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Analytical Control Facility (ACF) Laboratory Methods

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

Method Code

Method Title

001

Organophosphate/Carbamate Scanning for Tissue and Sediment

002

Organophosphate/Carbamate Scanning for Water

003

Aromatic Hydrocarbons for Sediment

004

Organochlorines for Tissue

005

Organochlorines for Sediment

006

ICP Scan for Water

007

ICP Scan for Tissue

008

ICP Scan for Soil/Sediment

009

Arsenic and Selenium for Tissue

010

Arsenic and Selenium for Water

011

Arsenic and Selenium for Sediment

012

Mercury for Sediment and Tissue

013

Total Suspended Solids (TSS)

014

Aluminum In Water

015

HGA: Sediment

016

Plant and Animal Tissues For Organochlorine Pesticides, Co-Planar and Other PCBs.

017

Mercury

018

Quantifying PCB Aroclors

020

Percent Moisture

021

Temephos in Water

022

Temephos in Soil/Sediment

023

Temephos in Tissue

024

Total Organic Carbon

025

Grain Size Analysis

026

White Phosphorus In Tissue

027

ICP Scan-Tissue

028

HGA Analytes in Tissue

029

Mercury in Tissue

030

Percent Lipid Determinations

031

Moisture by Freeze Drying

032

Total Petroleum Hydrocarbon in Soils/Sediments

033

Total Petroleum Hydrocarbon in Tissue

034

Percent Food Content in Digestive Tract

035

Temephos (Abate) in Tissue, Plants, Water and Sediment.

036

ICP-MS Scan Tissue

 

 

 

 

 

Lab Name: Analytical Control Facility                     Method Code: 001

Analytical Methodology for Organophosphate/Carbamate Scanning
for Tissue and Sediment

This method involves homogenization of the sample followed by mixing with acetone and methylene chloride to separate the pesticides from the tissue. The organic extract is filtered and adjusted to volume prior to gas chromatography using a flame photometric detector for organophosphate determinations and a nitrogenphosphorus detector for carbamate determinations. Magabore capillary columns are used for the GC separations.

Reference:

1.   Patuxent Wildlife Research Center, Analytical Chemistry Group SOP Organophosphate/Carbamate Scanning Method (0-25.00). April 28, 1989.

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Lab Name: Analytical Control Facility                     Method Code: 002

Analytical Methodology for Organophosphate/Carbamate Scanning for Water

The extraction procedure was a modified version of the one described in the EPA test Method #608, Section 10 (1). The water samples were extracted three times with methylene chloride (all containers were rinsed three times as well). The methylene chloride extracts were combined, dried with sodium sulfate and concentrated on a rotary evaporator. Sample extracts were refrigerated prior to analysis. Residues were quantified by gas chromatography using either an instrument selective for organophosphate pesticides (Flame Photometric Detector) or one selective for carbamate pesticides (Nitrogen Phosphorus Detector) similar to Belisle et al. (1988) (2). Megabore capillary columns were used for the GC separation.

References

1.    EPA test Method #608, Section 10. (sample extraction) 1982.

2.   Belisle, A.A., and D.M. Swineford. 1988. Simple, specific analysis of organophosphorous and carbamate pesticides in sediments using column extraction and gas chromatography. Environ. Toxicol. Chem. 7(9):749-752.

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Lab Name: Analytical Control Facility                     Method Code: 003

Analysis for Aromatic Hydrocarbons for Sediment

Ten gram homogenized aliquots of sediment were mixed with sodium sulfate and placed into a glass Soxhlet extraction thimble. Prior to extraction 1.6 ug of each of the following deuterated internal (surrogate) aromatic hydrocarbon standards were added to sample: d8 napthalene, d10 acenapthylene, d10 phenanthrene, d12 chrysene, and d12 perylene. These internal standards wereused to quantitate the aromatic hydrocarbon residues. Samples were extracted in the same manner as for pesticides (Cromartie et. al., 1975) except that petroleum ether was used instead of hexane as an extracting solvent. After extraction samples were concentrated to 10 mL using an air stream and treated with gel permeation chromatography (GPC) for cleanup. Samples were then concentrated to 1 mL and 1 mL of 1 ppm pyrene-d10 was added as a GC internal standard in order to monitor the recoveries of deuterated PAHs. Samples were quantified by GC/MS using Selective Ion Monitoring (Wade et al., 1988).

The GC/MS used was a Hewlett Packard 5970 MSD and 5890 gas chromatograph equipped with a 59970 ChemStation computer data system. The GC column used was a 50m bonded methyl phenyl (5%) silicone column, 0.32 ID, 0.25 micron film thickness. The GC conditions were: injection port - 300oC, transfer line 280oC. Temperature program: Initial temperature 100oC for 1 min followed by 7oC/min to 290oC and hold for 40 min.

Calibration is accomplished by integration of single ions characteristic of each compound using the five deuterated internal standards. The compounds, ions used, and standards used are shown below:

Compound Ion Standard Ion

Naphthalene

128

Naphthalene-d8

136

Acenaphthylene

152

Acenaphthylene-d10

164

Acenaphthene

154

Acenaphthylene-d10

164

Fluorene

166

Acenaphthylene-d10

164

Phenanthrene

178

Phenanthrene-d10

188

Anthracene

178

Phenanthrene-d10

188

Fluoranthene

202

Phenanthrene-d10

188

Pyrene

202

Chrysene-d12

240

Benzo(a)anthr.

228

Chrysene-d12

240

Chrysene

228

Chrysene-d12

240

Benzo(b)Fluor.

252

Perylene-d12

264

Benzo(k)Fluor.

252

Perylene-d12

264

Benzo(e)pyrene

252

Perylene-d12

264

Benzo(a)pyrene

252

Perylene-d12

264

Perylene

252

Perylene-d12

264

Indeno(123cd)per.

276

Perylene-d12

264

Benzo(ghi)per.

276

Perylene-d12

264

Dibenzo(ah)anth.

278

Perylene-d12

264

The lower detection limit is 0.01 ppm based on a 10 g sample wet weight.

References

1.   Cromartie, E.W., W.L. Reichel, L.N. Locke, A.A. Belisle, T.E. Kaiser, T.G. Lamont, B.M. Mulhern, R.M. Prouty, and D.M. Swineford. 1975. Residues of organochlorine pesticides and polychlorinated biphenyls and autopsy data for Bald Eagles, 1971-72. Pestic. Monit. J. 9:11-14.

2.   Wade, T.L., Atlas, E.L., Brooks, J.M., Kennicutt, M.C. II, Fox, R.G., Sericano, J., Garcia, B. and Defreitas, D. 1988. NOAA Gulf of Mexico Status and Trends Program: Trace organic contaminant distribution in sediments and oysters. Estuaries 11, 171-179.

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Lab Name: Analytical Control Facility                     Method Code: 004

Analytical Methodology for Organochlorines for Tissue

The analytical methods, including preparation, Soxhlet extraction, and lipid removal are described by Cromartie et al., 1975. Glass extraction thimbles were used. The silica gel separation of the pesticides from PCBs was different from the above reference in that four fractions were used instead of three to enable the separation of dieldrin and endrin from the rest of the pesticides. The pesticides in each fraction were quantified with a gas-liquid chromatograph (GLC), equipped with a 63Ni electron capture detector. The GLC column used was a 30m MEGABORE coated with a 1.0 micron film of 7% cyanopropyl 7% phenyl polysiloxane. Residues in 10% of the samples were confirmed by gas chromatography/mass spectrometry (GC/MS). The nominal lower limit of detection is 0.01 ppm for pesticides and 0.05 ppm for PCBs based on a 10 g aliquot wet weight.

Reference

1.   Cromartie, E.W., W.L. Reichel, L.N. Locke, A.A. Belisle, T.E. Kaiser, T.G. Lamont, B.M. Mulhern, R.M. Prouty, and D.M. Swineford. 1975. Residues of organochlorine pesticides and polychlorinated biphenyls and autopsy data for Bald Eagles, 1971-72. Pestic. Monit. J. 9:11-14.

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Lab Name: Analytical Control Facility                     Method Code: 005

Analytical Methodology for Organochlorines for Sediment

The Soxhlet extraction procedure was a modified version of the one described by Cromartie et al. (1975). Ten gram aliquots of moist soil were mixed together in activated florisil and ignited sea sand. The samples were then placed into a glass extraction thimble and extracted eight hours via Soxhlet extraction using an 8/1/1 hexane - acetone - methanol solution. The extracts were then extracted three times with water and the organic layers were then combined and cleaned up with florisil (Cromartie et. al.). The pesticides were separated from the PCBs using silica gel column chromatography as described by the above reference except that two fractions were used instead of three (Pesticide and PCB). Samples were quantified by a gas-liquid chromatograph (GLC), equipped with a 63Ni electron capture detector. The GLC column used was a 30m MEGABORE coated with a 1.0 micron film of 7% cyanopropyl 7% phenyl polysiloxane. Residues were confirmed in one of the samples by gas chromatography/mass spectrometry (GC/MS).

Reference

1.   Cromartie, E.W., W.L. Reichel, L.N. Locke, A.A. Belisle, T.E. Kaiser, T.G. Lamont, B.M. Mulhern, R.M. Prouty, and D.M. Swineford. 1975. Residues of organochlorine pesticides and polychlorinated biphenyls and autopsy data for Bald Eagles, 1971-72. Pestic. Monit. J. 9:11-14.

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Lab Name: Analytical Control Facility                     Method Code: 006

Analytical Methodology for ICP Scan for Water

ICP analyses were performed using the instrumental conditions recommended by the manufacturer (1). 100 grams of water was combined with 10 mL of concentrated nitric acid and evaporated gently in a teflon beaker to approximately 10 mL. Contents were then transferred to a 20 mL polypropylene centrifuge tube. 100 uL of 10,000 ppm scandium solution was added. The final volume of the tube was brought up to 20 mL with reverse phase osmosis deionized water. The analyses were performed using a Perkin Elmer Plasma II sequential inductively coupled plasma emission spectrometer.

Reference

1.   Perkin Elmer Corporation. 1985. Plasma II Emission Spectrometer. Vol. 1-3.

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Lab Name: Analytical Control Facility                     Method Code: 007

Analytical Methodology for ICP Scan for Tissue

ICP analyses were performed using the dry ash procedure described by Haseltine et al., 1981 (1) and the instrumental conditions recommended by the manufacturer (2). Up to 5 grams of tissue were weighed into a Vycor crucible (for other metals except boron) or a Coors crucible (boron only). The crucible was placed in a drying oven overnight at 105oC for moisture determination. After weighing the dried material, the crucible was then placed in a muffle furnace. The temperature was set at 200oC and was raised at a rate of 50oC per hour until the temperature was at 550oC. After ashing overnight the residues were dissolved in nitric and hydrochloric acids and transferred to a 15 mL polypropylene centrifuge tube. 500 micrograms of a scandium internal standard was added and the sample diluted to 10 mL with reverse osmosis deionized water. The analyses were performed using a Perkin Elmer Plasma II sequential inductively coupled plasma emission spectrometer.

Reference

1.   Haseltine, S.D., G.H. Heinz, W.L. Reichel, and J.F. Moore. 1981. Organochlorine and Metal Residues in Eggs of Waterfowl Nesting on Islands in Lake Michigan Off Door County, Wisconsin. Pestic. Monit. Jour. 15(2):90-97.

2.   Perkin Elmer Corporation. 1985. Plasma II Emission Spectrometer. Vol. 1-3.

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Lab Name: Analytical Control Facility                     Method Code: 008

Analytical Methodology for ICP Scan for Soil/Sediment

ICP analyses were performed using a 3:1 hydrochloric acid:nitric acid digestion procedure and the instrumental conditions recommended by the manufacturer (1). One gram aliquots were placed into 300 mL teflon beakers and 20 mL of 3:1 hydrochloric acid:nitric acid were added. Approximately 11 mL of acid was slowly evaporated off via hot plate. The sample was then transferred into a 50 mL centrifuge tube and 100 uL of 10,000 ppm scandium solution was added. The final volume of the tube was brought up to 20 mL with reverse phase osmosis deionized water. The analyses were performed using Perking Elmer Plasma II sequential inductively coupled plasma emission spectrometer.

Reference

1.   Perkin Elmer Corporation. 1985. Plasma II Emission Spectrometer. Vol. 1-3.

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Lab Name: Analytical Control Facility                     Method Code: 009

Analytical Methodology for Arsenic and Selenium for Tissue

Samples were analyzed for selenium and arsenic according to the method described by Krynitsky (1987). A 0.5 gram fresh weight aliquot of tissue was used for digestion in 5 ml of nitric acid. Determination was by Stabilized Temperature Platform Graphite Furnace Atomic Absorption Spectroscopy using Zeeman effect background correction. The nominal detection limit was 0. 1 ppm on a wet weight basis.

Reference

1.   Krynitsky, A.J. 1987. Preparation of biological tissue for determination of arsenic and selenium by graphite furnace atomic absorption spectrometry. Analytical Chemistry 59(14):1884-1886.

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Lab Name: Analytical Control Facility                     Method Code: 010

Analytical Methodology for Arsenic and Selenium for Water

Water samples were analyzed for selenium and arsenic in a similar way as described by Krynitsky (1987). However, 100 grams of water was combined with 10 mL of concentrated nitric acid and evaporated gently in a teflon beaker to a final volume of 20 mL. Determination was by Stabilized Temperature Platform Graphite Furnace Atomic Absorption Spectroscopy using a Perkin-Elmer Zeeman Model 3030 Graphite Furnace.

Reference

1.   Krynitsky, A.J. 1987. Preparation of biological tissue for determination of arsenic and selenium by graphite furnace atomic absorption spectrometry. Analytical Chemistry 59(14):1884-1886.

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Lab Name: Analytical Control Facility                     Method Code: 011

Analytical Methodology for Arsenic and Selenium for Sediment

Sediment samples were analyzed for selenium and arsenic according to the method described by Krynitsky (1987). A 0.5 gram fresh weight aliquot of sediment was used for digestion in 5 mL nitric acid and 0.5 mL of 30% hydrogen peroxide. However, the sediment samples needed further treatment with 5 mL hydrofluoric acid in order to free the analyte from the silicates. Determination was by Stabilized Temperature Platform Graphite Furnace Atomic Absorption Spectroscopy using a Perkin-Elmer Zeeman Model 3030 Graphite Furnace. The nominal detection limit was 0.1 ppm based on a 0.5 g wet weight basis.

Reference

1.   Krynitsky, A.J. 1987. Preparation of biological tissue for determination of arsenic and selenium by graphite furnace atomic absorption spectrometry. Analytical Chemistry 59(14):1884-1886.

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Lab Name: Analytical Control Facility                     Method Code: 012

Analytical Methodology for Mercury for Sediment and Tissue

One gram aliquots were digested under reflux in sulfuric and nitric acids as described by Monk. The determination was performed by cold vapor atomic absorption spectrophotometry using a Spectro Products mercury analyzer equipped with a Varian VGA-76 vapor generation accessory. The nominal lower limit of detection is 0.05 ppm on a wet weight basis.

Reference

1.   Monk, H.E. 1961. Recommended methods of analysis of pesticide residues in food stuffs. Report by the Joint Mercury Residue Panel. Anal. 82:608-614.

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Lab Name: Analytical Control Facility                     Method Code: 013

Analytical Methodology for Total Suspended Solids (TSS)

Preweigh empty beaker. Add 20gm of the sample to a tared beaker. Allow the aliquot to go to dryness.

TSS = weight of beaker + aliquot weight - weight of empty beaker.

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Lab Name: Analytical Control Facility                     Method Code: 014

Aluminum In Water

Summary: Water samples were analyzed for aluminum. 100 grams of water was combined with 10 ml of concentrated nitric acid and evaporated gently in a teflon beaker to a final volume of 20 ml. Determination was by Stabilized Temperature Platform Graphite Furnace Atomic Absorption Spectroscopy using a Perkin-Elmer Zeeman Model 3030 Graphite Furnace. The nominal detection limit was 0.0005 ppm based on a 100 gram sample of water.

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Lab Name: Analytical Control Facility                     Method Code: 015

HGA: Sediment

Sediment samples were prepared according to the method described by Krynitsky (1987). A 0.5-1.0 gram fresh weight aliquot was used for sample digestion in 5 ml of nitric acid and approximately 500 ul of 30% hydrogen peroxide was added to remove excess organic matter. The sample tubes and graphite furnace cups were prewashed in dilute nitric and hydrochloric acid prior to use. Determination was by Stabilized Temperature Platform Graphite Furnace Atomic Absorption Spectroscopy.

Reference:

1.   Krynitsky, A.J. 1987. Preparation of biological tissue for determination of arsenic and selenium by graphite furnace atomic absorption spectrometry. Analytical Chemistry 59(14):1884-1886.

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Lab Name: Analytical Control Facility                     Method Code: 016

Procedures for Analyzing Plant and Animal Tissues For
Organochlorine Pesticides, Co-Planar and Other PCBs.

The preparation methods include those described by Cromartie et al., 1975. The co-planar method was described by Chia-Swee Hong and Brian Bush at the Wadsworth Center for Laboratories and Research. Homogenized animal or plant tissue is extracted with a 6% ethyl ether/hexane mixture. The extract is cleaned up on a florisil column by eluting with the 6% ethyl/hexane mixture. The PCB fraction is separated from the other compounds by silica gel column chromatography. Non-ortho and mono-ortho PCB co-planars are separated from other PCB congeners by HPLC using a column of 1:12 mixture of activiated carbon and silica gel. The pesticides and PCBs in each fraction are quantified with a gas liquid chromatography (GLC), equipped with a 63 Ni electron capture detector. The GLC column used with a 30m Megabore, coated with 1.0 micron film of 7% cyano propyl, 7% phenyl polysiloxane. Co-planars and other PCBs are analyzed on Ultra-2, 50m, I.D. 0.20 mm, film thickness 0.33 microns. Residues in 10% of the samples were confirmed by gas chromatography/mass spectrometry (GC/MS). The nominal lower limit of detection is 0.01 ppm for pesticides 0.05 ppm for PCBs and 0.005 ppm for co-planar PCBs on a 10g aliquot wet weight.

Reference

1.   Cromartie, E.W., W.L. Reichel, L.N. Locke, A.A. Belisle, T.E. Kaiser, T.G. Lamont, B.M. Mulhern, R.M. Prouty, and D.W. Swineford. 1975. Residues of Organochlorine Pesticides and Polychlorinated Biphenyls and Autopsy Data for Bald Eagles, 1971-72. Pest. Mont. J. 9:11-14.

2.   Chemosphere, Vol. 21, Nos. 1-2, pp. 173-181, 1990 (Printed in Great Britain).

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Lab Name: Analytical Control Facility                     Method Code: 017

Analytical Methodology For Mercury

One half to one gram of tissue or sediment homogenate or 10 grams for water was digested under reflux in sulfuric and nitric acids as described by Monk. The mercury determination was by cold vapor atomic absorption spectroscopy as described by Hatch and Ott modified for use with a Perkin Elmer Atomic Absorption Spectrophotometer 3100 equipped with a Perkin Elmer FIAS 200.

Reference

1.   Monk, H.E. 1961. Recommended methods of analysis of pesticide residues in food stuffs. Report by the Joint Mercury Residue Panel. Anal., 86:608-614.

2.   Hatch, W.R., and W.L. Ott. 1968. Determination of submicrogram quantities of mercury by atomic absorption spectrophotometry. Perkin Elmer Corporation Manual. April 1991. Flow Injection Analysis System.

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Lab Name: Analytical Control Facility                     Method Code: 018

Quantifying PCB Aroclors

Samples were extracted by Soxhlet extraction with hexane, cleaned up by Florisil and silica gel fractionation per Kaiser et al. (1980). Limits of detection were 0.01 ppm for OC pesticides and 0.05 ppm for PCBs. Four sectors of the chromatogram were used to estimate the total amount of Aroclors 1242, 1248, 1254, and 1260 in the sample. The amount of 1242, e.g., was estimated by comparison with Aroclor 1242 using decachlorobiphenyl as an internal standard. The amount of 1242 standard represented by its selected area e.g., was calibrated by quantifying the percent of the total area of 1242 that was located in its selected sector and multiplying this value by the total amount of 1242 injected.

Reference

1.   Kaiser, T.E., W.L. Reichel, L.N. Locke, E. Cromartie, A.J. Krynitsky, T.G. Lamont, B.M. Mulhern, R.M. Prouty, and D.M. Swineford. 1980. Organochlorine pesticides, PCB, and PBB residues and necropsy data for bald eagles from 29 states -- 1975-1977. Pesticides Monitoring Journal 13:145-149.

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Lab Name: Analytical Control Facility                     Method Code: 020

Analytical Methodology for Percent Moisture

Preweigh pan. Add aliquot to tared pan. Allow sample to dry 24 hours in an oven at 200 degrees Fahrenheit. Samples are then placed in a desiccator to cool. Record pan + dry weight.

                        Percent Moisture = 1 - (pan + dry - pan weight / original aliquot) * 100.

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Lab Name: Analytical Control Facility                     Method Code: 021

Temephos in Water

The entire sample, including the container, was extracted by shake-out with 3x100 ml portions of methylene chloride. The extracts were pooled, concentrated, cleaned up by Florisil column chromatography, and analyzed by gas chromatography on a DB-1 megabore column using a flame photometric detector.

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Lab Name: Analytical Control Facility                     Method Code: 022

Temephos in Soil/Sediment

A 10 gram sample is mixed with 10 or more grams of sand and 20 or more grams of Sodium Sulfate. The mixture is added to a chromatography column over a 40 gram bed of Sodium Sulfate. The column is eluted with a 200ml mixture of 1:1 Acetone/Methylene Chloride at a rate of 5ml/min. The 200ml mixture is captured in round bottom flask, fitted to a Rota- Evap and concentrated to approximately25ml. The 25ml extract is transferred to a beaker with several rinses of Methylene Chloride and further concentrated to approximately 5ml in a warm water bath held at 45oC. The extract is transferred to a mills tube and diluted to a final volume of 10 ml. The extract is analyzed by Gas Chromatography/Flame Photometric Detection.

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Lab Name: Analytical Control Facility                     Method Code: 023

Temephos in Tissue

This method involves homogenization of the sample followed by mixing with acetone and methylene chloride to separate the pesticides from the tissue. The organic extract is filtered, cleaned up by Florisil column chromatography, and adjusted to volume prior to gas chromatography using a flame photometric detector for organophosphate determinations. DB-1 megabore capillary columns are used for the GC separations.

Reference

1.   Patuxent Wildlife Research Center, Analytical Chemistry Group SOP Organophosphate/Carbamate Scanning Method (0-25.00). April 28, 1989.

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Lab Name: Analytical Control Facility                     Method Code: 024

Total Organic Carbon

Total Organic Carbon (TOC) is determined by chemical oxidation of the organic carbon of a sample in an ampule. The sample is acidified, persulfate is added and the sample is purged of Total Inorganic Carbon (TIC). The ampule is sealed and placed in a oven or water bath. The strong oxidant quickly reacts with organic carbon at 100 C to CO2. When the oxidation is complete, the ampule is broken and the CO2 is purged, concentrated by trapping, desorbed, and carried into a non- dispersive infrared detector (NDIR). The measured mass of CO2 is equal to the mass of TOC in the sample.

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Lab Name: Analytical Control Facility                     Method Code: 025

Grain Size Analysis

A 15 to 20 gram homogenized sample is placed in a large glass jar. The sample is treated with 50 to 100 ml of Hydrogen Peroxide to oxidize organic matter. The sample is washed with distilled water to remove soluble salts. 400 ml of Sodium Hexametaphosphate (5.5g/L) is added to disperse the sample. The sample is shaken for 24 hours. After shaking, the sample is filtered through a 62.5 micron screen into a 1000 ml graduated cylinder. The sample is rinsed with dispersant in order that all fine-grain sediment is washed into the cylinder. This separates the gravel sand fraction (on the screen) from the silt/clay fraction (in the cylinder). The coarse fraction is washed into a pre-weighed beaker with distilled water and placed in a 100 degree oven for 24 hours. The sample is allowed to cool. The sample is weighed and weights recorded on the data sheets.

The silt/clay size material is determined by settling. A graduated cylinder is filled to exactly 1 liter. The sample is stirred and left to stand for one day. The sample is stirred vigorously. After removing the stirring rod, a 20 ml aliquot is taken from a depth of 20 cm after 20 seconds. This is the 4 phi aliquot and the total weight of the silt + clay fraction. The aliquot is placed in a pre-weighed beaker. At the 2 hour and 3 minute time another 20 ml aliquot is taken at the 10 cm depth. This is the 8 phi aliquot. Pipette the suspension into a different pre-weighed beaker. The beakers are dried overnight and cooled. The beakers are weighed, and the percent sand, silt, and clay fractions are determined.

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Lab Name: Analytical Control Facility                     Method Code: 026

White Phosphorus In Tissue

A 10-g sample of tissue is placed into a 120-ml vial or jar containing 10.0 ml of isooctane and 10.0 ml of degassed water. The sample is vortex-mixed for 1 min., then placed horizontally on a platform shaker for 18 hr. or overnight. The sample is then allowed to stand vertically for 15 min. to allow phase separation. A 3.0-ul aliquot of the isooctane layer is analyzed on gas chromatograph equipped with a nitrogen-phosphorus detector.

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Lab Name: Analytical Control Facility                     Method Code: 027

Analytical Methodology for ICP Scan-Tissue

Summary: Samples were lyophilized using a Labconco, Freeze Dry System, Model 7756. A one half to one gram aliquot of freeze dried aliquot was digested in 10 ml ultrapure nitric acid and 4 ml of 30% hydrogen peroxide using an OI Model 7301 Microwave Digestion System. After digestion a scandium internal standard was added. The analyses were performed using a Perkin Elmer Plasma II sequential inductively coupled plasma emission spectrometer.

Reference

1.   Labconco, Freeze Dry System Model 77560 Instruction Manual 1993.

2.   OI Analytical, Microwave Model 7301, Instruction Manual 1992.

3.   Perkin Elmer Corporation Manual. 1985. Plasma II Emission Spectrometer. Vol. 1-3.

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Lab Name: Analytical Control Facility                     Method Code: 028

Analytical Methodology For HGA Analytes in Tissue

Summary: Samples were lyophilized using a Labconco, Freeze Dry System Model 77560. A one half to one gram freeze dried aliquot was digested in 10 ml of ultrapurenitric acid and 4 ml of 30% hydrogen peroxide using an OI Analytical Model 7301 Microwave digestion System. Determination was by Stabilized Temperature Platform Graphite Furnace Atomic Absorption Spectroscopy using a Perkin Elmer Zeeman 3030 Atomic Absorption Spectrophotometer.

Reference

1.   Labconco, Freeze Dry System Model 77560 Instruction Manual 1993.

2.   OI Analytical, Microwave Model 7301, Instruction Manual 1992.

3.   Atomic Spectroscopy. Vol. 4 #3, "Recent Experiences with the Stabilized Temperature Platform Furnace and Zeeman Background Correction ." Slavin, W., G.R. Carnrick, D. C. Manning, and E. Pruszkowska.

4.   Perkin Elmer Corporation Manual. Atomic Absorption Spectrophotometer, Zeeman 3030.

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Lab Name: Analytical Control Facility                     Method Code: 029

Analytical Methodology for Mercury in Tissue

Summary: Samples were lyophilized using a Labconco, Freeze Dry System Model 77560. A one half to one gram aliquot of freeze dried tissue was digested in 10 ml ultrapure nitric acid and 4 ml of 30% hydrogen peroxide using an OI Analytical 7301 Microwave digestion System. The mercury determination was by cold vapor atomic absorption spectroscopy as described by Hatch and Ott modified for use with a Perkin Elmer Atomic Absorption Spectrophotometer 3100 equipped with a Perkin Elmer FIAS 200.

Reference

1.   Labconco, Freeze Dry System Model 77560 Instruction Manual 1993.

2.   OI Analytical, Microwave Model 7301, Instruction Manual 1992.

3.   Hatch, W.R., and W.L. Ott, 1968. Determination of submicrogram quantities of mercury by atomic absorption spectrophotometry.

4.   Perkin Elmer Corporation Manual. April 1991. Flow Injection Analysis System.

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Lab Name: Analytical Control Facility                     Method Code: 030

Percent Lipid Determinations

Summary: A portion of the extracted lipid solution is placed on a pre- weighed aluminum pan. The solvent is evaporated from pan and the pan is reweighed. The percent lipid is calculated accordingly as described in detail below.

Calculations:

    PE = Pan Empty

    PF = Pan Full after solvent has been evaporated

    AL = Sample Aliquot

    % Lipid = [(PF - PE) * 10 / AL) * 100

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Lab Name: Analytical Control Facility                     Method Code: 031

Analytical Methodology Moisture by Freeze Drying

Summary: Empty sample jars and their lids were weighed(WEIGHT1). Up to 20 G of sample homogenate were weighed(WEIGHT2) into each jar. Samples were lyophilized using a Labconco, Freeze Dry System Model 77560. After drying, the samples, their jars and lids were weighed(WEIGHT3).

                        Percent Moisture = (1 - (WEIGHT3 - WEIGHT1) / WEIGHT2) * 100.

Reference

1.   Labconco, Freeze Dry System Model 77560 Instruction Manual 1993.

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Lab Name: Analytical Control Facility                     Method Code: 032

Total Petroleum Hydrocarbon in Soils/Sediments

A 10-g sample of soil/sediment is mixed with anhydrous sodium sulfate placed in an extraction thimble and extracted with methylene chloride using a soxhlet extractor. The extract is dried and concentrated for analysis. The extract is analyzed by Gas Chromatography/Flame Ionization Detection. The resulting capillary column profile is compared against hydrocarbon standards used to identify and calculate the TPH concentrations.

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Lab Name: Analytical Control Facility                     Method Code: 033

Total Petroleum Hydrocarbon in Tissue

A 1-10g sample of tissue (depending on lipid content) is mixed with anhydrous sodium sulfate, placed in an extraction thimble and extracted with Methylene Chloride using a soxhlet extractor. The extract is concentrated and put on a florisil column. The column is eluted with 200 ml of Methylene Chloride and concentrated for analysis. The extract is analyzed by Gas Chromatography/Flame Ionization Detection. The resulting capillary column profile is compared against hydrocarbon standards using to identify and calculate the TPH concentrations.

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Lab Name: Analytical Control Facility                     Method Code: 034

Percent Food Content in Digestive Tract

Digestive tract samples are laid on a bench for thawing. After thawing, the digestive tract is carefully observed and a visual estimate is made as to what volume may be food.

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Lab Name: Analytical Control Facility                     Method Code: 035

Temephos (Abate) in Tissue, Plants, Water and Sediment.

Summary: A sample aliquot is extracted, dried with sodium sulfate, concentrated , cleaned up on Florisil with methylene chloride, and concentrated again for GC/FPD analysis as follows:. Water (about 800-1000 mls) is extracted with 3x 100 mls methylene chloride, filtered and dried with Na2SO4. For tissue, sediment, and plant material, a 10 g aliquot of tissue or sediment or 5 g of (less dense) homogenized plant material is placed in a 50 ml centrifuge tube and extracted by sonication with 3 x 20 mls of a 1:1 mixture of acetone: methylene chloride, filtered and dried with Na2SO4. Tissue, plant extracts, and "dirty" water and sediment extracts showing dark-colored coextracted material (e.g. from pond water) are cleaned up on Florisil using methylene chloride. GC analysis using flame photometric detection is performed on a megabore (0.53 mm I.D.) column of DB-1 or equivalent programmed from 150 C to 235 C.

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Lab Name: Analytical Control Facility                     Method Code: 036

Analytical Methodology for ICP-MS Scan Tissue

Samples were analyzed using a microwave digestion procedure with ICP-MS determination. Tissues were lyophilized using a Labconco Freeze Dry System Model 7730. A one half to one gram sample of the freeze dried tissue was digested in 10 ml ultrapure nitric acid and 4 ml of 30% hydrogen peroxide using an IO Model 7301 Microwave Digestion System. The final volume was brought to 25 ml with reverse osmosis deionized water. The analyses were performed using a Perkin Elmer Elan 6000 Inductively Coupled Plasma Mass Spectrometer with conditions recommended by the manufacturer.

Reference

1.   Labconco Freeze Dry System Model 7756 Instruction Manual. 1993.

2.   OI Analytical Microdigest Model 7301 Instruction Manual. 1992.

3.   Perkin Elmer Corporation Manual. 1998. Elan 6000 Inductively Coupled Plasma Mass Spectrometer Software Guide and Update Kit.

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