NOAA NST: 130.01: Organic contaminates in marine animal tissues by GC-FPD
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Official Method Name
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Capillary gas chromatography analysis for organic contaminates in marine animal tissues. |
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Current Revision
| March 1998 |
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Media
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ANIMAL TISSUE |
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Instrumentation
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Gas Chromatograph with Flame Photometric Detector |
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Method Subcategory
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Organic |
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Method Source
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Citation
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Sampling and Analytical Methods of the National Status and Trends Program Mussel Watch Project: 1993-1996 Update. NOAA Technical Memorandum NOS ORCA 130. March 1998. Silver Spring, MD. 233pp. |
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Brief Method Summary
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Measurements of organotin compounds in biological tissues require the isolation of these contaminants from the matrices. An aliquot of the homogenized tissue sample is extracted three times by maceration with 0.05% tropolone in dichloromethane in the presence of sodium sulfate. The extract is concentrated by Kuderna-Danish technique and the solvent is exchanged to 10 mL of hexane. Organotin compounds are hexylated with Grignard reagent and the derivatized extract is purified using silica gel/alumina chromatography before instrumental analysis. Quality control samples are processed with each bath of samples in a manner identical to that of the actual samples. |
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Scope and Application
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This method determines butyltins (i.e., tetra-, tri-, di-, and monobutyltins) in marine animal tissues at trace levels (parts per billion to parts per trillion). |
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Applicable Concentration Range
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0 - 182 ng Sn / g |
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Interferences
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Method interferences may be caused by contaminants in solvents, reagents, glassware, and other sample processing labware that lead to false positive detections. All materials used in this method are routinely demonstrated to be free from interferences by processing procedural blanks using the same procedure as that used for the samples (one blank per 20 samples or each batch whichever is more frequent). Matrix interferences may be caused by compounds other than the analytes of interest that are coextracted from the sample. Biogenic materials that cause interferences in the analysis of tissue extracts are removed prior to GC/FPD analysis by silica gel/alumina chromatography. |
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Quality Control Requirements
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The quality assurance / quality control requirements were as follows: Initial calibration and continuing calibration checks. Method blank analysis. Surrogate compound analysis Matrix spike analysis. Reference sample analysis |
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Sample Handling
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Collect samples in a glass container and store in the dark at or below -20 deg. C. Store extracts in the dark at 4 deg. C. |
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Maximum Holding Time
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6 months (frozen) |
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Relative Cost
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$201 to $400 |
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Sample Preparation Methods
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NOAA TM #130 |
