NOAA NST: 130.20: Dioxins and Furans in marine sediments by GC-MS
|
Official Method Name
|
Analysis of marine sediment for Polychlorinated Dibenzo-p-dioxins and Polychlorinated Dibenzofurans by GC-MS. |
|---|---|
|
Current Revision
| March 1998 |
|
Media
|
SOILS/SEDIMENT |
|
Instrumentation
|
Gas Chromatography with Mass Spectrometry Detection |
|
Method Subcategory
|
Organic |
|
Method Source
|
|
|
Citation
|
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. |
|
Brief Method Summary
|
This method provides procedures for the detection and quantitative measurement of polychlorinated dibenzo-p-dioxins (tetra- through octa-chlorinated homologues; PCDDs) and polychlorinated dibenzofurans (tetra- through octa-chlorinated homologues; PCDFs) in sediments at pg/g concentrations. |
|
Scope and Application
|
This procedure uses matrix-specific extraction and analyte-specific purification steps to allow the determination of the chlorinated dibenzop-dioxins (PCDDs) and dibenzofurans (PCDFs) in marine sediments using high resolution gas chromatography/high resolution mass spectrometry. The method provides selective cleanup procedures to aid in the elimination of interfering contaminants. |
|
Applicable Concentration Range
|
1 - 4000 ppt |
|
Interferences
|
Interferences in the matrix, solvents, reagents, glassware and other sample processing hardware may yield discrete artifacts and/or other elevated baselines that cause misinterpretation of chromatographic data. All materials used during the cleanup procedure were demonstrated to be free from interferences by analyzing laboratory method blanks at a frequency of one blank per 20 samples or one with each batch if the number of samples is less than 20. The minimum level for each analyte was defined as the level at which the entire system must give a recognizable signal and acceptable calibration point. It was equivalent to the concentration of the lowest calibration standard, assuming that all method specific sample weights, volumes, and procedures were employed. |
|
Quality Control Requirements
|
The quality assurance / quality control requirements are as follows: Method blank. Laboratory blank spike. Ongoing precision and recovery analyses. Matrix spike. Duplicates. Reference material (NIST SRM 1944) analyses. Labeled compound recovery. |
|
Sample Handling
|
Samples were collected and placed in pre-cleaned mason jars. Samples were stored in the dark at or below -20 C. Sample extracts were stored in the dark at 4 C. |
|
Maximum Holding Time
|
6 months (frozen) |
|
Relative Cost
|
Greater than $400 |
|
Sample Preparation Methods
|
NOAA TM #130 |
