EPA Method A in the EPA methods list database. View all EPA methods. EPA Method A: Chlorinated Biphenyl. Congeners by HRGC/HRMS. Horizon Technology, Inc., Salem, NH. Horizon Technology, Inc., 45 Northwestern Dr. Ecology may require or allow the use of the most current accepted revision of EPA Method (USEPA, ) at contaminated sites, instead.

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Alternatively, a separate sample aliquot may be used for the lipid determination. Each laboratory that uses this Method must demonstrate the ability to generate acceptable results using the procedure in Section 9. Concentration for Biosolids Figure is a plot of RSDs as a function of concentration for the congeners detected in biosolids. In selecting the samples, EPA’s objective will be to maximize the number of congeners represented and ensure that the congeners span the anticipated measurement range of the method, ranging from the upper end of the calibration range down to “not detected.

Adjust the vacuum to complete the extraction in no less than 10 minutes. Results differ most for the early-eluting labeled congeners. Remove the Snyder column and rinse the glass joint into the receiver with small portions of solvent.

Method A Interlaboratory Validation Study Report

Softer particles can be reduced by grinding in a Wiley mill or meat grinder, by homogenization, or in a blender. So that a sufficient amount of each sample was available to support the study, EPA identified several samples of each matrix type that could be combined to produce large volumes of Youden pairs with the desired congener distribution.

An objective of this review will be to maximize data use. Samples will be collected by individuals trained in appropriate sample collection and handling procedures. EPA will request that laboratories submit analytical results within 45 days of receipt of samples. If a 6-point calibration is used, prepare the CS Thus, the sample processing laboratory was instructed to first analyze an aliquot of wastewater from a publicly owned treatment works POTW to determine background PCB congener levels.


Laboratory 3 also reported loss of sensitivity, column deterioration, and expressed general dissatisfaction with the method.

EPA Method 1668A

If low background levels of the CBs are present in the reference matrix, the spike level of the analytes used in Section 9. This isomeric pair is uniquely resolved from all other congeners and these congeners have the same TEF and response factor. If possible, a single supplier will aggregate all standards solutions into a set, and package a set of standards for shipment to each laboratory. Grind the blank and reference matrix aliquots using a clean grinder. Because of the mixing scheme for both of these matrices, it was assumed that if the homogeneity for sample “B” is found e;a be acceptable, the homogeneity of sample “A” would also be acceptable.

The total number of participant laboratories will depend upon laboratory capability, availability, cost, and scheduling constraints. Following a review of the background results by SCC, EPA defined the spiking levels, and provided the sample processing laboratory with detailed instructions to divide the unspiked POTW matrix into the required number of aliquots and spike each aliquot separately rather than spiking a bulk volume of wastewater and then subdividing the spiked sample into replicate aliquots to the appropriate concentrations.

These windows may not be adequate for analyte identification See the note in Section Wpa holding a GMF filter above the SPE disk with tweezers, wet the filter with methylene chloride and lay the filter on the SPE disk, making sure that air is not trapped between the filter and disk.

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Although some congeners have only a single chlorine atom, the entire suite of chlorinated biphenyl congeners will be referred to as “PCBs” in the remainder of this study plan for consistency with common usage.

The dry weight data for laboratory 8 were corrected to wet weight based on percent solids data provided by laboratory 8 Since that presentation, the results have been further evaluated and presented in this report. The windows in Table 2 were developed based on the GC conditions given in Section Laboratories will not be allowed to average results or perform other data manipulations beyond those described in Method A. Retention time RT reference used to locate target congener.


Store in a screw-capped bottle with fluoropolymer-lined cap. Lipids must be removed by an anthropogenic isolation column procedure, followed by the gel permeation chromatography procedure as described in the method.

The method also determines the remaining CBs, approximately of which are resolved adequately on an SPB-octyl gas chromatographic column to be determined as individual congeners. Prewet the column by adding approximately 1 mL of solvent through the top. Laboratory 4 reported difficulties with the cleanup of both the biosolids samples. Labeled injection internal standard 5.

The acid 1668x gel Section 7.

US EPA METHOD A/B/C “STARTER KIT” – Cambridge Isotope Laboratories –

Florisil is recommended as an additional cleanup step. Repeat the acid washing until no color is visible in the aqueous layer, to a maximum of four washings. Development of accuracy statements is described in Section 9.

The references and bibliography at the end of Reference 8 are particularly comprehensive in dealing with the general subject of laboratory safety. Other sample collection techniques, or sample volumes may be used, if documented. At the proper rate of distillation, the balls of the eppa will actively chatter but the chambers will not flood. The 1668w of this interlab study met our objectives to characterize the performance of Method A in several laboratories and matrices, and use the results to replace the single-lab QC acceptance criteria in A with interlab criteria.

Glassware with removable parts, particularly separatory funnels with fluoropolymer stopcocks, must be disassembled prior to detergent washing.