NOAA NST: 130.00: Capillary gas chromatography analysis for organic contaminates in marine sediments.
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Official Method Name
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Capillary gas chromatography analysis for organic contaminates in marine sediments. |
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Current Revision
| March 1998 |
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Media
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SOILS/SEDIMENT |
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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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Assessment of the environmental impact of butyltins (i.e., tetra-, tri-, di-, and monobutyltins) requires their measurement in sediments at trace levels (parts per billion to parts per trillion). Freeze-dried samples were serially extracted with 0.2% tropolone in dichloromethane. The extract is then hexylated with a Grignard reagent. The hexylated extract is dried and concentrated. A silica gel/alumina column cleanup step is used to remove matrix interferences prior to high resolution, capillary gas chromatography using flame photometric detection (GC/FPD) instrumental analysis. |
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Scope and Application
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This method determines butyltins (i.e., tetra-, tri-, di-, and monobutyltins) in marine sediments 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 result from the co-extraction of compounds other than the analytes of interest. Previous analyses of sediments indicate that matrix interferences are generally low. |
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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 |
