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TDI Brooks International, Inc. (TDI) Laboratory Methods

Select one of the links below to display the method descriptions associated with TDI.

Method Code

Method Title

001

Tissue Extraction Method (PAH and OCs)

002

Aromatic Hydrocarbon Determination by Selected Ion Monitoring (SIM) Gas Chromatography/Mass Spectrometry (GC/MS)

003

Chlorinated Hydrocarbon Determination by Gas Chromatography/Electron Capture Detection (GC/ECD)

004

Confirmation of Analytes

005

Sediment Extraction Method (PAH and OCs)

006

Total Organic and Inorganic Carbon is Soils and Sediments

007

Determination of Particle Size Distribution in Sediments

008

Determination of Total Petroleum Hydrocarbons in Soil/Sediment

009

Determination of Aliphatic Hydrocarbons in Soil/Sediment

010

Volatile Organic Compounds (VOC) Determination by Purge and Trap Analysis with Gas Chromatography/Mass Spectrometry (GC/MS)

011

Water Extraction Method (PAH and OC)
012 Polybrominated Diphenyl Ether (PBDE) Determination by Negative Chemical Ionization (NCI)-Selected Ion Monitoring (SIM) Gas Chromatography/Mass Spectrometry (GC/MS)

 

 

 

 

 

Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 001

Tissue Extraction Method (PAH and OCs)

Tissue samples are either immediately processed or stored frozen (-20°C) until processing. Tissues are processed as appropriate for the tissue type (e.g. dissection, shucking). Processed tissues are homogenized using a variety of mechanical methods (Waring blender, Hobart meat grinder or Tissumisser), depending upon the tissue amount and type. After homogenization, an approximate 1 g aliquot is removed and dried in an oven at 105°C to a constant weight to determine % moisture. The remaining samples are stored in certified pre-cleaned jars frozen (- 20°C) until analysis. Prior to extraction, tissue samples may be lypholized or a wet aliquot is chemically dried using a dessicant such as Hydromatrix or sodium sulfate. Samples are then extracted using a Dionex ASE200 Accelerated Solvent Extractor (ASE). The dried sample or the sample and dessicant material is loaded into 22 or 33 mL stainless steel ASE extraction tubes. The extraction are performed using 100% dicholormethane at 100°C and 2000 psi. The extracted organics dissolved in the solvent are collected in 60 mL glass vials. The extract is concentrated to approximately 10 mL in the collection vials and then transferred to 25 mL Kurdena-Danish (KD) concentrator tubes. The sample extract is concentrated to 3 mL in a water bath at 55-60°C. If lipid weight is required, a 100 mL aliquot is removed and weighed using a microbalance. Interfering non-contaminant organic material (primarily lipids) must be removed prior to instrument analyses.

The extract is processed through silica gel/alumina chromatography columns and High Performance Liquid Chromatography (HPLC). The remaining 2.9 mL of sample extracted are loaded on top of 300 mm x 19 mm glass liquid chromatography columns packed with 10 g of deactivated alumina and 20 g of deactivated silica gel. The columns are loaded in 100 % dichloromethane. The dichloromethane is replaced by adding 40 mL of pentane. The extract is carefully added to the top of the chromatography columns. The column is flushed at a rate of 1-2 mL per minute using 200 mL of 50:50 pentane/dichloromethane and collected into 250 mL flasks. The eluent collected in the 250 mL flask is evaporated to 2 mL using a waterbath at 55-50°C. The samples is transferred into 4 mL amber vials. Extracts subsequently processed by HPLC to further remove lipid interferences. Lipid removal is accomplished by flushing samples with dichlormethane through size exclusion Phenogel 10 m GPC 100 A columns. Approximately 40 mL is collected using a fraction collector, which is concentrated to 0.5 mL using a water bath at 55-60C. The concentrated extract is then analyzed by GC/MS for polynuclear aromatic hydrocarbons (PAHs) or GC/ECD for selected organochlorines (OCs).

Additional column chromatography is required to separate PCBs from toxaphene/pesticides when toxphene analysis is
required and to separate planar PCBs. If toxaphene analyses is required, an aliquot of the extract prior to HPLC clean up is processed through a 3% deactivated silica gel column. The column is packed in dicloromethane which is then flushed with 50 mL of pentane. The sample extract is transferred to the top of the column and flushed with 100 mL of pentane. The fraction contains PCBs and DDTs. The column is then flushed with 120 mL of 50:50 pentane/dichloromethane. This fraction contains toxaphene and chlorinated pesticides. Both fractions are reduced to 1 mL using a water bath at 55-60°C. The extracts are then ready for instrument analysis.

If planar PCB analyses are required, the PCB/DDT fraction prepared by 3% silica gel column is further processed by column chromatography packed with 2 g of 1:19 (5% by weight) mixture of activated carbon/Celite. The column and flushed with 25 mL of 1:4 dichloromethane/cyclohexane mixture. The sample is added to the top of the column and flushed with 50 mL of 1:4 dichloromethane/cyclohexane mixture, followed by 30 mL of 9:1 dichloromethane/toluene. This is followed by the addition of 40 mL of toluene. The toluene fraction contains the planar PCBs and is concentrated to 1 mL in a Zymark TurboVap II concentrator at 42°C and 20 psi. The sample is ready for instrument analysis.

REFERENCES:

Lauenstein, G.G. and A.Y. Cantillo, ed. (1993). Sampling Analytical Methods of the National Status and Trends Program National Benthic Surveillance and Mussel Watch Projects 1984-1992; Volume IV: Comprehensive Descriptions of Trace Organic Analytical Methods. NOAA Technical memorandum NOS ORCA 71, Silver Spring, MD.

U.S. Environmental Protection Agency. 2001. National Coastal Assessment Quality Assurance Project Plan 2001-2004. United States Environmental Protection Agency, Office of Research and Development, National Health and Environmental Effects Research Laboratory, Gulf Ecology Division, Gulf Breeze, FL. EPA/6
20/R-01/002.

Environmental Protection Agency, "Method 3545: Pressurized Fluid Extraction (PFE)," in Test Methods for Evaluating Solid Waste, Physical/Chemical Methods EPA SW-846 [Version 2 (December 1997), Integrated Manual through Update III] Washington DC, U.S. Environmental Protection Agency (1997)

Zuloaga, O.; Etxebarria, N.; Fernandez L. A.;Madariaga, J.M.; Optimization and comparison of MAE, ASE and Soxhlet extraction for the determination of HCH isomers in soil samples. Fresenius J Anal Chem, 2000, 367, 733-737.

Schantz, M.; Nichols, J. J.; Wise, S. A.; Evaluation of Pressurized Fluid Extraction for the Extraction of Environmental Matrix Reference Material, Anal. Chem., 1997, 69, 4210-4219.

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 002

Aromatic Hydrocarbon Determination by Selected Ion Monitoring (SIM) Gas Chromatography/Mass Spectrometry (GC/MS)

Polycyclic aromatic hydrocarbons (PAH) and their alkylated homologues are analyzed in sample extracts by a HewlettPackard, model 5890 GS and model 5972 MS operated in SIM using a capillary column. The GC is operated in splitless mode and the capillary column is an Agilent Technologies HP-5MS (60 m x 0.25 mm ID and 0.25 mm film thickness). The carrier gas is helium at a flow rate of 1 mL/minute. The temperature of the injection port is 300°C and transfer line is 290°C. The initial oven temperature is 60°C, the ramp rate is 7°C/minutes to a final oven temperature of 310°C and held for 20 minutes. For analyte identification, the extracted ion current profiles of the primary m/z and the confirmatory ion for each analyte must be at a maximum in the same scan or within one scan of each other and the retention time must fall with 5 seconds of the retention time of the authentic standard or alkyl homologue grouping. The pattern of alkylated PAH homologue groupings is established by analysis of reference oil standards. The relative peak heights of the primary mass ion compared to the confirmation or secondary mass ion must fall within 30 % of the relative intensities of these masses in a reference mass spectrum.

REFERENCES:

Lauenstein, G.G. and A.Y. Cantillo, ed. (1993). Sampling Analytical Methods of the National Status and Trends Program National Benthic Surveillance and Mussel Watch Projects 1984-1992; Volume IV: Comprehensive Descriptions of Trace Organic Analytical Methods. NOAA Technical memorandum NOS ORCA 71, Silver Spring, MD.

U.S. Environmental Protection Agency. 2001. National Coastal Assessment Quality Assurance Project Plan 2001-2004. United States Environmental Protection Agency, Office of Research and Development, National Health and Environmental Effects Research Laboratory, Gulf Ecology Division, Gulf Breeze, FL. EPA/620/R-01/002.

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 003

Chlorinated Hydrocarbon Determination by Gas Chromatography/Electron Capture Detection (GC/ECD)

Chlorinated hydrocarbons are determined in samples by GC/ECD. Samples are extracted as previously described and analyzed on a HewletPackard (HP), model 5890 GC equipped with an ECD. Between 1 to 5 mL of sample is injected using an HP, model 7673A autosampler. The instrument is set up with dual columns. The primary capillary column is a J&W DB-5 (30 m x 24 mm ID and 0.25 mm film thickness). The second column, a confirmation column, is a J&W DB-17HT (30 m x 0.25 mm ID and 0.15 mm film thickness). The inlet system is splitless and the carrier gas is helium at a flow rate of 1 mL/min. For the analysis of standard halogenated hydrocarbons, the temperature of the injection port is 275°C and the detector is 325°C. The initial oven temperature is 100°C with a hold time of 1 minute. The ramp rate is 5°C/minute to 140°C with a hold time of 1 minute, followed by a ramp rate of 1.5°C /minute to 250C with a hold time of 1 minute and finally a ramp rate of 10°C/minutes to 300°C with a final hold time of 5 minutes. For planar PCBs the instrument is operated in the splitless mode withhelium as the carrier gas with a flow rate of 1 mL/minute. The temperature of the injection port is 275°C and the detector is 325°C. The initial oven temperature is 100°C, which is held for 1 minute. The ramp rate is 10°C/minute to 150°C, followed by a ramp rate of 6.0°C/minute to 270°C with a hold time of 3 minutes. The retention time of sample analytes must fall within 15 seconds of the retention time of analytes in a calibration standard or a retention index solutions. The levels of aroclors and toxophene are determined using retention index solutions of both complex mixtures. Arochlors are determined in a similar method to that described in EPA SW-846 Test Methods for Evaluating Solid Waste Physical/Chemical Methods, Method 8082 (1997).

REFERENCES:

Lauenstein, G.G. and A.Y. Cantillo, ed. (1993). Sampling Analytical Methods of the National Status and Trends Program National Benthic Surveillance and Mussel Watch Projects 1984-1992; Volume IV: Comprehensive Descriptions of Trace Organic Analytical Methods. NOAA Technical memorandum NOS ORCA 71, Silver Spring, MD.

U.S. Environmental Protection Agency. 2001. National Coastal Assessment Quality Assurance Project Plan 2001-2004. United States Environmental Protection Agency, Office of Research and Development, National Health and Environmental Effects Research Laboratory, Gulf Ecology Division, Gulf Breeze, FL. EPA/620/R-01/002.

Environmental Protection Agency, "Method 8082: Polychlorinated Biphenls (PCBs) by Gas Chromatography," in Test Methods for Evaluating Solid Waste, Physical/Chemical Methods EPA SW-846 [Version 2 (December 1997), Integrated Manual through Update III] Washington DC, U.S. Environmental Protection Agency (1997)

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 004

Confirmation of Analytes

The presence of pesticides and PCBs is confirmed by gas chromatography/mass spectrometry (GC/MS) in either full scan or selection ion monitoring mode (SIM). Samples are extracted as previously described. Samples are initially screened by GC/ECD and GC/MS to confirm the presence of specific analytes in a sample. When analytes are detected at 10 x the SIM limit of detection they may be confirmed by SIM GC/MS. The samples are analyzed on a HewlettPackard 5890GC/ 5972MS. The GC is temperature- programmed and operated in splitless mode. The analytical column is an Aglient Technologies HP5MS (60 m x 0.25 mm ID and with a 0.25 mm film thickness). The carrier gas is helium with a flow rate of 1mL/min. The temperature of the injection port is 300°C and the transfer line is 290°C. The oven is at an initial temperature of 60°C with a ramp time of 7°C/minute. Analytes are "confirmed" when the spectrum contains at least 3 of the major ions. The chromatographic peaks must be at least 3 x the background noise and must be within once scan of each other and match the retention time of the standard run under the same conditions to be "confirmed"

REFERENCES:

Environmental Protection Agency, "Method 8270C: Organic Compounds by Gas Chromatography/Mass Spectrometry (GC/MS)" in Test Methods for Evaluating Solid Waste, Physical/Chemical Methods EPA SW-846 [Version 2 (December 1997), Integrated Manual through Update III] Washington DC, U.S. Environmental Protection Agency (1997)

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 005

Sediment Extraction Method (PAH and OCs)

Sediment samples are either immediately processed or stored frozen (- 20°C) until processing. A sediment aliquot is dried in a convection oven at 40°C. After the sediment is dry is it thoroughly homogenized using a ceramic motar and pestle. An additional aliquot of approximately 1 g of wet sediment is removed and dried in an oven at 105°C to a constant weight to determine % moisture. Samples are extracted using a Dionex ASE200 Accelerated Solvent Extractor (ASE). The dried sample is loaded into 22 or 33 mL stainless steel ASE extraction tubes. The extractions are performed using 100% dicholormethane at 100 °C and 2000 psi. The extracted organics dissolved in the solvent are collected in 60 mL glass vials. The extract is concentrated to approximately 10 mL in the collection vials and then transferred to 25 mL Kurdena-Danish (KD) concentrator tubes. The sample extract is concentrated to 3 mL in a water bath at 55-60°C. If extractable organic material weight is required, a 100 mL aliquot is removed and weighed using a microbalance. Interfering non-contaminant organic materials must be removed prior to instrument analyses.

The extract is processed through silica gel/alumina chromatography columns. The sample extract is loaded on top of 300 mm x 19 mm glass liquid chromatography columns packed with 10 g of deactivated alumina and 20 g of deactivated silica gel. The columns are loaded in 100 % dichloromethane. The dichloromethane is replaced by adding 40 mL of pentane. The extract is carefully added to the top of the chromatography columns. The column is flushed at a rate of 1-2 mL per minute using 200 mL of 50:50 pentane/dichloromethane and collected into 250 mL flasks. The eluent collected in the 250 mL flask is evaporated to 2 mL using a waterbath at 55-50°C. The samples is transferred into 2 mL amber vials. The concentrated extract is then analyzed by GC/MS for polynuclear aromatic hydrocarbons (PAHs) or GC/ECD for selected organochlorines (OCs).

Additional column chromatography is required to separate PCBs from toxaphene/pesticides when toxphene analysis is required and to separate planar PCBs. If toxaphene analyses is required, an aliquot of the extract after silica/alumina clean-up is processed through a 3% deactivated silica gel column. The column is packed in dicloromethane which is then flushed with 50 mL of pentane. The sample extract is transferred to the top of the column and flushed with 100 mL of pentane. The fraction contains PCBs and DDTs. The column is then flushed with 120 mL of 50:50 pentane/dichloromethane. This fraction contains toxaphene and chlorinated pesticides. Both fractions are reduced to 1 mL using a water bath at 55-60°C. The extracts are then ready for instrument analysis.

If planar PCB analyses are required, the PCB/DDT fraction prepared by 3% silica gel column is further processed by column chromatography packed with 2 g of 1:19 (5% by weight) mixture of activated carbon/Celite. The column and flushed with 25 mL of 1:4 dichloromethane/cyclohexane mixture. The sample is added to the top of the column and flushed with 50 mL of 1:4 dichloromethane/cyclohexane mixture, followed by 30 mL of 9:1 dichloromethane/toluene. This is followed by the addition of 40 mL of toluene. The toluene fraction contains the planar PCBs and is concentrated to 1 mL in a Zymark TurboVap II concentrator at 42°C and 20 psi. The sample is ready for instrument analysis.

References:

Lauenstein, G.G. and A.Y. Cantillo, ed. (1993). Sampling Analytical Methods of the National Status and Trends Program National Benthic Surveillance and Mussel Watch Projects 1984-1992; Volume IV: Comprehensive Descriptions of Trace Organic Analytical Methods. NOAA Technical memorandum NOS ORCA 71, Silver Spring, MD.

U.S. Environmental Protection Agency. 2001. National Coastal Assessment Quality Assurance Project Plan 2001-2004. United States Environmental Protection Agency, Office of Research and Development, National Health and Environmental Effects Research Laboratory, Gulf Ecology Division, Gulf Breeze, FL. EPA/620/R- 01/002.

Environmental Protection Agency, "Method 3545: Pressurized Fluid Extraction (PFE)," in Test Methods for Evaluating Solid Waste, Physical/Chemical Methods EPA SW-846 [Version 2 (December 1997), Integrated Manual through Update III] Washington DC, U.S. Environmental Protection Agency (1997)

Zuloaga, O.; Etxebarria, N.; Fernandez L. A.;Madariaga, J. M.; Optimization and comparison of MAE, ASE and Soxhlet extraction for the determination of HCH isomers in soil samples. Fresenius J Anal Chem, 200
0, 367, 733-737.

Schantz, M.; Nichols, J. J.; Wise, S. A.; Evaluation of Pressurized Fluid Extraction for the Extraction of Environmental Matrix Reference Material, Anal. Chem., 1997, 69, 4210-4219.

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 006

Total Organic and Inorganic Carbon is Soils and Sediments

Sediments samples are either immediately processed or stored frozen (- 20°C) until processing. A sediment aliquot is dried in a convection oven at 105°C. For total carbon analysis an aliquot of approximately 350 mg is placed in a clean, carbon-free combustion boat. The sample boats are loaded into a LECO autosampler rack assembly. The dried sample is combusted at 1350°C under an oxygen atmosphere in a LECO CR-412 Carbon Analyzer. Carbon present in the samples is oxidized to form CO2 gas. The gaseous sample flows through a nondispersive infrared (NIDR) detection cell. The mass of carbon dioxide is measured and converted to a percentage value with respect to sample weight. Percent total organic carbon is determined by pre- treating dry samples with 1:1 phosphoric acid to remove all inorganic carbon. Approximately 350 mg of treated sample is loaded into a clean, carbon-free combustion boat. The sample boats are loaded into a LECO autosampler rack assembly. The dried sample is combusted at 1350°C under an oxygen atmosphere in a LECO CR-412 Carbon Analyzer. Carbon present in the samples is oxidized to form CO2 gas. The gaseous sample flows through a nondispersive infrared (NIDR) detection cell. The mass of carbon dioxide is measured and converted to a percentage value with respect to sample weight.

References:

Kahn, Lloyd. 1988. Determination of total organic carbon is sediment. USEPA.

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 007

Determination of Particle Size Distribution in Sediments

Sediment samples are stored refrigerated at 4°C until processing. Samples are thoroughly mixed and an aliquot of approximately 25 to 50 g is weighed and placed into 750 mL wide-mouth jars. Approximately 250 mL of deflocculent solution (2.5 g/L sodium hexametaphosphate in DI water) is added to the jar. The jar is sealed and shaken until the sample is disaggregated. Once shaken the sample and deflocculent solution is poured through a 63 mm sieve into 1000 mL graduated cylinder. The coarse sediment left on top of the 63 mm sieve is concentrated into a 150 mL beaker. Deflocculent is added to 975 mL in the graduate cylinder. The coarse sediment in the beaker is dried in an oven at 70°C to 90°C. The weight is noted and then transferred to the top sieve (-1 phi) in a sieve stack that is arranged in descending order (-1 phi and +4 phi). The sieve stack is covered and shaken for 15 minutes on a sieve shaker. Empty the material from the top sieve onto a large piece of clean paper and weigh. The material from the next sieve is emptied onto the large piece of clean paper and weighed. Any material that passes through both sieves is added to the graduated cylinder. The phi fraction represents the gravel size and the + 4 phi represents the sand size. The silt/clay fraction is determined by filling the corresponding graduated cylinder to 1000 mL with deflocculent solution. After allowing the cylinder to stand for 24 hours at 24°C, the cylinder is thoroughly mixed. After 20 seconds a 25 mL aliquot is withdrawn from a depth of 20 cm (representing the silt fraction). The aliquot is emptied into a tared 50 mL beaker. A second 25 mL aliquot is withdrawn from the graduated cylinder froma depth of 10 cm at an interval of 2 hours and 3 minutes (representing the clay fraction) and placed into a tared 50 mL beaker. The 50 mL beakers are dried in an oven at 70°C to 90°C until dry. The dried samples are then weighed.

References:

APHA. 1989. Standard Methods for the Examination of Water and Wastewater. Clesceri, Greenberg, and Trussel, eds. American Public Health Association, 17th edition.

Folk, R.L. 1974. Petrology of Sedimentary Rocks. Hemphill Publishing Co., Austin, TX 184 pp.

Plumb, R.H. 1981. Procedure for Handling and Chemical Analysis of Sediment and Water Samples. Technical Report EPA/CE 81-1, prepared by Great Lakes Laboratory, State University College at Buffalo NY for the U.S. EPA/Corps of Engineers Technical Committee on Criteria for Dredged and Fill Material. Published by the U.S. Army Engineer Waterways Experiment Station, Vicksburg, MS.

Tetra Tech. 1986. Quality Assurance and Quality Control (QA/QC for 301 (h) Monitoring Programs. Guidance on Field and Laboratory Methods. USEPA, TC-3953-04, Final Report, 267 pp.

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 008

Determination of Total Petroleum Hydrocarbons in Soil/Sediment

Sediment samples are extracted as described in method 005. Total petroleum hydrocarbons (TPH) are determined by quantifying the TPH with gas chromatography/flame ionization detection (GC/FID)

TPH are analyzed using a HewelettPackard, model 5890 Gas Chromatograph (GC) with a Flame Ionization Detector (FID) operated in a splitless mode. A HP-1MS capillary column (30m x 0.25 mm ID and 0.25 mm film thickness) is used to resolve peaks. The carrier gas is helium at a flow rate of 1.5 mL/min. The temperature of the injection port is 300°C and transfer line is 300C. The initial oven temperature is 60°C, the ramp rate is 12°C/min to a final oven temperature of 180°C. For analytes of interest, a response factor relative to the internal standard is determined at each calibration level. All 5 response factors are averaged for a mean relative response factor. Data are surrogate corrected. TPH is determined by straight line integration between the retention times for n-C10 and n-C34.

Environmental Protection Agency, "Method 8100/8015. Polynuclear Aromatic Hydrocarbons/Nonhalogenated Organics using GC/FID"," in Test Methods for Evaluating Solid Waste, Physical/Chemical Methods EPA SW-846 [Version 2 (December 1997), Integrated Manual through Update III] Washington DC, U.S. Environmental Protection Agency (1997)

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 009

Determination of Aliphatic Hydrocarbons in Soil/Sediment

Sediment samples are extracted as described in method 005. Aliphatic hydrocarbons are determined by quantifying target analytes with a gas chromatography/flame ionization detection (GC/FID)

Aliphatic hydrocarbons are analyzed using a HewelettPackard, model 5890 Gas Chromatograph (GC) with a Flame Ionization Detector (FID) operated in a splitless mode. A HP-1MS capillary column (30m x 0.25 mm ID and 0.25 mm film thickness) is used to resolve peaks. The carrier gas is helium at a flow rate of 1.5 mL/min. The temperature of the injection port is 300°C and transfer line is 300C. The initial oven temperature is 60°C, the ramp rate is 12°C/min to a final oven temperature of 180°C. Normal alkanes with 10 to 34 carbons and the isoprenoids pristine and phytane are determined using this procedure. For analytes of interest, a response factor relative to the internal standard is determined at each calibration level. All 5 response factors are averaged for a mean relative response factor. Data are surrogate corrected.

Environmental Protection Agency, "Method 8100/8015. Polynuclear Aromatic Hydrocarbons/Nonhalogenated Organics using GC/FID"," in Test Methods for Evaluating Solid Waste, Physical/Chemical Methods EPA SW-846 [Version 2 (December 1997), Integrated Manual through Update III] Washington DC, U.S. Environmental Protection Agency (1997).

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 010

Volatile Organic Compounds (VOC) Determination by Purge and Trap Analysis with Gas Chromatography/Mass Spectrometry (GC/MS)

Volatile organic compounds (VOC) are introduced into a gas chromatograph by a purge-and-trap method (OI Corp Model 4560 with a DPM 16 Autosampler). The samples are purged with purified helium for 12 minutes and capturing VOC on a Tenax trap. The analytes are introduced directly to a narrow-bore capillary column by flash evaporation. The capillary column is temperature-programmed to separate the analytes. Resolved analytes are detected with a Thermo- Finnigan PolarisQ ion-trap mass spectrometer (MS) interfaced to the Thermo-Finnigan TRACE gas chromatograph (GC). The GC is operated in splitless mode and the capillary column is a J&W Scientific/Agilent Technologies DB-1 (60 m x 0.25-mm ID and 1.0 mm film thickness). The carrier gas is helium at a flow rate of 2 mL/minute. The temperature of the injection port is 175°C and transfer line is 290°C. The initial oven temperature is 45°C for 2 minutes, the ramp rate is 5°C/minutes to an oven temperature of 120°C and held for 0 minutes, then ramped at a rate of 10°C/minutes to a final oven temperature of 220°C and held for 5 minutes. For analyte identification, the extracted ion current profiles of the primary m/z and the confirmatory ion for each analyte must be at a maximum in the same scan or within one scan of each other and the retention time must fall with 5 seconds of the retention time of the authentic standard. The relative peak heights of the primary mass ion compared to the confirmation or secondary mass ion must fall within 30 % of the relative intensities of these masses in a reference mass spectrum.

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 011

Water Extraction Method (PAH and OC)

Water samples are either immediately processed or stored refrigerated (4 degrees C) until processing. The pH of samples is adjusted to <2 by the addition of 1 mL of hydrochloric acid. Samples are serially extracted using separatory funnels and dichloromethane. For a 1 L sample, 100 mL of dichloromethane is added. The sample is then shaken for three minutes. The organic layer is allowed to separate from the aqueous phase. The organic layer is drained into a 500 mL round bottom flask through a glass funnel containing a glass fiber filter and combusted sodium sulfate. This process is repeated twice more. The extract is concentrated to approximately 10 mL in the 500 mL round bottom flasks in a water bath at 55-60 degrees C and then transferred to 25 mL Kurdena-Danish (KD) concentrator tubes. The sample extract is concentrated to 3 mL in a water bath at 55-60 degrees C. If extractable organic material weight is required, a 100 micro litter aliquot is removed and weighed using a microbalance. Interfering non-contaminant organic materials may be removed prior to instrument analyses.

If the extract is colored then sample clean up may be required. The extract is processed through silica gel/alumina chromatography columns. The sample extract is loaded on top of 300 mm x 19 mm glass liquid chromatography columns packed with 10 g of deactivated alumina and 20 g of deactivated silica gel. The columns are loaded in 100 % dichloromethane. The dichloromethane is replaced by adding 40 mL of pentane. The extract is carefully added to the top of the chromatography columns. The column is flushed at a rate of 1-2 mL per minute using 200 mL of 50:50 pentane/dichloromethane and collected into 250 mL flasks. The eluent collected in the 250 mL flask is evaporated to 2 mL using a waterbath at 55-50 degrees C. The samples is transferred into 2 mL amber vials. The concentrated extract is then analyzed by GC/MS for polynuclear aromatic hydrocarbons (PAHs) or GC/ECD for selected organochlorines (OCs).

Additional column chromatography may be required to separate PCBs from toxaphene/pesticides when toxphene analysis is required and to separate planar PCBs. If toxaphene analyses is required, an aliquot of the extract after silica/alumina clean-up is processed through a 3% deactivated silica gel column. The column is packed in dicloromethane which is then flushed with 50 mL of pentane. The sample extract is transferred to the top of the column and flushed with 100 mL of pentane. The fraction contains PCBs and DDTs. The column is then flushed with 120 mL of 50:50 pentane/dichloromethane. This fraction contains toxaphene and chlorinated pesticides. Both fractions are reduced to 1 mL using a water bath at 55-60 degrees C. The extracts are then ready for instrument analysis.

If planar PCB analyses are required, the PCB/DDT fraction prepared by 3% silica gel column is further processed by column chromatography packed with 2 g of 1:19 (5% by weight) mixture of activated carbon/Celite. The column and flushed with 25 mL of 1:4 dichloromethane/cyclohexane mixture. The sample is added to the top of the column and flushed with 50 mL of 1:4 dichloromethane/cyclohexane mixture, followed by 30 mL of 9:1 dichloromethane/toluene. This is followed by the addition of 40 mL of toluene. The toluene fraction contains the planar PCBs and is concentrated to 1 mL in a Zymark TurboVap II concentrator at 42 degrees C and 20 psi. The sample is ready for instrument analysis.

References:

Lauenstein, G.G. and A.Y. Cantillo, ed. (1993). Sampling Analytical Methods of the National Status and Trends Program National Benthic Surveillance and Mussel Watch Projects 1984-1992; Volume IV: Comprehensive Descriptions of Trace Organic Analytical Methods. NOAA Technical memorandum NOS ORCA 71, Silver Spring , MD.

U.S. Environmental Protection Agency. 2001. National Coastal Assessment Quality Assurance Project Plan 2001-2004. United States Environmental Protection Agency, Office of Research and Development, National Health and Environmental Effects Research Laboratory, Gulf Ecology Division, Gulf Breeze, FL. EPA/620/R-01/002.

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Lab Name: TDI Brooks International, Inc. (TDI) Laboratory                                         Method Code 012

Polybrominated diphenyl ethers are analyzed in sample extracts by a Thermo Trace GC and DSQ-II MS operated in SIM using a capillary column. The GC is operated in splitless mode using a PTV injection port and the capillary column is an Agilent Technologies DB-XLB (15 m x 0.25 mm ID and 0.10 mm film thickness). The carrier gas is helium at a flow rate of 1 mL/minute and methane is used as the reactant gas with a flow rate of 2.0 mL/min. The temperature of the injection port is 40 degrees C (ramp to 300 degrees C) and transfer line is 290 degrees C. The initial oven temperature is 110 degrees C, the ramp rate is 7 degrees C/minutes to a final oven temperature of 280 degrees C and held for 20 minutes. For analyte identification, the extracted ion current profiles of the primary m/z and the confirmatory ion for each analyte must be at a maximum in the same scan or within one scan of each other and the retention time must fall with 5 seconds of the retention time of the authentic standard.