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Environmental Services, Inc. (HES) Laboratory Methods

Select one of the links blelow to display the method descriptions associated with HES.

Method Code

Method Title

001

Elemental Analysis by Inductively Coupled Plasma Spectroscopy

002

Mercury by Cold Vapor Atomic Absorption

003

Mercury in Water by Cold Vapor Atomic Absorption

004

Arsenic by Graphite Furnace

005

Arsenic in Water by Graphite Furnace

006

Selenium by Graphite Furnace

007

Selenium in Water by Graphite Furnace

008

Extraction by Separatory Funnel

009

Extraction by Sonication

010

Extraction by Soxhlet

011

Determination of Percent Lipids

012

Determination of Percent Moisture

013

Gel-Permeation Chromatography Cleanup

014

Florisil Cleanup - PCBs Only

015

Florisil Cleanup - Organochlorine Pesticides and PCBs

016

Florisil Cartridge Cleanup for PCBs and Pesticides

017

Silica Gel Cleanup and Separation

018

Sulfur Cleanup

019

Moisture Determination

020

GC Analysis for Organochlorine Pesticides and PCBs

021

Total Organic Carbon

022

Grain Size

 

 

 

 

 

Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 001

Elemental Analysis by Inductively Coupled Plasma Spectroscopy

SCOPE:

This method is applicable to plant and animal tissue, soil/sediment, and water.

Sample Preparation:

1) Plant and Animal Tissue

- Digest 5.00 g of tissue in Teflon vessel with 5 mL nitric acid in microwave digester. Transfer into 50 mL volumetric flask and dilute to volume with 0.005% Triton X-100 solution. Filter.

2) Soil/Sediment

- Digest 1.00 g in covered Teflon beaker on hot plate using 10 mL nitric acid. Add 30% hydrogen peroxide in 1 mL aliquots until effervescence no longer occurs. Add 1.25 mL hydrochloric acid, heat 10 minutes, and transfer to a 50 mL volumetric flask. Dilute to volume with DDI water. Filter.

3) Water

- Digest 100.0 mL sample in Teflon beaker on hot plate with 0.5 mL nitric acid and 2.5 mL hydrochloric acid. Reduce volume to 15 to 20 mL. Transfer into 50 mL volumetric flask. Dilute to volume with DDI water. Filter.

PRINCIPLE:

Each analyte concentration in the sample solution is determined by comparing its emission intensity with the emission intensities of a known series of analyte standards. The analytical wavelengths are tabulated with the raw concentration data. Analytical data is corrected for background and interfering element effects by the spectrometer program. The detection limit of each analyte is listed in the data report with each respective unknown value, it is a function of the instrument detection limit (IDL), and the sample mass and volume to which it is diluted. With each batch of 20 samples of the same matrix type, at least one duplicate, one sample spike, one analytical blank, and one appropriate reference material are assayed.

REFERENCES:

Test Methods for Evaluating Solid Waste - EPA Publication No. SW-846, 3rd edition, Methods (3030, 3040, or 3050) and 6010, US EPA, Washington DC (revised December 1987).

Dahlquist, R.L. and Knoll, J.W., "Inductively coupled Plasma - Atomic Emission Spectrometry: Analysis of Biological Materials and Soils for Major, Trace, and Ultra-Trace Elements," Applied Spectroscopy, 32 (1) 1-29 (January/February 1978).

Official Methods of Analysis - 14th Edition, method 43.292-43.296, AOAC: Arlington, Virginia (1984).

Official Methods of Analysis - 1st Supplement, 14th Edition, Method 3.A01-3.A04, AOAC, Arlington, Virginia (1985).

U.S. Environmental Protection Agency Contract Laboratory program, Statement of Work, Inorganic Analysis, Multimedia, Multi- concentration, S.O.W. 7/88.

"Inductively Coupled Plasma-Atomic Emission Spectrometric Method of Trace Element Analysis of Water and Wastes," Method 200.7, edited by Theodore D. Martin and John F. Kopp, U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory, Cincinnati, Ohio.

"Method Procedures, Analytical Chemistry Department, Inorganic Chemistry." Method MP-ICPS-MA, Hazleton Laboratories America, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 002

Mercury by Cold Vapor Atomic Absorption

SCOPE:

This method is applicable to most materials including animal tissues, plants, soils.

PRINCIPLE:

Sample weight: 2.00 g
Sample volume: 100 mL.

Samples are digested with a mixture of sulfuric and nitric acid. Mercury is reduced with sodium borohydride for determination. The amount of mercury is determined at a wavelength of 253.7 nm by comparing the signal of the unknown sample, measured by the atomic absorption spectrophotometer with the MHS-20 hydride generation unit, with the signal of the standard solutions.

Using a 2.0-g sample, the lowest detection limit of this assay is 0.025 ppm.

REFERENCES:

Digestion: Analyst, 86:608 (1961) with modifications.

Determination: Analytical Chemistry, 40:2085 (1968).

Test Methods for Evaluating Solid Waste, EPA Publication No. SW-846, 2nd Ed., Methods 3030, 3040 or 3050 and 7470, U.S. EPA: Washington, D.C. (revised April 1984).

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 003

Mercury in Water by Cold Vapor Atomic Absorption

SCOPE:

This method is applicable to drinking, surface, saline, and waste waters, and effluents.

PRINCIPLE:

Sample volume for digest: 50 mL
Final volume: 100 mL

Samples are digested with sulfuric acid, potassium permanganate, and potassium persulfate. Mercury is reduced with sodium borohydride for determination. The amount of mercury is determined at a wavelength of 253.7 nm by comparing the signal of the unknown sample, measured by the atomic absorption spectrophotometer with the MHS-20 hydride generation unit, with the signal of the standard solutions.

Using a 50-mL sample, the lowest detection limit of this assay is 0.0004 mg/L.

REFERENCES:

Method for Chemical Analysis of Water and Wastes, EPA Publication No. 600/4-79-020, Metals 1-19 and Method 245.2, U.S. EPA: Cincinnati, Ohio.

Test Methods for Evaluating Solid Waste, EPA Publication No. SW-846, 2nd Ed., Methods 3020 and 7470, U.S. EPA: Washington, D.C. (revised April 1984).

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 004

Arsenic by Graphite Furnace

SCOPE:

This method is applicable to animal tissues, plants, sediments, sludges, and soils.

SAMPLE PREPARATION:

1) Animal or Plant Tissue

- Digest 1.00 g with nitric acid in a microwave digestor. Transfer to 100 mL.

2) Sediment or Soil

- Digest 1.00 g with nitric acid and 30% hydrogen peroxide using covered glass beakers on hot plates. Transfer to 100 mL.

PRINCIPLE:

The amount of arsenic is determined at a wave length of 193.7 nm by comparing the signal of the unknown sample, measured by the graphite furnace atomic absorption spectrophotometer, with the signal of the standard solutions. The method of standard additions is used where interferences are indicated. Nickel matrix modification is employed in the analysis.

Using a 1.00-g sample, the lowest detection limit of this assay is 0.1 ppm.

REFERENCES:

Test Methods for Evaluating Solid Waste, EPA Publication No. SW-846, 2nd Ed., Methods 3030, 3040 or 3050 and 7060, U.S. EPA: Washington, D.C. (revised April 1984).

Contract Laboratory Program Statement of Work No. 785, Method 206.2 CLP-M, U.S. EPA: Cincinnati, Ohio.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 005

Arsenic in Water by Graphite Furnace

SCOPE:

This method is applicable to waters and aqueous wastes.

SAMPLE PREPARATION:

Sample volume: 25 mL (minimum)
Final volume: 25 mL

Digest the sample with nitric acid and 30% hydrogen peroxide using covered glass beakers and hot plates. Transfer to 25 mL.

PRINCIPLE:

The amount of arsenic is determined at a wavelength of 193.7 nm by comparing the signal of the unknown sample, measured by the graphite furnace atomic absorption spectrophotometer, with the signal of the standard solutions. The method of standard additions is used where interferences are indicated. Nickel matrix modification is employed in the analysis.

Using a 25-mL sample, the lowest detection limit of this assay is 1 mg/L.

REFERENCES:

Methods for Chemical Analysis of Water and Wastes, EPA Publication No. 600/4-79-020, Metals 1-19 and Method 206.2, U.S. EPA: Cincinnati, Ohio.

Test Methods for Evaluating Solid Waste, EPA Publication No. SW-846, 2nd Ed., Methods 3020 and 7060, U.S. EPA: Washington, D.C. (revised April 1984).

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 006

Selenium by Graphite Furnace

SCOPE:

This method is applicable to animal tissues, plants, sediments, sludges, and soils.

SAMPLE PREPARATION:

1) Animal or Plant Tissue

- Digest 1.00 g with nitric acid in a microwave digestor. Transfer to 100 mL.

2) Sediment or Soil

- Digest 1.00 g with nitric acid and 30% hydrogen peroxide using covered glass beakers on hot plates. Transfer to 100 mL.

PRINCIPLE:

The amount of selenium is determined at a wavelength of 196.0 nm by comparing the signal of the unknown sample, measured by the graphite furnace atomic absorption spectrophotometer, with the signal of the standard solutions. The method of standard additions is used along with nickel matrix modification in the analysis.

Using a 1.00-g sample, the lowest detection limit of this assay is 0.1 ppm.

REFERENCES:

Test Methods for Evaluating Solid Waste, EPA Publication No. SW-846, 2nd Ed., Methods 3030, 3040, or 3050 and 7740, U.S. EPA: Washington, D.C. (revised April 1984).

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 007

Selenium in Water by Graphite Furnace

SCOPE:

This method is applicable to waters and aqueous wastes.

SAMPLE PREPARATION:

Sample volume: 25 mL (minimum)
Final volume: 25 mL

Digest the sample with nitric acid and 30% hydrogen peroxide using covered glass beakers and hot plates. Transfer to 25 mL.

PRINCIPLE:

The amount of selenium is determined at a wavelength of 196.0 nm by comparing the signal of the unknown sample, measured by the graphite furnace atomic absorption spectrophotometer, with the signal of the standard solutions. The method of standard additions is used along with nickel matrix modification in the analysis.

Using a 25-mL sample, the lowest detection limit of this assay is 1 mg/L.

REFERENCES:

Methods for Chemical Analysis of Water and Wastes, EPA Publication No. 600/4-79-020, Metals 1-19, and Method 270.2, U.S. EPA: Cincinnati, Ohio.

Test Methods for Evaluating Solid Waste, EPA Publication No. SW-846, 2nd Ed., Methods 3020 and 7060, U.S. EPA: Washington, D.C. (revised April 1984).

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 008

Extraction by Separatory Funnel

SCOPE:

This method covers the extraction of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) in ground, surface, and waste waters.

SAMPLE PREPARATION:

Measure 1000 ml of aqueous sample and transfer to a two liter separatory funnel. Adjust the pH of the sample within the range of 5 to 9 using either 10 N sodium hydroxide or 1:1 sulfuric acid. Add 1.0 ml of the pesticide spiking solution to the matrix spike and the control spike. Add 500 ul of the 2,4,5,6-tetrachloro-mxylene (TMX) surrogate spiking solution to all samples and QC samples.

PROCEDURE:

Add 60 ml of methylene chloride to the separatory funnel, cap it and shake for two minutes. Allow the organic and aqueous layers to separate for about ten minutes and then drain the organic layer into a 250 ml erlenmeyer flask.

Repeat the above extraction two additional times with fresh portions of methylene chloride, combining the organic extracts in the erlenmeyer flask.

Pour the combined extract through a drying column containing enough anhydrous sodium sulfate to absorb any water. Drain the extract into a 500 ml Kuderna-Danish (K-D) flask fitted with a 10 ml concentrator tube. Attach a three ball snyder column to the K-D flask and concentrate the extract on a hot water bath, adjusting the temperature such that the concentration is completed within 15-20 minutes.

When the apparent volume reaches approximately 5.0 ml, remove the K-D apparatus from the water bath and allow to drain and cool for at least 10 minutes. Add 50 ml of hexane to the K-D flask and return to the hot water bath, concentrating the extract to 5.0 ml.

REFERENCES:

Environmental Protection Agency, "Test Methods for Evaluating Solid Waste - Physical/Chemical Methods - EPA Publication No. SW-846," Method 3510, Office of Solid Waste and Emergency Response, Washington, D.C. (September 1986)

"Determination of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) in Ground, Surface, and Waste Waters." Method MP-FWSW-MA, Hazleton Environmental Services, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 009

Extraction by Sonication

SCOPE:

This method covers the extraction of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) in soils and sediments.

SAMPLE PREPARATION:

Blend 20 grams of soil or sediment with 40 grams of anhydrous sodium sulfate in a 250 ml beaker. If there is not 20 grams of sample available, then remove at least one gram for percent moistures and weigh the remainder for extracting. For wet samples, more sodium sulfate may be required. If a sufficient amount has been added, the sample will appear granular. Add 1.0 ml of the pesticide spiking solution to the matrix spike and the control spike. Add 200 ul of the 2,4,5,6-tetrachloro-m-xylene (TMX) surrogate spiking solution to all samples and QC samples. Allow the soil/sediment and sodium sulfate to dry under a hood for a couple of hours, stirring it occasionally.

PROCEDURE:

Add 100 ml of methylene chloride:acetone (1:1). Place the ultrasonic probe 1/2 inch below the surface of the solvent but above the sediment layer and sonicate for 3 minutes using the 0.75 inch horn at full power with the pulse set at 50% duty cycle.

Decant and filter the extract through Whatman #4 filter paper into a 500 ml Kuderna-Danish (K-D) flask fitted with a 10 ml concentrator tube. Repeat the above extraction two more times with two additional 100 ml portions of methylene chloride:acetone (1:1) combining the resultant extracts.

Attach a three ball snyder column to the K-D flask and concentrate the extract on a hot water bath, adjusting the temperature such that the concentration is completed within 15-20 minutes.

When the apparent volume reaches approximately 5.0 ml, remove the K-D apparatus from the water bath and allow to drain and cool for at least 10 minutes. Bring up to a volume of 10 ml with methylene chloride if the sample is to be cleaned by GPC. It is recommended that GPC cleanup be used for very contaminated extracts. If the extract is not to be cleaned by GPC then exchange the solvent to hexane.

REFERENCES:

Environmental Protection Agency, "Test Methods for Evaluating Solid Waste - Physical/Chemical Methods - EPA Publication No. SW-846," Method 3550, Office of Solid Waste and Emergency Response, Washington, D.C. (September 1986)

"Determination of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) in Soils and Sediments." Method MP-FWSS-MA, Hazleton Environmental Services, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 010

Extraction by Soxhlet

SCOPE:

This method covers the extraction of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) in biological tissues.

SAMPLE PREPARATION:

Blend 20 grams of ground tissue with 40 grams of anhydrous sodium sulfate in a 250 ml beaker. If there is not 20 grams of sample available the remove at least one gram for percent moistures and weigh the remainder for extracting. For

wet samples, more sodium sulfate may be required. If a sufficient amount has been added the sample will appear granular. Add 1.0 ml of the pesticide spiking solution to the matrix spike and the control spike. Add 200 ul of the 2,4,5,6-tetrachloro-m-xylene (TMX) surrogate spiking solution to all samples and QC samples. Allow the ground tissue/sodium sulfate to dry under a hood for a couple of hours, stirring it occasionally.

PROCEDURE:

Load the prepared sample into the soxhlet extractor between two plugs of pre-extracted glass wool. Place 250 ml of methylene chloride into a pre-rinsed 500 ml erlenmeyer flask containing three to five teflon boiling chips. Attach the flask to the extractor. Add 100 ml of methylene chloride to the mixing beaker, swirl, and add the solvent to the extractor prior to attaching the condenser. Adjust the temperature of the heating mantle so that the extractors cycle at a rate of 12 to 15 cycles per hour. Allow the system to cycle for 16 to 20 hours.

Allow the extract to cool after the extraction is complete. Rinse the condenser with extraction solvent and drain the soxhlet apparatus into the bottom collection flask.

Pour the extract through a Whatman #4 filter into a 500 ml K-D flask fitted with a 10 ml concentrator tube. Attach a three-ball snyder column to the K-D flask and concentrate the extract on a hot water bath, adjusting the temperature so that the concentration is completed within 15 to 20 minutes.

When the apparent volume reaches approximately 5.0 ml, remove the K-D apparatus from the water bath and allow it to drain and cool for at least 10 minutes. Bring up to a volume of 10 ml with methylene chloride.

REFERENCES:

Environmental Protection Agency, "Test Methods for Evaluating Solid Waste - Physical/Chemical Methods - EPA Publication No. SW-846," Method 3540, Office of Solid Waste and Emergency Response, Washington, D.C. (September 1986)

"Determination of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) in Biological Tissues." Method MP-FWST-MA, Hazleton Environmental Services, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 011

Determination of Percent Lipids

SCOPE:

This method covers the gravimetric determination of percent lipids in biological tissue samples.

PROCEDURE:

One milliliter of the 10 ml extract is placed into a preweighed aluminum weighing pan. The pan is allowed to sit lightly covered in a hood overnight to allow the solvent to evaporate. The pan is then weighed again. The following equation is then used to calculate the percent lipid:

((weight(g) of pan + lipid) - weight(g) of pan) x 10 ml x 100 = %lipid

------------------------------------------------------------------------------------

grams extracted

REFERENCES:

"Determination of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) in Biological Tissues." Method MP-FWST-MA, Hazleton Environmental Services, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 012

Determination of Percent Moisture

SCOPE:

This method covers the gravimetric determination of percent moisture in soil, sediment and biological tissue samples.

PROCEDURE:

One to 10 g of the sample is placed into a preweighed aluminum weighing pan. The pan is weighed again with the sample in it. The pan and sample are then placed into an oven at 105 C for 16 hours. The sample is allowed to cool in a desiccator and then weighed again. The following equation is used to calculate the percent moisture:

((mass(g) pan + wet sample) - (mass(g) pan + dry sample))x100=% moisture

------------------------------------------------------------------------------------------------

grams of sample

If samples are to be calculated based on dry weight, the percent moisture is converted to a correction factor (M). The calculation of the factor is:

100 / (100 - % moisture) = M

REFERENCES:

Environmental Protection Agency, "Test Methods for Evaluating Solid Waste - Physical/Chemical Methods - EPA Publication No. SW-846," Method 3550, Office of Solid Waste and Emergency Response, Washington, D.C. (September 1986)

"Determination of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) in Soils and Sedients." Method -FWSS-MA, Hazleton Environmental Services, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 013

Gel-Permeation Chromatography Cleanup

SCOPE:

This method covers the cleanup of soil, sediment and biological extracts by gel-permeation chromatography (GPC).

PROCEDURE:

After extraction, the sample extracts are concentrated in Kuderna- Danish (K-D) apparatus and the volume is adjusted to 10 ml with methylene chloride. Five milliliters of this extract is then injected on an ABC Laboratories Model 1002B GPC system using a column packed with 70 g of S-X3 Bio-beads and methylene chloride as the carrier solvent. A dump, collect, and rinse cycle is then run which is consistent with exhibit D, section 7.1 of reference 1 below.

The collected fraction is then quantitatively transferred to a 500 ml K-D apparatus fitted with a 10 ml concentrator tube. A three ball snyder column is attached and the extract is concentrated on a hot water bath, adjusting the temperature such that the concentration is completed within 15-20 minutes.

When the apparent volume reaches approximately 5.0 ml, the K-D apparatus is removed from the water bath. 50 ml of hexane is added to the flask and it is returned to the hot water bath and the extract is concentrated to 5.0 ml.

REFERENCES:

USEPA Contract Laboratory Program, "Statement of Work for Organic Analysis, multi-media, multi-concentration", Document number OLMOl.O (March 1990) including revisions OLMOl.l (December l990 and OLM01.2 (January 1991)

"Determination of Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs) in Biological Tissues." Method MP-FWST-MA, Hazleton Laboratories America, Inc., Madison, Wisconsin.

Instrument Operating Procedure for Gel-Permeation Chromatograph, Method OP-6004-36, Hazleton Environmental Services, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 014

Florisil Cleanup - PCBs Only

SCOPE:

This method is applicable to any sample extract in hexane that requires additional cleanup before determination of polychlorinated biphenyls (PCBs) only. It does not apply when analyzing for organochlorine pesticides.

SAMPLE PREPARATION:

The sample extract should be at a volume of 5.0 ml in hexane.

PROCEDURE:

To a Florisil column, 19 mm id x 300 mm length with a 300 ml reservoir, is added a plug of glass wool, 20 g of Florisil and topped with 2 cm of anhydrous sodium sulfate. The Florisil is prerinsed with 150 ml of petroleum ether, taking the solvent down to the top of the sodium sulfate.

The sample extract is added to the column and drawn down to the top of the sodium sulfate. The column is then eluted with 250 ml petroleum ether at the rate of approximately 5 ml/minute. A single fraction is collected in a 500 ml erlenmeyer flask as the column is allowed to run dry.

The collected fraction is then quantitatively transferred to a 500 ml K-D apparatus fitted with a 10 ml concentrator tube. A three ball snyder column is attached and the extract is concentrated on a hot water bath, adjusting the temperature such that the concentration is completed within 15-20 minutes.

When the apparent volume reaches approximately 5.0 ml, the K-D apparatus is removed from the water bath and allowed to cool for at least 10 minutes. 50 ml of hexane is added to the flask and it is returned to the hot water bath and the extract is concentrated to 5.0 ml.

This method is the same as that in reference 1 except:

a) the Florisil is rinsed with 150 ml petroleum ether instead of 60 ml hexane.

b) the sample extract is eluted with 250 ml of petroleum ether and only one fraction is collected.

c) the florisil is not activated before use.

REFERENCES:

Environmental Protection Agency, "Test Methods for Evaluating Solid Waste - Physical/Chemical Methods - EPA Publication No. SW-846," Method 3620, Office of Solid Waste and Emergency Response, Washington, D.C. (Septeber 1986)

"Florisil Cleanup of Samples for PCBs", Method OP-6004-37, Hazleton Environmental Services, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 015

Florisil Cleanup - Organochlorine Pesticides and PCBs

SCOPE:

This method is applicable to any sample extract in hexane that requires additional cleanup before determination of organochlorine pesticides and polychlorinated biphenyls (PCBs).

SAMPLE PREPARATION:

The sample extract should be at a volume of 5.0 ml in hexane.

PROCEDURE:

To a Florisil column, 19 mm id x 300 mm length with a 300 ml reservoir, is added a plug of glass wool, 20 g of Florisil and topped with 2 cm of anhydrous sodium sulfate. The Florisil is prerinsed with 150 ml of petroleum ether, taking the solvent down to the top of the sodium sulfate.

The sample extract is added to the column and drawn down to the top of the sodium sulfate. The column is then eluted with 250 ml of a mixed solvent containing 1% ethanol, 49% diethyl ether, and 50% petroleum ether at the rate of approximately 5 ml/minute. A single fraction is collected in a 500 ml erlenmeyer flask as the column is allowed to run dry.

The collected fraction is then quantitatively transferred to a 500 ml K-D apparatus fitted with a 10 ml concentrator tube. A three ball snyder column is attached and the extract is concentrated on a hot water bath, adjusting the temperature such that the concentration is completed within 15-20 minutes.

When the apparent volume reaches approximately 5.0 ml, the K-D apparatus is removed from the water bath and allowed to cool for at least 10 minutes. 50 ml of hexane is added to the flask and it is returned to the hot water bath and the extract is concentrated to 5.0 ml.

This method is the same as that in reference 1 except:

a) the Florisil is rinsed with 150 ml petroleum ether instead of 60 ml hexane.

b) the sample extract is eluted with 250 ml of a mixed solvent containing 1% ethanol, 49% diethyl ether, and 50% petroleum ether and only one fraction is collected.

REFERENCES:

Environmental Protection Agency, "Test Methods for Evaluating Solid Waste - Physical/Chemical Methods - EPA Publication No. SW-846," Method 3620, Office of Solid Waste and Emergency Response, Washington, D.C. (September 1986)

"Florisil Cleanup of Samples for Organochlorine Pesticides and PCBs", Method OP-6004-37, Hazleton Environmental Services, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 016

Florisil Cartridge Cleanup for PCBs and Pesticides

SCOPE:

This method is applicable to extracts which require additional cleanup prior to the determination of PCBs and Pesticides.

SAMPLE PREPARATION:

The sample extract should be in hexane.

PROCEDURE:

A florisil cartridge is placed onto a vacuum manifold and at least 5.0 ml of a hexane/acetone (90:10) rinse is pulled through the cartridge. A 1.0 ml sample extract is placed on the cartridge and eluted through it with 10 ml of hexane acetone (90:10). The extract is concentrated to the desired volume under a gentle stream of nitrogen.

REFERENCES:

USEPA Contract Laboratory Program, "Statement of Work for Organic Analysis, multi-media, multi concentration", Document number OLM01.0 (March 1990) including subsequent revisions.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 017

Silica Gel Cleanup and Separation

SCOPE:

This method is applicable to any sample extract in hexane which requires additional cleanup and the separation of polychlorinated biphenyls (PCBs) from many of the organochlorine pesticides.

SAMPLE PREPARATION:

The sample extract should be at a volume of 5.0 ml in hexane.

PROCEDURE:

The silica gel (100/200 mesh) is prepared by swirling it in a slurry of 40% acetonitrile and 60% methylene chloride, vacuum filtering, and then rinsing it successively with methylene chloride and hexane. It is then dried at 140 C overnight and deactivated with 0.5% (w/v) distilled water.

Fifteen grams of this silica gel is then slurried in petroleum ether, poured into a chromatography column, and topped with anhydrous sodium sulfate. The sample extracts are then drawn into the top of the column. The first fraction is eluted with 140 ml petroleum ether. The second fraction is eluted with 250 ml of a mixture of 1% acetonitrile, 19% hexane, and 80% methylene chloride (v/v).

The first fraction should include all PCBs, p,p'-DDE, hexachlorobenzene, and mirex. It may also include some portion of p,p'-DDT, o,p'-DDE, o,p'-DDT, and trans-nonachlor. The remaining portion of these 4 pesticides, along with all other organochlorine pesticides, will be found in the second fraction.

Both fractions are then quantitatively transferred to a 500 ml K-D apparatus fitted with a 10 ml concentrator tube. A three ball snyder column is attached and the extract is concentrated on a hot water bath, adjusting the temperature such that the concentration is completed within 15-20 minutes.

When the apparent volume reaches approximately 5.0 ml, the K-D apparatus is removed from the water bath and allowed to cool for at least 10 minutes. 50 ml of hexane is added to the flask and it is returned to the hot water bath. If the extract was cleaned by gel- permeation chromatography (GPC), it is concentrated to 5.0 ml. If it did not undergo GPC cleanup then it is concentrated to 10.0 ml.

REFERENCES:

Technical Operating Procedure, "Silica Gel Cleanup and Separation of Organochlorine Pesticides and PCBs", Method OP-6004-45, Hazleton Environmental Services, Inc., Madison, Wisconsin.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 018

Sulfur Cleanup

SCOPE:

This method is applicable to any sample extract which requires removal of sulfur before determination of organochlorine pesticides and/or polychlorinated biphenyls (PCBs) by gas chromatography.

PROCEDURE:

The sample extract is placed in a Teflon-sealed vial and 1 to 3 drops of mercury are added. The vial is then vigorously agitated on a vortex shaker for approximately 30 seconds. If a black precipitate forms, it is set aside and allowed to settle. The sample extract is then drawn off with a disposable pipet and transferred to a clean vial. This procedure is repeated until there is no formation of the precipitate.

REFERENCES:

Environnental Protection Agency, "Test Methods for Evaluating Solid Waste - Physical/Chemical Methods - EPA Publication No. SW-846," Method 3660, Office of Solid Waste and Emergency Response, Washington, D.C. (September 1986)

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 019

Moisture Determination

SCOPE:

This method is applicable to plant tissue, animal tissue, and soil/sediment.

PRINCIPLE:

The prepared sample is weighed in to a tared aluminum dish and is dried in an oven to constant weight (approximately 12-18 hours) at 100 C.

SENSITIVITY:

This method is capable of detecting 0.1% moisture.

REFERENCES:

Official Methods of Analysis, 15th Ed., Methods 926.08, 925.09, Assoc. of Off. Analytical Chemists, Arlington, VA (1990) modified.

USEPA Contract Laboratory Program, Statement of Work for Inorganics Analysis, Exhibit D, S.O.W. 3/90, Document No. ILMO1.0.

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 020

GC Analysis for Organochlorine Pesticides and PCBs

PROCEDURE:

All extracts are analyzed using gas chromatography with an electron capture detector. The sample extracts are analyzed and compared with external standards for qualitative and quantitative purposes. If the extract has been separated into a pesticide and a PCB fraction using silica gel, then each fraction is analyzed only for those analytes expected in the fraction.

Pesticide Analysis

The pesticides are analyzed on a gas chromatograph with dual wide-bore capillary columns and two electron capture detectors. An initial injection of an evaluation mixture containing 4,4'-DDT and endrin is made. Breakdown of the 4,4'-DDT into 4,4'-DDD and 4,4'-DDE and/or endrin into endrin ketone and endrin aldehyde must not exceed 20%.

Calibration standards are analyzed followed by the sample extracts. Ongoing standards are injected after a maximum of ten samples to verify the system is still within specifications. Sample chromatograms are compared to the standard chromatograms to identify peaks which match on two different GC columns. Identified pesticides are quantified using the initial standards.

PCB Analysis:

The individual PCBs are identified by pattern recognition. Individual PCB quantification is done by summing the areas of at least five sample peaks and also summing the same five peaks in the initial standard closest in area to the sample (for example, the A standard of Aroclor 1242, if the amount of Aroclor 1242 in the sample is near the detection limit). Total PCBs are obtained by summing the individual Aroclors present in the sample extract.

REFERENCES:

United States Environmental Protection Agency (EPA) Method 608, Federal Register, 49, (209):43321-43336, (October 16, 1984).

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 021

Total Organic Carbon

Total Organic Carbon

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Lab Name: Environmental Services, Inc. (HES) Laboratory                     Method Code: 022

Grain Size

Grain Size

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