NEMI Method Summary

Method Summary Information

Method Number: 130.00 Media: SOILS/SEDIMENT
Revision: March 1998
Method Source: National Oceanic and Atmospheric Administration (NOAA)
Analytes in this method
Subcategory: ORGANIC
Official Name: Capillary gas chromatography analysis for organic contaminates in marine sediments.
Descriptive Name Capillary gas chromatography analysis for organic contaminates in marine sediments.
Source Info: National Oceanic and Atmospheric Administration (NOAA)
National Status and Trends Program (NS&T;)
SSMC-4, N/SCI-1
1305 East West Highway
Silver Spring, MD 20910
Tel. 301-713-3028
Citation: Sampling and Analytical Methods of the National Status and Trends Program: 1993-1996 Update
990997
Brief Method
Summary:
 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.
Scope And
Application:
 This method determines butyltins (i.e., tetra-, tri-, di-, and monobutyltins) in marine sediments at trace levels (parts per billion to parts per trillion).
Applicable
Conc Range:
 0 - 182 ng Sn / g
Interferences: 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.
QC Requirements: 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
Sample Handling: 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.
Max Holding Time:
 6 months (frozen)
Sample Prep Met NOAA TM #130
Relative Cost: $201 to $400
URL to obtain ordering information for this method:
http://nsandt.noaa.gov/publications/download_pdf/techmemo130.pdf
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