This kit provides all of the necessary materials to conduct the EPA A test. It can be used to analyze finished drinking water, drinking water in any stage for. EPA Method a – Screening for Polychlorinated Biphenyls by Perchlorination and Gas Chromatography. Analyzer Description. Configuration: 1-capillary. Subsequently, the LabCert program has only offered certification for the analysis of PCBs in drinking water by EPA method A. Method A, and s.

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Environmental Protection Agency, and approved for publication. Mention of trade names or commercial products does not constitute endorsement or recommendation for use.

This publication of the Environmental Monitoring Systems Laboratory – Cincinnati titled, “Determination of Organic Compounds in Drinking Water” was prepared to gather together under a single cover a set of 13 laboratory analytical methods for organic compounds in drinking water. We are pleased to provide this manual and believe that it will be of considerable value to many public and private laboratories that wish to determine organic compounds in drinking water for regulatory or other reasons.

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,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, Five of the methods utilize the inert gas purge-and-trap extraction 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 basedion a high performance liquid chromatography separation. Special thanks and appreciation are due to Patricia L. Ciampone, and Glenora F. Scruggs who provided outstanding secretarial and word processing support for the entire effort. In addition, James J.

Lichtenberg and James E.

Longbottom, who managed the drinking water organic methods development program for a number of years, are recognized for their many important contributions. Wilson and Carol Brockhoff typed many of the earlier drafts of the methods. Donnelly provided electronics engineering support during several of the methods development projects.

McKee served as a manager during the development of several of the methods. The staff of the Technical Support Division of the Office of Drinking Water, and particularly Richard Reding, provided extensive comments on the first draft of this manual, and on previous revisions of many methor the analytical methods.

Madding, working under the direction of Dr. Herbert Brass, tested and provided data for the cryogenic interface option in Method Finally, all the authors and contributors wish to thank the administrators and managers of the Environmental Protection Agency for their support during the development and preparation of this manual.

Metho appreciation is due to Robert L. Budde Many of the nearly organic analytes included in this manual may be identified and measured in drinking water using two or more of the documented analytical methods.

For example, nearly 50 compounds are listed as analytes in four different methods. This approach of multiple methods for many analytes was selected to provide the maximum flexibility to method users from small and large laboratories. Some methods require relatively modest equipment, and others require sophisticated instrumentation. This flexible approach should meet the needs and requirements of nearly all laboratories.

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. This flexibility comes at the cost of some duplication of material, for example, the definitions of terms section of each method is nearly identical. The authors believe that the added mfthod of the manual is a small price to pay for the flexibility of the format. An important feature of the methods in this manual is the consistent use of terminology, and this feature is especially helpful in the quality control sections where standardized terminology is not yet available.

The terms were carefully selected to be meaningful without extensive definition, and therefore should be easy to understand and use. The names of authors of the methods are provided to assist users in obtaining direct telephone support when required. While some of these methods may provide reliable results with more complex water matrices, for example, industrial wastewaters and beverages, 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.


Therefore caution is needed when applying these methods to matrices other than relatively clean water. Methods developed for drinking 50a8 include provisions for removal of free chlorine dechlorination which is assumed to be present in all samples. Dechlorination is necessary to stop the formation of trichloromethanes and other disinfection by-products, or to prevent the formation of method interferences and analytes generated from chlorination of mefhod in reagents and solvents.

These mrthod are intended to provide an indication of the capability of the method, but they may not be of regulatory significance. The EDL is either the MDL, 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. If the replicate measurements needed to calculate an MDL are obtained under ideal conditions, for example, during a short metnod of time within a work shift, the resulting standard deviation may be small and give an unrealistically low MDL.

The data acquired for measurement of an MDL mthod be obtained over a period of time several days or more.

50a Obtained in this way, the standard deviation includes normal day-to-day variations, and the MDL will be more realistic. 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. Calibration standards and quality control samples may be available commercially, or may be available on a limited basis from jethod Quality Assurance Research Division, Environmental Monitoring Systems Laboratory – Cincinnati, 26 W.

These are Methods Five of these methods utilize the same basic purge-and-trap extraction technique, but, depending on the specific method 508w, the user has a choice of a packed or capillary column gas chromatography GC separation and a mass spectrometer MS or conventional GC detector.

The other method Method is a microextraction procedure for two compounds of special interest, ethylene dibromide EDB and l,2-dibromochloropropane DBCP. Solicited and unsolicited written and telephoned comments have been received from some of the laboratories using the VOC methods, and some of these users suggested certain technical and editorial changes. In addition, the staff of the Chemistry Research Division recognized that some changes were needed to make the methods easier to understand and use, and bring them up-to-date.

The revisions of the six VOC methods contained in the manual incorporate a few technical and many editorial changes which are summarized below. Few technical changes were made to the six VOC methods. The use of ascorbic acid as a dechlorinating agent is described. Ascorbic acid has been extensively tested as a dechlorinating agent, and has been found to be as effective as sodium thiosulfate, but without the undesirable generation of sulfur dioxide at low pH. Data is presented in the method to show that the open split interface can provide acceptable precision, accuracy, and detection limits.

The previous revision of Method Methov laboratories will find the open split interface to be the most economical for this method. Changes were made in the recommended chromatographic conditions and internal standards in Method These changes allow the measurement of all 60 VOCs in a single calibration solution. Extensive editorial changes were made in. These editorial changes were necessary to provide an organized, consistent, and much eps complete presentation of the myriad details needed by laboratories to successfully implement the methods.

The addition of these details, the 50a8 use of terminology, and the uniform organization of all the methods should substantially msthod the number of questions received and provide the user community with the information needed to obtain high quality results. Spa 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, and Rpa of the methods Method A was designed as a screening procedure for polychlorinated epz PCBs.


EPA Method a – Screening for Polychlorinated Biphenyls by Perchlorination and Gas Chromatography

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, and detected with an electron capture detector. Method provides a rapid procedure for chlorinated hydrocarbon pesticides emthod commercial PCB mixtures Aroclors.

This method uses a high resolution capillary column GC separation and detection with an electron methid detector. The cartridges are small about 0. The disks are made of Teflon containing silica which is coated with a chemically bonded C organic phase.

Water samples are passed through the cartridges or disks and some organic compounds are sorbed on the solid phase. After air drying, the organic compounds are eluted using a very small volume of an organic mmethod.

Cartridges from six suppliers were used in the methods research, and a quality control procedure was developed to permit epw of cartridges with acceptable performance characteristics. The disks are manufactured by a single company, methood only one type was evaluated. The LSE procedure is attractive because it greatly reduces the use and worker exposure to methylene chloride and similar solvents. This allows the simultaneous determination of 42 SOCs including chlorinated hydrocarbon pesticides, polycyclic aromatic hydrocarbons, phthalate and adipate esters, individual PCB congeners, several triazine pesticides, and pentachlorophenol.

Laboratories will find this method attractive because of its potential economy of operation when a wide variety of analytes are to be determined. Bellar – Method Determination of complex mixtures containing partially resolved compounds may be hampered by concentration differences larger than a factor of This problem commonly occurs when finished drinking waters are analyzed because of the relatively high trihalomethane content.

When such samples are analyzed, chloroform will affect the method detection limit for 1,2-dichloroethane. It is also recommended for use only with a purge and trap system devoted to the analysis of low level samples.


EPA Method 508A Screening for Polychlorinated Biphenyls by Perchlorination

Purged sample components are trapped in a tube containing suitable sorbent materials. When purging is complete, the sorbent tube is heated and backflushed with an inert gas to desorb trapped metod components onto a gas chromatography GC column.

The gas chromatograph is temperature programmed to separate the method analytes which are then detected with a halogen specific metuod. The internal standard must be an analyte that is not a sample component. Analyses of LD1 and LD2 give a measure of the precision associated with laboratory procedures, but not with sample collection, preservation, or storage procedures. The LRB is used to 508x if method analytes or other interferences are present in the laboratory environment the reagents, or the apparatus.

The purpose of the FRB is to determine if method analytes or other interferences are present in the field environment. The LFB is analyzed exactly like a sample, and its purpose is to determine whether the methodology is in control, and whether the laboratory is capable of making accurate and precise measurements at the required method detection 508.

Decachlorobiphenyl, A / Reference Standards / Chromatography Products at

The LFM is analyzed exactly like a sample, and its purpose is to determine whether the sample matrix nethod bias to the analytical results.

The background concentrations of the analytes in the sample matrix must be 3. Stock standard solutions are used to prepare primary dilution standards. The CAL solutions are used to calibrate the instrument response with respect to analyte concentration.

The QCS is generated from a source of reagents different than those used to prepare the primary dilution standards and the calibration standard and is used to check laboratory performance.

The use of non-polytetrafluoroethylene PTFE plastic tubing, non-PTFE thread sealants, or flow controllers with rubber components in the purging device should be avoided since such materials out-gas organic compounds which will be concentrated in the trap during the purge operation.

Analyses of laboratory reagent blanks Sect. When potential interfering peaks are noted in laboratory reagent blanks, the analyst must eliminate the meghod before analyzing samples. Subtracting blank values from sample results is not permitted.