Dalapon DCPA (Dacthal) and metabolites Decanal 524.2 524.2.2010 19:05:46] . 555 524.2 553 553 524.2 524.2 524.12.epa.2 552.2.2 524. 555 554 http://www.2 524.2 554 524.html#organics_supp_ii[8.1 524.2 524.2 524.2 554 554 552.2 515.2 524.gov/nerlcwww/methmans.2 524.2 524. 5-Dichlorobenzoic acid 2.3-Dichloropropane 2.2 524.2 524.2.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Dibromoacetic acid Dibromochloromethane 1.4dichlorophenoxyacetic acid) 1.1-Dichloropropanone cis-1.2.1-Dichloropropene 1.2 524. 555 524.epa.2-Dibromo-3chloropropane 1.2 524.2 524.2 515.2 515.2-Dichloroethene 2.1 524. 555 515.html#organics_supp_ii[8.1-Dichloroethene cis-1.2 524.3- 552.4-Dichloro-2butene Dichlorodifluoromethane 1.2-Dichloroethane 1.2 524.2010 19:05:46] .2 524.2.2 524.2 524.3'-Dichlorobenzidine 3.2 524.2 524.3-Dichlorobenzene 1.2-Dichloropropane 1. 555 552.12.1-Dichloroethane 1.2 553 515.2.2-Dichlorobenzene 1.4-DB (2.3-Dichloropropene trans-1. 555 524.2 524.2-Dibromoethane Dibromomethane Dicamba Dichloroacetic acid 1.4-Dichlorobenzene 3.2-Dichloroethene trans-1.gov/nerlcwww/methmans.2 http://www.4dichlorobutanoic acid) trans-1.2 524.4-D (2.1 524.2 524.2 524.2-Dichloropropane 1.2 524. 2 554 554 524.1 http://www.2 524.2 554 524. 555 524.2010 19:05:46] .1 552.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Dichloropropene Dichlorprop Diethyl ether 3.2 524.2 515.2 553 553 515.2 524.2.2.2 524.2 524.2 553 524.2 524.epa.2 524.2.1 553 548. 555 524.gov/nerlcwww/methmans.html#organics_supp_ii[8.3'-Dimethylbenzidine Dinoseb Diquat Diuron Endothall Ethylbenzene Ethyl methacrylate Formaldehyde Heptanal Hexachlorobutadiene Hexachloroethane Hexanal 2-Hexanone 5-Hydroxydicamba Isopropylbenzene 4-Isopropyltoluene Linuron (Lorox) Methacrylonitrile Methylacrylate Methylene chloride Methyl iodide Methylmethacrylate 4-Methyl-2-pentanone Methyl-t-butyl ether Monobromoacetic acid Monochloroacetic acid 515.12.2 552. 555 549.2 524.3'-Dimethoxybenzidine 3.1 524.2 524. 2 554 554 549.1.epa.1. 555 524.2 553 553 515.2010 19:05:46] .2 1.2 http://www.2.2 515.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Monuron Naphthalene Nitrobenzene 4-Nitrophenol 2-Nitropropane Nonanal Octanal Paraquat Pentachloroethane Pentachlorophenol (PCP) Pentanal Picloram Propanal Propionitrile n-Propylbenzene Rotenone Siduron 2.2 524.2 524.2 524.2.12.4.2 552.1 524.1.2 524.2 Tetrahydrofuran Toluene Trichloroacetic acid 1. 555 524.html#organics_supp_ii[8.1.2 1.2.2 524.1 524.1-Trichloroethane 1.2 524. 555 554 524.1.2 524.2.2.2.2 524.2-Tetrachloroethane 524.gov/nerlcwww/methmans.5-TP (silvex) Styrene Tetrachloroethene 553 524. 555 554 515.4-Trichlorobenzene Trichloroethene 1.2 515.2.3-Trichlorobenzene 1.2-Tetrachloroethane 524.2-Trichloroethane 524. 5-Trimethylbenzene Vinyl chloride m-Xylene o-Xylene p-Xylene 524.2 515.2 524.5trichlorophenoxyacetic acid) 1.3.2 524. 555 524.4. This manual provides eight analytical methods for 133 organic contaminants. originally scheduled for regulation by June 19. Eichelberger U. http://www." EPA/600/4-88/039. and the determination of the efficacy of various water treatment approaches.gov/nerlcwww/methmans. S.epa. health effects studies.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Trichlorofluoromethane 2.4. Efforts have been made to provide a manual that is consistent with the earlier versions. which may be present in drinking water or drinking water sources.2 Introduction James W. In addition.2 524. EPA published "METHODS FOR THE DETERMINATION OF ORGANIC COMPOUNDS IN DRINKING WATER. when adequate analytical methodology is not available. to propose 25 more of these by January 1988 for subsequent regulation. Regulatory Background Analytical methodology for monitoring water quality serves a number of related purposes.2 524. The amended Act also required EPA to develop a priority list of additional contaminants. form the supporting basis for water quality regulations. Environmental Protection Agency An integral component of the role of the Environmental Protection Agency (EPA) in protecting the quality of the Nation's water resources is the provision of means for monitoring water quality.2.html#organics_supp_ii[8. EPA develops and disseminates analytical methods for measuring chemical and physical parameters affecting water quality. including chemical contaminants that may have potential adverse effects upon human health. This original manual was revised and reprinted in July 1991.2 524. in turn. This manual is a second supplement to the July 1991 revision of the earlier 1988 manual. containing nine methods to determine 54 compounds. and the support of these regulations is the ultimate purpose of the analytical methods. The Act requires EPA to promulgate regulations for drinking water contaminants that may cause adverse health effects and which are known or anticipated to occur in public water systems. The 1986 amendments require regulations to include Maximum Contaminant Levels (MCLs) with compliance determined by regulatory monitoring or by the application of an appropriate treatment.2010 19:05:46] . a manual containing 13 methods for approximately 200 potential drinking water contaminants. In December 1988. and to continue this process by the addition of 25 from the priority list on a triennial basis thereafter.2. including occurrence studies in community water systems.2.2 524. the 1986 amendments specified 83 contaminants.4-Trimethylbenzene 1. This manual provides methods to determine analytes that appear at a later time in the regulatory framework. 1989. Supplement I. Limitations on the levels of specific contaminants are codified in proposed and promulgated Federal regulations developed in response to the Safe Drinking Water Act (SDWA) of 1974 and the SDWA amendments of 1986.5-T (2. and technology that supports the EPA Pollution Prevention Policy. was published in July 1990.3-Trichloropropane 1. In keeping with this role.12. These activities. Supplement I provides analytical methods for many of the remaining contaminants on the original list of 83: namely. EPA will quickly approve the new versions of these five methods. or "Methods for the Determination of Organic Compounds in Drinking Water .1.2 Revision 4. which are cast in the same terminology as the December 1988 manual.Cincinnati). This group included six compounds which.0. and appeared in either of the two previously published organic methods manuals ("Methods for the Determination of Organic Compounds in Drinking Water. and 6 other organics from the list of 83 was promulgated on July 17. These methods utilize new sample preparation technology such as disk or cartridge liquid-solid extraction. Phase V of EPA regulations for 3 volatile compounds. July 1990.0. 1992. sample matrices. endothall. Where feasible. by authority of provisions in the 1986 amendments.. 502. 503. routine analyses of reagent blanks.12. or use new relatively harmless methylating reagents. the older versions should be retained for compliance purposes.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Of the original 83 pollutants.1.html#organics_supp_ii[8. and 552. 9 pesticides. 10 volatile compounds and 20 pesticide and related compounds. analytical methods for all 30 compounds are by the VOC methods above or SOC methods also included in the 1988 manual. heptachlor. Analytical methods for these eight as well as other unregulated VOCs were published in the December 1988 manual (EPA Methods 502. Method 554 for ozonation disinfection by-products. The MDLs provided were determined by replicate analyses of fortified reagent water over a relatively short period of time. http://www. The Analytical Methods This manual contains eight methods. December 1988. are assembled in the format recommended by the Agency's Environmental Monitoring Management Council (EMMC). 549. requiring no other source material for application.2.2. nevertheless. surrogate analytes have been included in the methods as well as internal standards for calibration. calibration curves and overall method performance.g. 524. aldicarb sulfone. diquat.epa. heptachlor epoxide and styrene. In particular. The older versions were numbered 515. directly support the Environmental Protection Agency's Policy on Pollution Prevention. The methods are designed primarily for drinking water and drinking water sources. e. were substituted into the original list of 83 in January 1988 (53 FR 1892): namely.2010 19:05:46] . Environmental Monitoring Systems Laboratory . General Comments Supplement II provides methods.1 replace older versions of these methods. aldicarb sulfoxide. phthalates and dioxin.1 and 524. the July 1991 revision. and calibration and quality control samples. and Method 555 for phenoxyacetic acid herbicides using the novel approach of in-line liquid-solid extraction and high performance liquid chromatography. the analyses of field reagent blanks. The remaining three are new methods for the determination of semivolatile or nonvolatile compounds: Method 553 for nonvolatile organics using a high performance liquid chromatograph interfaced to a mass spectrometer through a particle beam interface. However. As such. Methods 515. Thus. analyses of fortified reagent blanks and fortified matrix samples. The Environmental Protection Agency's Office of Ground Water and Drinking Water believes that only one version of any analytical method should be approved for compliance with drinking water regulations. therefore. 549. regulations for eight volatile organic chemicals (VOCs) were promulgated in June 1987 (see 52 FR 25690 and 51 FR 11396). these methods are written in standardized terminology in a stand-alone format. The methods in this manual. With the exception of lindane. were finalized and published in January 1991." EPA/600/4-90/020. adipates.1. Until these methods are promulgated by EPA. 524. 524.gov/nerlcwww/methmans. instrument control samples and performance evaluation samples.2 Revision 3.Supplement I. Regulations for 30 organic chemicals. 548. glyphosate.1. method detection limits (MDLs).initial demonstration of performance. these are somewhat idealized limits. 548. ethylbenzene. unlike previous manuals. Surrogate recoveries and the internal standard response should be routinely monitored as continuing checks on instrument performance. and Supplement I. revised July 1991. These same comments apply herein. Reporting limits for reliable quantitative data may be considerably higher. and analyses of quality control (QC) samples.2). some performance data are included for more complex matrices such as wastewater. and 552 respectively. polycyclic aromatic hydrocarbons (PAHs). The quality control sections are uniform and contain minimum requirements for operating a reliable monitoring program -.1." EPA/600/4-88/039. The introductions to the earlier manuals discuss general method features on format. Other QC practices are recommended and may be adopted to meet the particular needs of monitoring programs. provide a useful index of method performance. A flame ionization detector may be used if a second dissimilar column is used for corroboration. Dalapon. This method utilizes a new liquid-solid disk extraction procedure.12. in-line concentration of the analytes on a concentrator column. The disk extraction replaces the cumbersome liquid-liquid extraction and the Florisil cleanup in Method 515.1 is a liquid-solid extraction method to determine haloacetic acid disinfection byproducts and the chemically similar chlorinated herbicide. Method 549. Initial studies were conducted to evaluate 48 candidate VOCs of environmental interest for possible inclusion into this method. aldicarb sulfone regulated in January 1991 and carbofuran regulated in May 1992. This compound is now determined using Method 552. a method analyte in Method 515. and still require the use of the stronger reagent. water soluble compounds which are very difficult to remove from the water matrix.2010 19:05:46] . MDLs for these newly added compounds are generally 1 g/L or lower. MDLs for the analytes in this method range from 3 to 69 g/L. Method 515. This method utilizes a new extraction approach. Dimethyl endothall is then identified and measured with gas chromatography/mass spectrometry (GC/MS).2. These carbonyl compounds are either known or suspected disinfection by-products from the ozonation disinfecting process.1 and 515.gov/nerlcwww/methmans. This method also utilizes cartridge liquid-solid extraction technology in support of the Agency's Pollution Prevention Policy. bringing the total number of method analytes to 84 compounds.1 is an improvement over the existing Method 549 in that it now utilizes liquid-solid disk extractions in addition to the cartridges. This method was designed as a simplified alternative to the cumbersome Method 552 which employs liquid-liquid extraction. Method 553 is a new method for the determination of nonvolatile organic compounds.1. Some of the phenolic herbicides are very difficult to derivatize.2.0 contains 24 new target analytes. The expanded liquid-solid extraction technology significantly reduces the amount of organic solvent required to carry out the extraction. and to the possibility of a diazomethane explosion. Using less potentially harmful solvents directly supports the Environmental Protection Agency's Policy on Pollution Prevention in the laboratory. Among the compounds on the analyte list for this method are two regulated compounds.1 is an improved method for the determination of endothall and is intended to replace the older Method 548. This method provides a much superior technique for Dalapon over the complex herbicide procedure described in Method 515. which are marked in the analyte list with an asterisk. The entire amount of herbicide contained in a 20-mL sample aliquot is introduced into the analytical system giving the method the needed sensitivity. in water. is no longer a method analyte in this new method. and the analytes are methylated directly in the eluant using acidic methanol instead of diazomethane. Comparable MDLs below a part per billion are achieved with both disks and cartridges. Method 552.1. Method 555 is a new method utilizing HPLC with a conventional photodiode array HPLC detector to determine the same chlorinated herbicides on the analyte lists in Methods 515. This method utilizes an intermediate strength amine anion exchange sorbent to extract the endothall from a 100 mL sample aliquot. Revision 4.2. This method directly supports the Pollution Prevention Policy. including benzidines and nitrogen containing pesticides. Method 548.epa.1. These candidate compounds included many polar.1 has a MDL approximately ten times lower than the older 548. http://www. and completely eliminates the possible exposure of the analyst to harmful extracting solvent vapors. This method requires no derivatization procedure which completely eliminates the need for diazomethane or even acidic methanol. diazomethane. Method 548. Method 554 is a new HPLC method optimized for the determination of selected carbonyl compounds in finished drinking water and raw source water. in water. This new technology provides the analyst the ability to determine a large.html#organics_supp_ii[8.2 is an improved method to determine chlorinated herbicides in water. Results indicated that only 24 of these candidates were stable in water over a 14-day holding time and could be efficiently purged and trapped from water with acceptable accuracy and precision. This method employs reverse phase high performance liquid chromatography (HPLC) interfaced to a mass spectrometer through a particle beam interface. The sample is extracted with a miniature anion exchange column. dalapon. MDLs using this method for matrices which pose no analyte losses due to matrix effects are generally 1 g/L or lower. new scope of nonvolatiles heretofore extremely difficult or impossible to determine in a water matrix. and forms the dimethyl derivative quickly and easily using acidic methanol as the methylating reagent.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Method 524. which requires only the HPLC mobile phase as the extracting solvent. 00. Two methods utilize a mass spectrometer for the unambiguous identification and measurement of the compounds separated by high resolution GC. 551. 524. 515.Method Cross Reference Introduction Volatile Organic Compounds in Water by Purge and Trap Capillary Column Gas Chromatography with Photoionization and Electrolytic Conductivity Detectors in Series Title Revision Page 2.1 and 552.epa. Abstract Fifteen analytical methods for organic compounds in drinking water are documented in detail.1. Essentially all of the major chlorine disinfection by-products that have been identified in drinking water are included in the methods in this manual. 506.2.1. and editorial improvements to the previously published analytical methods. 507.2.1.2 Foreword Abstract Acknowledgment Analyte .gov/nerlcwww/methmans. 509. 525. Most methods have also been multilaboratory validated although not all possible analytes have been included in these studies. The versions in Supplement III provide corrections. 508. 508. Environmental Protection Agency Cincinnati. 531.html#organics_supp_ii[8. 505. Fourteen of the fifteen methods utilize high resolution gas chromatography (GC) for separation of analytes from each other and from other substances in the water sample. Table of Contents Method Number 502.12.2.S. 504. the cost is $67. Address your request for this manual to NTIS and ask for their order number PB95-261616. minor technical enhancements. One method employs high performance reverse phase liquid chromatography for the separation.2.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA To the: Chemical Exposure Research Branch Top of page Methods for the Determination of Organic Compounds in Drinking Water Supplement III National Exposure Research Laboratory Office of Research and Development U. Several previously distributed but not formally published methods are also included. Ohio 45268 EPA-600/R-95/131 August 1995 This manual is available from NTIS and contains Methods 502. Most of these methods were published as prior versions in other methods manuals in this series.1.2010 19:05:46] .1 iii iv vii viii 1 http://www. 515.2. These two methods are extremely versatile and have been single-laboratory validated for a total of 194 individual compounds and 8 commercial product mixtures. 0 509 1.1 4.html#organics_supp_ii[8.gov/nerlcwww/methmans.2 4. and 1.1 506 Determination of Phthalate and Adipate Esters in Drinking Water by Liquid-Liquid Extraction or Liquid-Solid Extraction and Gas 1.epa. and Organohalides by LiquidSolid Extraction and Electron Capture Gas Chromatography Determination of Ethylene Thiourea (ETU) in Water using Gas Chromatography with a Nitrogen-Phosphorus Detector Determination of Chlorinated Acids in Water by Gas Chromatography with an Electron Capture Detector Determination of Chlorinated Acids in Water using Liquid-Solid Extraction and Gas Chromatography with an Electron Capture Detector Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry Measurement of N-Methylcarbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post Column 3.12.2010 19:05:46] .0 531.1 515.1 507 508 508.2.1 3.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 504.1 515.and PhosphorusContaining Pesticides in Water by Gas 2.1 Chromatography with Photoionization Detection Determination of Nitrogen.1 525.2-Dibromoethane (EDB).1 524.1 Chromatography with a Nitrogen-Phosphorus Detector Determination of Chlorinated Pesticides in Water by Gas Chromatography with an Electron Capture Detector Determination of Chlorinated Pesticides.1 http://www. 1. Herbicides.1 1.2 1.2-Dibromo-3Chloro-propane (DBCP).2 2.3Trichloropropane (123TCP) in Water by Microextraction and Gas Chromatography Analysis of Organohalide Pesticides and Commercial Polychlorinated Biphenyl (PCB) Products in Water by Microextraction and Gas Chromatography 1.1 2.1 505 2. 515.2 507.1. 507. 507. 551.0 552.1 531.1 1. and Halogenated Pesticides/Herbicides in Drinking Water by Liquid-Liquid Extraction and Gas Chromatography with ElectronCapture Detection Determination of Haloacetic Acids and Dalapon in Drinking Water by Liquid-Liquid Extraction.gov/nerlcwww/methmans.2 507.2. Derivatization and Gas Chromatography with Electron Capture Detection Analyte .2 505.1. 525.2 525.1.1 531. 525.0 http://www.1 505.2 515.html#organics_supp_ii[8.1 531.2 524.2 505.Method Cross Reference Analyte Acenaphthylene Acetone Acifluorfen Acrylonitrile Alachlor Aldicarb Aldicarb sulfone Aldicarb sulfoxide Aldrin Allyl chloride Ametryn Anthracene Atraton Atrazine Method No.1 551.525.2 1. 525.2010 19:05:46] .12. 525.2 524. 508. 551. 525.epa.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Derivatization Determination of Chlorination Disinfection Byproducts. 508. 508. 508. Chlorinated Solvents.1.2.2 524. .2 507. 525.2.2010 19:05:46] 531.2 525.2 551.2.1 552.h. 524.2.2.gov/nerlcwww/methmans.1 515.2 506 506 502. 551.1 552.2.2 502.epa.i]perylene Bis (2-ethylhexyl) phthalate Bis (2-ethylhexyl) adipate Bromobenzene Bromacil Bromochloroacetic acid Bromochloroacetonitrile Bromochloromethane Bromodichloroacetic acid Bromodichloromethane Bromoform Bromomethane Butachlor 2-Butanone Butylate Butylbenzylphthalate http://www.html#organics_supp_ii[8.1 502.2 525. 525. 524.1 502. 524.2 525.2 502. 515.12.2 506.2 507.2 525. 551.2 524.2 502. 508.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Baygon Bentazon Benzene Benz[a]anthracene Benzo[b]fluoranthene Benzo[k]fluoranthene Benzo[a]pyrene Benzo[g. 524.1. 524. 525.2 507. 524.1.2.2. 551.2.2 525.2. 508.2. 508. 508 505. 508.2 502.2.2 531. 524.2 531.1. Gamma-chlordane Trans nonachlor Chloroacetonitrile Chlorobenzene Chlorobenzilate 2-Chlorobiphenyl Chlorodibromoacetic acid 1-Chlorobutane Chloroethane Chloroform http://www.2010 19:05:46] . 525.2 552.2 502. 524.1. 525.2.2 502.2 524.1 507. 524.1 551.2 502. 508.1 515.2 n-Butylbenzene sec-Butylbenzene tert-Butylbenzene Carbaryl Carboxin Carbofuran Carbon disulfide Carbon tetrachloride Chloramben Chloral Hydrate Chlordane Alpha-chlordane 502.2 502.2 525.2. 524. 525.html#organics_supp_ii[8.gov/nerlcwww/methmans.12.1. 551. 525.2.2 525.1 524. 508.2.2 502.epa.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 525.2 524.2.2 505.2.1 505. 524.2 508. 524. 524.2. 515.1 508.2.2 508. 515.2 551.2 525. 508.1. 524. 515.2 515.1 507. 525.2 508. 525.2.1. 525.2 507.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 551.1. 551.2 525.html#organics_supp_ii[8.2 508.2 502.1 Chloromethane Chloroneb Chloropicrin Chlorothalonil 2-Chlorotoluene 4-Chlorotoluene Chlorpropham Chlorpyrifos Chrysene Cyanazine Cycloate Dacthal(DCPA) 2.1. 515.epa. 525. 508.12.1 508.2010 19:05:46] . 525.2.2 515.2. 508.2 508.2 525. 508.4'-DDD 4. 552.1.1.1.1. 508.4-D Dalapon 2.2.4-DB DCPA acid metabolites 502.1.4'-DDE http://www. 524.2 515.2 502. 525. 524.gov/nerlcwww/methmans. 525.2 4. 1 502. 524.2.1 502.2 502. 524.1.2. 551.4'-DDT Diazinon Dibenz[a.1-Dichloroethane 1.5-Dichlorobenzoic acid trans-1.2.epa.1.12.2 552.2 525. 525.2 524.2.2 515. 515.2.2. 515. 1.2 551.2.4-Dichlorobenzene 3. 504. 551.2-Dibromoethane Dibromomethane Dicamba Dichloroacetic acid Dichloroacetonitrile 1.2 507. 504.1.2 502.2.3-Dichlorobenzene 1.2 502.4-Dichloro-2butene 1.1 502.1. 525.1 502.2.2 551.2 502.2. 524.2.2-Dichlorobenzene 1.h]anthracene Dibromoacetic acid Dibromoacetonitrile Dibromochloromethane 508.2.2 515.2-Dichloroethane http://www.html#organics_supp_ii[8. 524. 524.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 4.2-Dibromo-3chloropropane 1.2 502. 551.1. 524.2.2010 19:05:46] . 524.gov/nerlcwww/methmans. 524. 508.2 552.1 502. 524. 2 506. 508.2. 524.2. 524.2-Dichloropropane 1.3-Dichlorobiphenyl Dichlorvos Dieldrin Diethyl ether Diethyl phthalate Di(2-ethylhexyl)adipate Di(2-ethylhexyl)phthalate 524.2 502.2 524.gov/nerlcwww/methmans.1-Dichloro-2-propanone Dichloroprop Di-n-butyl phthalate Di-n-octyl phthalate 2. 515.2. 524. 524.2 506 525.2.2 502. 524.2 502.2 524.1-Dichloropropanone cis-1.2 525.1. 525. http://www.3-Dichloropropene trans-1.2-Dichloroethene trans-1.2 502.2 502.html#organics_supp_ii[8.2.2 507.2 551. 524.1-Dichloroethene cis-1. 525. 525.2 502.12. 524.2.2 502.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 1.2 506.3-Dichloropropene 1.2 502.2 525.1.2 502. 525.2. 508.2.2 506.2 505.2-Dichloropropane 1.2010 19:05:46] .2-Dichloroethene Dichlorodifluoromethane 1. 524. 524.epa.3-Dichloropropane 2.1-Dichloropropene 1.1 515.2. 551. 508.1. 524.2 507. 525.1. 525.2.1 507. 515.1. 525.1 551.2.2.12.2 507.1. 508.2010 19:05:46] . 525. 508. 525.2 507.2 515. 551.1 508.2 505.2 508. 508.2 507.6-Dinitrotoluene Dinoseb Diphenamid Disulfoton Disulfoton sulfone Disulfoton sulfoxide Endosulfan I 525.2 508.1.2 502.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Dimethyl phthalate 2. 508.2 509 Endosulfan II Endosulfan sulfate Endrin Endrin aldehyde Endrin ketone EPTC Ethoprop Ethylbenzene Ethyl methacrylate Ethylene thiourea http://www.2 507. 508. 525.html#organics_supp_ii[8. 525. 525.2 525.2 524. 525.epa.2 508. 525.1.2 525. 525.4-Dinitrotoluene 2.gov/nerlcwww/methmans. 2 525.4'.3. 508.1.2 http://www.gov/nerlcwww/methmans.3'.2010 19:05:46] .5.1 525.2 525.1. 525.2'.2 Hexachlorocyclopentadiene 525.2 507. 525.2.6Heptachlorobiphenyl Hexachlorobenzene Hexachlorobutadiene 505.html#organics_supp_ii[8.6'Hexachlorobiphenyl Hexachlorocyclohexane. 551.2 525.4.12.1 502. 508. 508.2 507. 525. 508.2 505. 551. 525. 551. 551. 525.2 525.2 524.1.1.4'. 508. alpha Hexachlorocyclohexane.epa. 508.2 507.2.2 Heptachlor Heptachlor Epoxide 2.1 505.2.2'.2 Hexachloroethane 2-Hexanone 524. Hexachlorocyclopentadiene 508. 524. beta Hexachlorocyclohexane. 508.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Etridiazole Fenamiphos Fenarimol Fluorene Fluridone 508.4.2.1. delta 525. 525. 525.2 505.1 2. 3.2 524.2 525.1 531.d]pyrene Isophorone Isopropylbenzene 4-Isopropyltoluene Lindane (gamma-BHC) Merphos Methacrylonitrile Methiocarb Methomyl Methoxychlor Methylacrylate Methylene chloride Methyl iodide Methylmethacrylate Methyl paraoxon 4-Methyl-2-pentanone 507.html#organics_supp_ii[8.2 http://www. 508. 508.2.2010 19:05:46] . 524.2 524. 525.2 502.1 508. 508. 525.2 507.2 524.2.1 508.12.1 508. 525.1. 525. 508.2.2. 508.1 524.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Hexazinone HCH-alpha HCH-beta HCH-delta HCH-gamma (lindane) 3-Hydroxycarbofuran 5-Hydroxydicamba Indeno[1. 551.2 508.2 505.epa.2 502.1 507.2 525.1 505.1 515. 515. 524.1. 508.2 524.2 531.2.1 531.c.2 524. 525.gov/nerlcwww/methmans. 551. 2010 19:05:46] .2 524.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Methyl-t-butyl-ether Metolachlor 524.epa.1.6Pentachlorobiphenyl Pentachloroethane Pentachlorophenol http://www.1 507.2 524.2 525. 525.2.1 524. 551.2'.2 515. 525.12.3'. 525.2'.2 507. Metribuzin Mevinphos MGK 264 Molinate Monobromoacetic acid Monochloroacetic acid Naphthalene Napropamide Nitrobenzene 4-Nitrophenol 2-Nitropropane cis-Nonachlor Norflurazon 2.html#organics_supp_ii[8.1.2 507.5'. 515. 525. 508.2 515.2 552. 525.3'.2 508.3. 525.2 507. 551. 524.2 531.6'Octachlorobiphenyl Oxamyl Pebulate 2.2 552. 508.gov/nerlcwww/methmans.1 507.4.2. 525.2 505 507.2 507. 525.2 525.2.2.2 502.1.6.4. 525.1 507. 508. 525.2 507. 525. 515.1.1. 525. 515.2 524. 525.2 502.html#organics_supp_ii[8. 525.2 515. 525.2 525.2 507. 525. 525.2 507.1.2 524.5-TP Tebuthiuron Terbacil http://www.2 525.4.1. 507.2 507.1. 525.2 515.1.1. 515.12.2010 19:05:46] .gov/nerlcwww/methmans.2 515.2 502.2 507.2. 508.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA cis-Permethrin 508.2 508. 524.4. 508. 525.2 507.2 505. 525.2 508.2 507.5-T 2. Trans-Permethrin Phenanthrene Picloram Prometon Prometryn Pronamide Propachlor Propazine Propionitrile Propylbenzene n-Propylbenzene Pyrene Simazine Simetryn Stirofos Styrene 2.epa.2 507. 1 505.2.1 502.1.1.2 507.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 525.2.2. 525.2.12.4-Trichlorobenzene 1. 524.2 552.1 505. 524.4.2.2 551.1 524.1.1-Trichloroethane 507. http://www. 524.html#organics_supp_ii[8.2010 19:05:46] 1. 508.1. 508.2-Tetrachloroethane 1.2.3-Trichlorobenzene 1.2.2.1.2 Terbufos Terbutryn 2.2 502.2.2 505.2-Tetrachloroethane Tetrachloroethene Tetrachloroethylene Tetrahydrofuran Toluene Toxaphene Triademefon Tribromoacetic acid Trichloroacetic acid Trichloroacetonitrile 1.2 551.2 551. 551.2 505.2 502.2.1. 525.2 502.gov/nerlcwww/methmans.2.1 502.2 507. 551.2.2 552.2 525. 524. 525.2. 524. 524.epa. 524.2 502.2'.4'Tetrachlorobiphenyl 1. 524.2.2 502. 524. 525.2.2-Trichloroethane Trichloroethene Trichloroethylene . 2 508.1.4. 508.2 507. 508.1 502. 524.1 502. 524. 551.2 505.3-Trichloropropane 2.2 502. 524.1.2 505.2.2 551.2 505. 525.2 502.1-Trichloro-2propanone 1.4-Trimethylbenzene 1.12. 525.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Trichlorofluoromethane 1. 525. 508.1.1.1.2.2 502.html#organics_supp_ii[8. 524.2.2. 524.2. 525.2. 524.2 505.2 505.2.1. 524.2 Trifluralin 1.2.5-Trimethylbenzene Vernolate Vinyl chloride 0-Xylene m-Xylene p-Xylene Aroclor 1016 Aroclor 1221 Aroclor 1232 Aroclor 1242 http://www.1 504. 508.5-Trichlorobiphenyl Tricyclazole 524.2. 525.3. 525. 525.2 502.epa. 508.2. 508. 508. 508. 508.2010 19:05:46] .1. 525.2 507. 551.2.gov/nerlcwww/methmans. photocopied.2 Aroclor 1254 Aroclor 1260 Introduction William L. While the title of supplement III. EPA/600/R-94/173. these methods will very likely be applicable to other aqueous matrices including surface water. and used without loss of information. ground water. and waste water. and dates if they are known.1. S. The purpose of this very brief method history is to assist users who may have older versions in their files in understanding the chronological relationship of methods as technical improvements were made over the years. each method may be removed from the manual.2010 19:05:46] . http://www. Environmental Protection Agency at the time of their contributions. that is. in which both phases of the equilibrium partition process are named. 508. However since some methods have been tested with only reagent water and/or drinking water. The cover page of each method gives the title. method number. is used throughout the manual in place of the misleading commercial term "solid phase extraction".1. 525.2 which has been tested in a large multi-laboratory validation study with a variety of aqueous matrices. Some methods in supplement III utilize the liquid-solid extraction technology which was pioneered by the USEPA in the original Method 525 in 1988. 525. 508. Unless otherwise indicated. 508. each of the methods in Supplement III was intended to stand alone.1. and date.2 505. but the authors believe that the added bulk of the methods is a small price to pay for the flexibility of the format. Budde and Jean W.2 505. previous authors. minor technical enhancements. 508. 508. all authors were direct Federal employees of the U. It also gives due credit to previous authors who contributed to the development of the methods in this and previous manuals in this series.gov/nerlcwww/methmans. revision.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Aroclor 1248 505.12. The stand-alone character of the methods comes at some cost of duplication of material. 525. Some of these modifications were described in "Technical Notes on Drinking Water Methods". One exception is Method 524. 1994 and these method changes have been incorporated into the body of the methods in this supplement. As in other manuals in this series. Colloquial lab terms such as "clean-up" and "spike" are replaced by "sample preparation" or "interference separation" and "fortified" respectively. Munch U.epa. The scientifically correct term liquid-solid extraction (LSE). A change in the revision number indicates a relatively small modification to the method and a change in the method number usually indicates a relatively larger change in the method.html#organics_supp_ii[8. and previous manuals in this series. and also lists the previous versions. inserted into another binder. beverages. October. S. Environmental Protection Agency The purpose of this third supplement to "Methods for the Determination of Organic Compounds in Drinking Water" is to provide corrections. specifies drinking water. caution is needed when applying these methods to matrices other than reagent or drinking water. All methods in this supplement are written in a format specified by the United States Environmental Protection Agency's Environmental Monitoring Management Council. and editorial improvements to some previously published analytical methods and to document several significantly enhanced or previously unpublished methods. 508. All the methods in supplement III have been given new dates and version numbers or slightly modified method numbers to distinguish them from pre-viously published versions. Alternative detectors are eliminated except mass spectrometry for qualitative confirmation. Alternative detectors are eliminated except mass spectrometry for qualitative http://www.2 g/L to 80 g/L and generally excellent accuracy and precision was reported. and the 504.1 compound 1. and detection limits.0 which was published in EPA/600/4-88/03s.1 addition of method detection limits. Rev.1 is modified to remove alternative detectors 505 except mass spectrometry for qualitative confirmation and to rev. 1988 and July 1991. 3. Data tables are reorganized for clarity and 507 rev. 1988 and July 1991.3-trichloropropane is added to the analyte list.1 Cautions are included on the frequent coelution of ethylene dibromide and bromodichloromethane.1 is modified to remove mercuric chloride as a preservative. Conditions which do not require a photoionization detector are specified.2 in terms of accuracy. 2. ground water. the citation and date of publication of the previous version. several industrial waste waters.1 is modified to correct errors in themethod rev. Rev. I) in July. precision.2010 19:05:46] . Rev 3.0 was published in EPA/600/4-88/039 in Dec. Rev.1 improves Method 504 rev. 2.1 addition of method detection limits.1 provide additional instructions on the measurement of multicomponent mixtures. 1.html#organics_supp_ii[8.0 using 68 of the volatile organic compound analytes. Rev. 1988 and July 1991.epa. Rev. 2.1 is modified to specify conditions under which alternative trapping materials may be used and 502.2 rev.0 was published in EPA/600/4-88/039 in Dec. 1988 and July 1991. Rev.1 summary. revision 3.2. 1. rev. 506 1990.2. 1. 2. Method in Supp. 2.1 instructions are clarified for sample preservation and dechlorination. 2.0 was published in EPA/600/4-90/020 (Supp.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA During 1992 the USEPA and the American Society for Testing and Materials (ASTM) Committee D19 on Water jointly conducted a multi-laboratory study of an ASTM version of Method 524. 2. The methods in supplement III are listed below along with a comment for each that gives the previous version of the method. the holding time. 2. Method 504. Over 40 volunteer laboratories participated in the study to characterize the performance of Method 524. Rev.gov/nerlcwww/methmans. and a simulated hazardous waste site aqueous leachate. Analyses were conducted using fortified reagent water. Rev. and the highlights of the changes in the version in supplement III. 2. Data tables are reorganized for clarity and 508 rev.0 was published in EPA/600/4-88/039 in Dec.1 is modified to remove mercuric chloride as a preservative.0 was published in EPA/600/4-88/039 in Dec. drinking water. Fortified analyte concentrations ranged from 0. 3. 2.12. III Comments Rev. Full details of that study will be published by the ASTM. 1. I) in July 1990. Rev.1 is an improvement to Method 551 which was published in EPA/600/4-90/020 (Supp.0 analytes. 1990.0 Method 508 substances including the former commercial Aroclor mixtures. Method 552. 4. Rev. Rev. Rev.1 is modified to remove mercuric chloride as 515. 4.2 includes criteria for judging the 525. 3.1 freeze the samples. 3. rev. 1988 and July 1991. 1992.1 trimethylsilyldiazomethane (TMSD) as an alternative methylating agent. Rev. 4. Method 509 is a single analyte method for the pesticide 509 metabolite ethylenethiourea. Rev.html#organics_supp_ii[8. Method 525.2 equivalency of alternative liquid-solid extraction cartridges and rev.2 which was published in EPA/600/4-88/039 in July. II) in August.1 is modified to remove the requirement to 531.1 a preservative.0 disks. and a new sample preservation technique is used.1991.0 was published in EPA/600/4-88/039 in Dec. http://www. This method is derived from rev. It employs the liquid-solid extraction technology of Method 525.2 is similar to Method 552 which was published in EPA/600/4-90/020 (Supp. 1.2010 19:05:46] .2 rev.0 is an improvement to Method 525.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA confirmation.12. Method 551.1 is modified to include 515. 1988 and July 1991. Method 525.2 rev. rev.1 addition of method detection limits. 2.2 rev. Method 508.0 acidic methanol for methylation instead of diazomethane and expands the analyte list. 2.1 Pentane is included as an alternative solvent for some rev.1 is a significant improvement to Method 508. 4. Data tables are reorganized for clarity and rev.epa.gov/nerlcwww/methmans.1 instructions are clarified for sample preservation and dechlorination. Rev. The quality assurance section is clarified and data for two analytes are added. The elution solvent is modified and data are included for additional analytes including all former commercial Aroclor mixtures.0 was published in EPA/600/4-88/039 in Dec.1 rev.2. I) in July. 1992.0 was published in EPA/600/R-92/129 (Supp. Trimethylsilyldiazomethane (TMSD) is added as an alternative methylating agent. 1.1 is modified to specify conditions under which alternative trapping materials may be used and 524.2 uses 552. 2. 1. 551. 1. Method 552. 4. 3. 4. Data tables are revised for clarity and method detection limits are included.1 and has an analyte list consisting of many Method 507 and rev.1 national pesticide survey Method 6. 1. the analyte list is expanded. II) in August. 2. Rev. 1.1.2 508.0 was published in EPA/600/R-92/129 (Supp. 4 350. Environmental Protection Agency Cincinnati.epa.1 300. total kjeldahl nitrogen (TKN).2. phosphorus.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA To the: Chemical Exposure Research Branch Top of page Methods for the Determination of Inorganic Substances in Environmental Samples Environmental Monitoring Systems Laboratory Office of Research and Development U. quality control.0 335. 351. in an expanded form.0 8/93 8/93 8/93 8/93 8/93 ii iii iv vi 1 Determination of Inorganic Anions by 2.S.0.4 and 420. 335. 375. Abstract This manual contains ten updated and revised automated.2 Disclaimer Foreword Abstract Acknowledgment Introduction Determination of Turbidity Title Revision Date Page 2. chemical oxygen demand (COD) and generic phenolics.2.html#organics_supp_ii[8. Address your request for this manual to NTIS and ask for their order number PB94-120821. semi-automated or manual methods amenable to automation for the determination of a variety of inorganic substances in water and wastewater. Methods amenable to automation include turbidity and inorganic anions by ion chromatography. 353.00. 350. Ohio 45268 EPA/600/R-93/100 August 1993 This manual is available from NTIS and contains Methods 180.2010 19:05:46] .0 2.4. Semi-automated methods cover cyanide.0 2.0 http://www. Automated methods are included for nitrate-nitrite. 365.1 Ion Chromatography Determination of Total Cyanide by Semi-Automated Colorimetry Determination of Ammonia Nitrogen by Semi-Automated Colorimetry Determination of Total Kjeldahl Nitrogen by Semi-Automated Colorimetry 1. information concerning safety.gov/nerlcwww/methmans.4. These methods include and address.2.1. 300.1 351. and waste management.1. ammonia. 410.12. pollution prevention. Table of Contents Method Number 180.1. and sulfate. Methods were selected which minimize the amount of hazardous reagents required and maximize sample throughput to allow expanded quality control. the cost is $31. and therefore should be easy to understand and use.0 2.4 Determination of Nitrate-Nitrite by Automated Colorimetry Determination of Phosphorus by Automated Colorimetry Determination of Sulfate by Automated Colorimetry Determination of Chemical Oxygen Demand by Semi-Automated Colorimetry 2." For both the metals and non-metals manuals.2010 19:05:46] . Although a number of other methods included the 1983 edition of USEPA "Methods for Chemical Analysis of Water and Wastes". Faster analysis allows more time to perform the updated quality control required to insure valid results. New sections are included with expanded useful coverage of safety. or amenable to automation methodology that provides the following advantages over their manual counterparts: Higher sample throughput for faster analysis and improved precision. William L. Standard Methods for the Examination of Water and Wastewater. The methods contained in the 1983 manual form the basis for most of the methodology approved for compliance monitoring of inorganic parameters specified under the Clean Water Act (NPDES) and contaminants regulated under the Safe Drinking Water Act. O'Dell. They represent a selection of air segmented automated.0 2.0 2. semi-automated.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 353. 16020---07/71. the decision was made to revise and update selected non-metal methods to be issued under the name "Methods for the Determination of Inorganic Substances in Environmental Samples. was revised and issued in March 1983.html#organics_supp_ii[8. an updated second printing of the third edition. All methods are presented in the new EPA standard Environmental Monitoring Management Council (EMMC) format. Budde U. and the third edition in 1979 as EPA 600/4/79-020." With the creation of the United States Environmental Protection Agency (USEPA) in 1970 came "Methods for Chemical Analysis of Water and Wastes 1971" Publication No.12. "Methods for the Determination of Metals in Environmental Samples. the revised methods contained in this publication are considered to be the most useful in terms of future regulatory requirements. a number of new and revised metals methods were incorporated into a new publication entitled.0 8/93 James W.4 Determination of Total Recoverable Semi-Automated Colorimetry Introduction 1. John D." Concurrently. Pfaff. Environmental Protection Agency The original version of this manual was issued in November 1969 by the Federal Water Pollution Control Administration as "FWPCA Methods for Chemical Analysis of Water and Wastes.1 375. quality control. The second edition was issued in 1974 as EPA 625/6-74-003. The terms were carefully selected to be meaningful without extensive definition. http://www. In 1991. a feature especially helpful in the quality control sections where standardized terminology is not yet available.epa.0 8/93 8/93 8/93 8/93 420. The most recently published version. and American Society for Testing and Materials Annual Book of Standards (ASTM) are acceptable for compliance monitoring. several important features were adopted: Consistent use of terminology.2 410. S.2 365. pollution prevention and waste management.gov/nerlcwww/methmans. 245.50. atomic absorption (AA) spectroscopy. The 10 complete methods involve a wide range of analytical instrumentation including inductively coupled plasma (ICP)/atomic emission spectroscopy (AES). 218.1.2.2.epa. To the: Chemical Exposure Research Branch Top of page Methods for the Determination of Metals in Environmental Samples Environmental Monitoring Systems Laboratory Office of Research and Development U. and 245. sediments. 200. 200.S.8.9. The inclusion of multi-laboratory data generated from USEPA performance evaluation studies. Also included are methods that will accommodate biological tissues. Three of these methods are sample preparation procedures that require a separate determinative step found in other methods in this manual or elsewhere.5 and 245.7.gov/nerlcwww/methmans. Address your request for this manual to NTIS and request their order number PB91-231498.12. ICP/mass spectroscopy (MS). The optional use of a non-mercury catalyst in EPA TKN Method 351. and soils. Please note that revised versions of Methods 200.2. ion chromatography (IC).2.0 for anions by ion chromatography.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Lower per analysis reagent consumption to reduce waste production and minimize disposal costs. All methods allow the optional use of reduced reagent and distillation-digestion volumes. and high performance liquid chromatography (HPLC).3.8.3. 245.html#organics_supp_ii[8. 1994) of the Metals manual.2010 19:05:46] . 200. 200. groundwater and landfill leachate. Abstract Thirteen analytical methods covering 35 analytes which may be present in a variety of environmental sample types are described in detail. 200. A new stand alone semi-automated revision of EPA cyanide Method 335.6. An updated version of EPA Method 300.1. the cost is $61.11. 200. 200. The following methods are included with specific features and improvements: A revised version of EPA turbidity Method 180. 200. 245. Ohio 45268 EPA-600/4-91-010 June 1991 This manual is available from NTIS and contains Methods 200. 200. Environmental Protection Agency Cincinnati.9. Table of Contents Method Number Title Revision Date Page http://www. A new semi-automated version of the EPA phenolics Method 420.6. 200.7.10. Application of these techniques to a diverse group of sample types is a somewhat unique feature of this manual.1 are contained in Supplement I (May.1 that minimizes the direct use of hydrazine sulfate.2 that specifies the use of the downsized midi-distillation procedure. 218. Sample types include waters ranging from drinking water to marine water as well as industrial and municipal wastewater.6. Most of the methods include the option of limited performance-based modifications or improvements. 7 3.2010 19:05:46] .0 2.9 1.0 4/91 23 200.2 4/91 123 200. and Industrial Wastewater Effluents by Ion Chromatography Determination of Mercury in Water by Cold Vapor Atomic Absorption Spectrometry Determination of Inorganic Mercury (II) and Selected Organomercurials in Drinking and Ground Water by High 2.11 Determination of Metals in Fish Tissue by Inductively Coupled Plasma-Atomic 2. 3.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 200.12.3 4/91 177 218.1 Emission Spectrometry Determination of Dissolved Hexavalent Chromium in Drinking Water.1 200.3 - ii iii iv vii ix 1 4/91 3 4/91 13 200.1 4/91 227 http://www.6 4/91 211 245.3 4/91 31 200.8 4.Mass Spectrometry 2.epa.2 Disclaimer Foreword Abstract Analyte .4 4/91 153 200.Mass Spectrometry Determination of Trace Elements by Stabilized Temperature Graphite Furnace Atomic Absorption Spectrometry Determination of Trace Elements in Marine Waters by On-Line Chelation Preconcentration and Inductively Coupled Plasma .3 1.10 1.Method Cross Reference Acknowledgement Introduction and General Comments Determination of Acid Soluble Metals Sample Preparation Procedure for Total Recoverable Elements Sample Preparation Procedure for Spectrochemical Determination of Total Recoverable Elements in Biological Tissues Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma-Atomic Emission Spectrometry Determination of Trace Elements in Water and Wastes by Inductively Coupled Plasma .html#organics_supp_ii[8.2 Groundwater.gov/nerlcwww/methmans.4 4/91 83 200. 200.3.7. 200. 200.7. 200.7.10.2.9.7. 200.2010 19:05:46] .9. 200.7. 200. 200.Method Cross Reference Analyte Aluminum Antimony Arsenic Barium Beryllium Boron Cadmium Calcium Chromium Chromium VI Cobalt Copper Method No. 200. 200. 200.11 200. 200. 200.7 200. 200.7.2.11 200.2. 200.html#organics_supp_ii[8. 200. 200. 200. 200.11 200.8.3. 200. 200.6 Determination of Mercury in Tissuesby Cold Vapor Atomic Absorption 2.10.1.3 4/91 267 245. 200. 200. 200. 200.6 200.2. 200. 200. 200.1. 200. 200.1.2.3. 200. 200.1 4/91 241 245.3. 200. 200. 200.11 200.8.8. 200. 200.8.gov/nerlcwww/methmans.8.11 218. 200.9.1. 200.2.8 200. 200. 200.2.3. 200. 200.11 200.epa.7. 200.3 Performance Liquid Chromatography(HPLC) with Electrochemical Detection (ECD) Determination of Mercury in Sediment by Cold Vapor Atomic Absorption Spectrometry 1.11 200.11 200.7.9. 200.7.10 200. 200. 200.2.8.2.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 245. 200.3. 200. 200.7.9.3 Spectrometry Analyte .7.3. 200. 4/91 281 http://www.3.3.12.2.9.8. 200.2.3.3.5 2. 200.8. 200.10.11 200. 200. 200. 200.2. 200.10. 200.7.7.3 245. 200.2.8. 200. 200.3. 200. 200.3 200. 200. 200.3.8. 200. 200. 200. 200. 200. 200. Total Mercury.9 200.2.3. 200.7.epa.2.11 200.2. 200. 245.2.3. 200. 200. 245. 200. 200. 200.2.3.11 200.7.2.9.9.5.7. 200. 200. 200.8.11 200. Organic Mercury II Molybdenum Nickel Phosphorus Potassium Selenium Silica Silver Sodium Strontium Thallium Thorium Tin Uranium Vanadium http://www. 200.2.3.3. 200. 200.9 200.7.9 200. 200.7.2.10 200. 200. 200. 200.2.8 200.html#organics_supp_ii[8. 200.8.6 245.7.3.11 200.7.11 200. 200.2.3. 200.2. 200.7.7 200. 200.3. 200.2.3.9.8 200. 200.2010 19:05:46] 200.gov/nerlcwww/methmans. 200. 200. 200. 200.3. 200.7.2.3.11 200. 200. 200. 200.3. 200. 200. 200. 200.3.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Iron Lead Lithium Magnesium Manganese Mercury.1.8.11 200.9. 200.7.2. 200.2.3.9.12. 200. 200.11 200. 200. 245.1.8. 200. .8.7 200.3.2. 200.2.7 200.7.3. 200. and therefore should be easy to understand and use. 200. each method may be removed from the manual. and this feature is especially helpful in the quality control sections where standardized terminology is not yet available. the definitions of terms section of each method is nearly identical.12. instrument control samples and performance evaluation samples. analyses of field reagent blanks. Three of the methods are sample preparation procedures that refer to instrumental techniques in other methods for multi-analyte or single-analyte quantitation. The methods applicable for use in marine and estuary waters will be available for use in the Agency's National Estuary Program and subsequent EMAP studies that may involve the determination of toxic metals in the water column. routine analyses of reagent blanks.8. These methods are.2010 19:05:46] . The names of authors of the methods are provided to assist users in obtaining direct telephone support when required. The ICP/AES. 200.11 Introduction Larry B.epa. for example.3.2. compliance monitoring program. manuals have been developed and published that respond to specific regulations. An important feature of the methods in this manual is the consistent use of terminology. inserted into another binder. and analyses of quality control (QC) samples.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 200. In the past. This flexibility comes at the cost of some duplication of material. The quality assurance sections are uniform and contain minimum requirements for operating a reliable monitoring program: initial demonstration of performance.8.gov/nerlcwww/methmans. General Comments The methods in this manual are not intended to be specific for any single EPA regulation. available for incorporation into several regulatory programs due to their applicability to such diverse sample types.g. or specific study. and used without loss of information.10 Zinc 200. Environmental Protection Agency An integral component of the role of the Environmental Protection Agency (EPA) in assessing and protecting the quality of the environment is the provision of means for monitoring environmental quality. such as the Safe Drinking Water Act (SDWA) or to special studies such as the Environmental Monitoring and Assessment Program (EMAP) Near Coastal Demonstration Project. The authors believe that the added bulk of the manual is a small price to pay for the format flexibility. Other QC practices are recommended and may be adopted to meet the particular needs of monitoring programs e.9. S. To the: Chemical Exposure Research Branch Top of page Methods for the Determination of Metals in http://www.html#organics_supp_ii[8. photocopied. 200. analyses of fortified reagent blanks and fortified matrix samples. ICP/MS and AA methods have been or will be approved for use in the drinking water and the permit programs. Lobring U. The terms were carefully selected to be meaningful without extensive definition. This manual provides 13 analytical methods for 35 analytes which may be present in a variety of environmental sample types. however. In keeping with this role. that is. 200. including contaminants which may have potential adverse effects upon the health of our environment. EPA develops and disseminates analytical methods for measuring chemical and physical parameters affecting this most important resource. 200. The remaining 10 analytical methods were written to stand-alone. Revisions of these methods will be made available in a similar stand-alone format to facilitate the replacement of existing methods as new technical developments occur. 200..7. However.2 5/94 . cold vapor atomic absorption (CVAA). These methods utilize inductively coupled plasma (ICP)/atomic emission spectrometry (AES). Ohio 45268 EPA-600/R-94/111 May 1994 This manual is available from NTIS and contains new versions of Methods 200.2010 19:05:46] Title Revision Date Page 2. and ion chromatography (IC). Abstract This manual includes seven analytical methods four of which are considered multi-analyte methods.8.html#organics_supp_ii[8.9 2.9. and 200.1 and new Method 200.7. 218.9.S.2. 200.12.2 Disclaimer Foreword Abstract Acknowledgement Introduction Sample Preparation Procedure for Spectrochemical Determination of Total Recoverable Elements Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma-Atomic Emission Spectrometry Determination of Trace Elements in Water and Wastes by Inductively Coupled Plasma . graphite furnace atomic absorption (GFAA).6 and 245. procedures for the analysis of solid samples such sludges and soils also are included in the multi-analyte methods 200.8 5/94 ii iii iv vi vii 200.gov/nerlcwww/methmans. Address your request for this manual to NTIS and request their order number PB95-125472. 200. two are single analyte methods.15.4 5/94 200. drinking and ambient waters.7 4.3 5/94 200.Mass Spectrometry Determination of Trace Elements by Stabilized Temperature Graphite Furnace Atomic Absorption Spectrometry Determination of Metals and Trace Elements in Water by Ultrasonic http://www. 200. Environmental Protection Agency Cincinnati. ICP/mass spectrometry (MS).epa.. and the total recoverable sample preparation procedure is given as a separate method write up. the cost is $44. Table of Contents Method Number 200.00.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Environmental Samples Supplement I Environmental Momitoring Systems Laboratory Office of Research and Development U. Application of these methods is directed primarily toward aqueous samples such as wastewater. 200.7.8 5.8. 9.7.15 218.8.2.2.15 200.7.gov/nerlcwww/methmans.15 200.7.15 200. 200. 200. 200.2010 19:05:46] .2.15 200. 200.3 Groundwater.8. 200. 200.7. 200. 200.15 200.7.15 200. 200. 200. 200.html#organics_supp_ii[8.8.8. 200.9. 200.8.15 Nebulization Inductively Coupled Plasma-Atomic Emission Spectrometry 1. 200.7. 200.8. 200.9.6 Determination of Dissolved Hexavalent Chromium in Drinking Water.8.2. 200.2.15 3.15 200.15 200.2. 200.7.7.9.2.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 200. 200.12.2. 200. 200. 200. 200.epa.7.2.2. 200.2 5/94 218. 200.15 200. 200. 200.0 5/94 245. 200.Method Cross Reference Analyte Aluminum Antimony Arsenic Barium Beryllium Boron Cadmium Calcium Chromium Chromium VI Cobalt Copper Iron Lead Method No. 200. 200. 200. 200. 200. 200. 200.1 5/94 http://www. 200.9.8.8. 200.7. 200. 200.7. 200. 200.9.7.9. 200. 200.15 200.9.8.7. 200.2. 3.6 200.15 200. and Industrial Wastewater Effluents by Ion Chromatography Determination of Mercury in Water by Cold Vapor Atomic Absorption Spectrometry Analyte .2. 7.epa. 200. 200. Martin U. 200. 200. Total Molybdenum Nickel Phosphorus Potassium Selenium Silica Silver Sodium Strontium Thallium Thorium Tin Titanium Uranium Vanadium Zinc 200.8 200.15 200.2. 200.2. 200.2.9.15 200. 200. 200.7. 200. Determination of Metals and Trace Elements in Water by Ultrasonic Nebulization Inductively Coupled Plasma-Atomic Emission Spectrometry.8.7. 200.2. EPA 600 4-91/010.9. 200.2.7. 200.7. 245.html#organics_supp_ii[8. 200. 1991.15 200.8. The one new method appearing in this supplement is Method 200. 200. 200.gov/nerlcwww/methmans.9. 200.2. 200.7.15 200.15 200.15 200.1. 200.8.8.15 was developed to extend the analytical range of the ICP-AES http://www. S. 200.8. June.12. 200.2. 200. 200.15.9.7 200.7.15 200.2.9.2. 200.7.15 200.2010 19:05:46] . 200.2. 200. 200.2. 200. Method 200. 200.2.15 200. 200. 200. 200.7. 200.7.15 200.2. 200. 200.8. 200. 200.2.8 200.2.7.8.7.15 Introduction Theodore D. 200. 200.2. 200.15 200.2. 200.2.15 200.15 200.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Lithium Magnesium Manganese Mercury. Environmental Protection Agency Six of the seven methods appearing in this supplement were included in the first publication of the manual "Determination of Metals in Environmental Samples".7.8.9.8. 200. 200.15 200. 200. 200. 200.7.7.7.15 200.15 200. 200. 200. 200. 200. 200.2. 200. Using a common sample preparation for all spectrochemical techniques is convenient and can reduce cost of analyses. Address your request for this manual to NTIS and request their order number PB93-182913.50. 440. the required limits used in assessing recovery data from fortified matrices have been widened. Abstract This manual contains seven methods for determination of nutrients. http://www. and 200. Ohio 45268 EPA/600/R-92/121 November 1992 This manual is available from NTIS and contains Methods 200.S.epa. This procedure also is applicable to flame atomic absorption determinations. Changes to previous versions of specific methods are as follows: Cerium has been added to Method 200.2 as a stand-alone procedure.10. Also. 353. These methods are also useful for the analysis of ambient waters with the exclusion of marine water.4.gov/nerlcwww/methmans. 200.7 for correction of potential spectral interferences Titanium has been added as an analyte to Method 200.7 Mercury has been added to Method 200. Its purpose is for use in compliance monitoring of National Pollution Discharge Elimination System (NPDES) effluents as required under the Clean Water Act and compliance monitoring of drinking water as required under the Safe Drinking Water Act.7.5.9 because its determination by the graphite furnace technique is impractical Digestion of Method 245. metals and chlorophyll. and assessing ongoing laboratory performance is mandatory. this supplement is focused more on the analysis of water and wastes. the cost is $21. 365.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA technique to lower concentrations.9.12.0. The multi-analyte methods (200.12.1 mercury calibration standards is no longer required To the: Chemical Exposure Research Branch Top of page Methods for the Determination of Chemical Substances in Marine and Estuarine Environmental Samples Environmental Monitoring Systems Laboratory Office of Research and Development U. Environmental Protection Agency Cincinnati.8 for the analysis of drinking water with turbidity of < 1 NTU Zinc has been deleted from Method 200. The methods included in this supplement have been prepared in the format adopted by the Environmental Monitoring Management Council (EMMC).13. In this format method sections are ordered in a specific manner and purpose with the addition of two new sections on pollution prevention and waste management. Where available multi-laboratory data and regression equations have been included in the methods. However. Its usefulness for the analysis of drinking water is evident by the performance data included in the method. All methods have the same approach to analytical quality control in that initial demonstration of performance is required prior to method use.8. the required frequency of demonstration has been lessened and the acceptance control limits have been widened.15) all utilize the same total recoverable sample digestion procedure that is described in Method 200.2010 19:05:46] .0 and 445.html#organics_supp_ii[8. 200. Unlike the 1991 manual (EPA 600 4-91/010) which contains 13 methods for avariety of sample matrices. 200. Method 365.2010 19:05:46] . The method has been retained in this manual so that further testing can continue using a standardized method description.13 1.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA Methods 353. and the particulate carbon and nitrogen. Two of the methods are graphite furnace atomic absorption techniques and the third uses inductively coupled plasma mass spectrometry. Procedures for partitioning the organic and inorganic fractions of carbon are also presented. Single laboratory performance data are included in the methods.12 1.Mass Spectrometry Determination of Trace Elements in Marine Waters by Stabilized Temperature Graphite Furnace Atomic Absorption Determination of Trace Elements in Marine Waters by Off-Line Chelation Preconcentration with Graphite Furnace Atomic Absorption Determination of Nitrite+ Nitrate in Estuarine and Coastal Waters by Automated Colorimetric Analysis Determination of Orthophosphate in Estuarine and Coastal Waters by Automated Colorimetric Analysis Title Revision Date Page 1.3.2.gov/nerlcwww/methmans. respectively. revision 1.4 in the study indicated that the cadmium reduction column chemistry and maintenance requires further investigation.0 11/92 200. Although few laboratories currently have the instrumentation capabilities to perform all of these methods. The performance of Method 353. and the results will be included in a subsequent revision of the method.5. Since then they have undergone multilaboratory validation studies. This method has been used for many years for low level measurement of chlorophyll.4 1. it is extremely important to present them in order to stimulate the development of laboratory capability before multilaboratorystudies can be conducted.4.0 for measurement of total particulate carbon and nitrogen is based upon a well established combustion technique.5 1.0 is for the determination of chlorophyll a and the phaeopigments using fluorescence detection. revision 1.epa. appeared in the 1991 interim manual. Method 440.12. Table of Contents Method Number 200. A multilaboratory study is in progress.6 11/92 ii iii iv vi 1 200. The three metals methods represent current state-of-the-science in metals measurements. and 365.html#organics_supp_ii[8. Method 445. Introduction Determination of Trace Elements in Marine Waters by On-Line Chelation Preconcentration and Inductively Coupled Plasma . for the measurement of nitrite+nitrate and orthophosphate.0 11/92 353. The method was evaluated using two natural water samples of primarily green and blue-green algae.10 Disclaimer Foreword Abstract Acknowledgment. and chlorophyll methods are 400 series. The numbering of methods was correlated with previous EMSL-Cincinnati methods whenever possible.5 performed well in the study and multilaboratory data are presented in the revision of the method that appears here.3 11/92 365.4 11/92 http://www. The metals methods are 200 series. the nutrients nitrite+nitrate and orthophosphate are 300 series. and c and the carotenoids is not included in this edition of the manual because more research is required for a thorough evaluation of this method. The two methods that use the chelation preconcentration chromatography system offer detection limits http://www. Method 440. Another distinction of this manual is the eventual multilaboratory validation study of each method. nonetheless. Environmental Protection Agency The principal aim of this manual is to bring together under one cover a suite of analytical methods specifically adapted or developed for the examination of marine and estuarine environmental samples. Larry B. however. Method 353.4.Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA 440. performed quite well in a multilaboratory study. On the other hand. Method 445.2010 19:05:46] . Three of the methods presented here are adaptations of analytical techniques which. appears in this manual with appropriate caveats for the user so that further testing can continue using a standardized method description. for many years. Methods that reach this level of evaluation have been thoroughly investigated by a single laboratory and have usually been informally adopted as standard methods by the analytical community. and the use of the Environmental Monitoring Management Council (EMMC) methods format. The method.1 11/92 Elizabeth J. "Determination of Nitrite+Nitrate in Estuarine and Coastal Waters by Automated Colorimetric Analysis". despite its wide acceptance and routine use in the marine community.epa. William L. Method 353. b. S. Hallmarks of the methods which appear in this manual. Multilaboratory validation studies test the ruggedness of methods. The three metals methods presented here represent current state-of-the-science in metals measurement and are suitable for low-level concentrations in high salinity waters.12. "Determination of Orthophosphate in Estuarine and Coastal Waters by Automated Colorimetric Analysis".0 1.4. did not give acceptable multilaboratory results. Arar. provide single-analyst and multilaboratory precision and accuracy statements and method detection limits that are "typical" of what most laboratories can achieve. are the integrated quality control/quality assurance requirements. Method 365.0. An effort has been made to include a review of the current pertinent literature on chlorophyll measurement. A visible spectrophotometric method for chlorophyll a. The results from that study will be incorporated into the next revision of this manual.0 for the in vitro determination of chlorophyll a and the phaeopigments using fluorescence detection was evaluated using primarily freshwaterphytoplankton samples. As a result of the study. and it must return to the development phase. Their data suggest that the cadmium reduction column chemistry and maintenance require further investigation.5. The mandatory demonstration of laboratory capability and the continuing checks on method performance ensure the quality and comparability of data reported by different laboratories and programs. a widely accepted method in the marine community. We do not believe this prohibits its inclusion in a marine methods manual since the analytical steps are the same regardless of algae classification. A table has been added to the method to summarize single-analyst and multilaboratory precision and accuracy of the method for three water matrices.html#organics_supp_ii[8. pooled method detection limits for orthophosphate in a wide range of water salinities have also been added to the method.gov/nerlcwww/methmans. Lobring U. have been used routinely by the marine community.4 11/92 445. the use of standardized terminology. for particulate carbon and nitrogen uses a well established combustion technique and is currently undergoing multilaboratory validation. failed the ruggedness test when 50% of the participating laboratories in the multilaboratory study returned unacceptable data. Budde.0 Determination of Carbon and Nitrogen in Sediments and Particulates of Estuarine/Coastal Waters Using Elemental Analysis In Vitro Determination of Chlorophyll a and Phaeophytin a in Marine and Freshwater Phytoplankton by Fluorescence Introduction 1. Analytical Chemistry Methods Manuals | Microbiological and Chemical Exposure Assessment Research | US EPA roughly an order of magnitude lower than their conventional counterpart methods. the methods will undergo multilaboratory validation studies. revised and validated. such as the Environmental Monitoring and Assessment Program (EMAP) Near Coastal Demonstration Project.12. As the instrumentation for these techniques becomes more prevalent in analytical laboratories.2010 19:05:46] . nutrients and metals continually being added.epa. In the past. The methods in this manual are not intended to be specific for any single USEPA regulation. This manual should be viewed as a living document. such as the Safe Drinking Water Act (SDWA). We encourage users of the methods in this manual to share their experiences with us and to obtain new editions of the manual as they become available.html#organics_supp_ii[8. or to special studies. To the: Chemical Exposure Research Branch Top of page Microbiological and Chemical Exposure Research EPA Microbiology | Exposure Research http://www. manuals have been developed and published that respond to specific regulations.gov/nerlcwww/methmans. however. with methods for organics. These methods are. or specific study. There is also much work to be done in assuring the provision of SRMs and quality control samples to the marine monitoring community. compliance monitoring program. updated. available for incorporation into regulatory programs that require the measurement of nutrients and metals in marine waters.
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