Midwest Research Institute (MRI) Laboratory Methods

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Lab Name: Midwest Research Institute                     Method Code: 001

Analytical Methodology for Mercury in Sediment

Summary: A 0.2 gram fresh weight aliquot is digested in sulfuric and nitric acids at 95oC for two minutes then cooled. Potassium permanganate and hydroxylamine sulfate are added to the digestate and the sample is returned to the water bath for an additional 30 minute digestion at 95oC. Excess permanganate is reduced with potassium persulfate and the sample is diluted to 200 mL. The determination is performed by cold vapor atomic absorption using a PSA Merlin Plus mercury analyzer. The nominal detection limit is 0.2 ug/g.

Reference:

U.S. Environmental Protection Agency, Office of Water Regulations and Standards, Method 1620, Draft, September 1989.

U.S. Environmental Protection Agency, Contract Laboratory Program Statement of Work for Inorganics Analysis of Multi-Media Multi- Concentration Samples, Document No. ILM03.0.

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Lab Name: Midwest Research Institute                     Method Code: 002

Analytical Methodology for Mercury in Tissue

Summary: A 0.5 gram aliquot of wet homogenized tissue is digested in sulfuric and nitric acids at 60oC for one hour. Potassium permanganate and hydroxylamine sulfate are added to the digestate and the sample is returned to the water bath for an additional 30 minute digestion at 95oC. Excess permanganate is reduced with potassium persulfate and the sample is diluted to 200 mL. The determination is performed by cold vapor atomic absorption using a PSA Merlin Plus mercury analyzer. The nominal detection limit is 0.08 ug/g on a wet weight basis.

Reference:

Methods For The Determination of Metals in Environmental Samples, Environmental Monitoring Systems Laboratory, Office Of Research and Development, U.S. Environmental Protection Agency, Report No. EPA-600/4-91-010 (1991) Method 245.6.

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Lab Name: Midwest Research Institute                     Method Code: 003

Analytical Methodology for Mercury in Water

Summary: A 100 mL aliquot of water is digested using sulfuric acid, nitric acid, potassium permanganate, and potassium persulfate for one hour in a 95oC water bath. Excess permanganate is reduced with sodium chloride-hydroxylamine sulfate persulfate and the sample is diluted to 200 mL. The determination is performed by cold vapor atomic absorption using a PSA Merlin Plus mercury analyzer. The nominal detection limit is 0.2 ug/L.

Reference:

Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Governmental Printing Office, Washington, DC, SW-846, Method 7470 (1986).

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Lab Name: Midwest Research Institute                     Method Code: 004

Analytical Methodology for ICP Scan for Water

Summary: 100 mL of water is combined with 10 mL of concentrated nitric acid and evaporated gently to approximately 10 mL(1). The contents are transferred to a 100 mL volumetric flask and diluted to volume using Milli-Q reagent grade water. The analyses are performed using a Thermo Jarrell Ash Model 61E simultaneous inductively coupled plasma emission spectrometer (2).

Reference:

(1) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Governmental Printing Office, Washington, DC, SW-846,

Method 3020 (1986).

(2) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 6010A (1986).

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Lab Name: Midwest Research Institute                     Method Code: 005

Analytical Methodology for ICP Scan for Sediment

Summary: A one gram aliquot for dried coarsely ground soil is transferred to a beaker and metals are extracted using nitric acid and hydrogen peroxide (1). The contents are transferred to a 100 mL volumetric flask and diluted to volume using reagent grade water. The analyses are performed using a Thermo Jarrell Ash Model 61E simultaneous inductively coupled plasma emission spectrometer (2).

Reference:

(1) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office,

Washington , DC , SW-846, Method 3050A (1986).

(2) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 6010A (1986).

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Lab Name: Midwest Research Institute                     Method Code: 006

Analytical Methodology for ICP Scan for Tissue

Summary: A one gram aliquot of freeze dried coarsely ground sample is weighed and digested using nitric acid and hydrogen peroxide (1). The contents are transferred to a 100 mL volumetric flask and diluted to volume using reagent grade water. The analyses are performed using a Thermo Jarrell Ash Model 61E simultaneous inductively coupled plasma emission spectrometer (2).

Reference:

(1) Methods For The Determination Of Metals in Environmental Samples, Environmental Monitoring Systems Laboratory, Office Of Research and Development, U.S. Environmental Protection Agency, Report No. EPA-600/4-91-010 (1991) Method 245.6.

(2) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 6010A (1986).

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Lab Name: Midwest Research Institute                     Method Code: 007

Analytical Methodology for Arsenic and Selenium in Tissue

Summary: A one gram aliquot of freeze dried coarsely ground sample is weighed and digested using nitric acid and hydrogen peroxide (1). The contents are transferred to a 100 mL volumetric flask and diluted to volume using reagent grade water. The analyses are performed using Varian SpectrAA Graphite Furnace Zeeman Corrected single element atomic absorption spectrometer (2).

Reference:

(1) Methods For The Determination Of Metals In Environmental Samples, Environmental Monitoring Systems Laboratory, Office Of Research And Development, U.S. Environmental Protection Agency, Report No. EPA- 600/4-91-010 (1991) Method 200.3.

(2) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 7000 (1986).

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Lab Name: Midwest Research Institute                     Method Code: 008

Analytical Methodology for Arsenic and Selenium in Water

Summary: 100 mL of water is combined with 10 mL of concentrated nitric acid and evaporated gently to approximately 10 mL (1). The contents are transferred to a 100 mL volumetric flask and diluted to volume using reagent grade water. The analyses are performed using a Varian SpectrAA Graphite Furnace Zeeman Corrected single element atomic absorption spectrometer (2).

Reference:

(1) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 3020.

(2) Test Methods for Evaluating Solid Waste, Physical/chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 7000 (1986).

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Lab Name: Midwest Research Institute                     Method Code: 009

Analytical Methodology for Arsenic, Selenium and Cadmium in Soil

Summary: A one gram aliquot of the dried soil is transferred to a beaker and metals are extracted using nitric acid and hydrogen peroxide (1). The contents are transferred to a 100 mL volumetric flask and diluted to volume using reagent grade water. The analyses are performed using a Varian SpectrAA Graphite Furnance Zeeman Corrected single element absorption spectrometer (2).

Reference:

(1) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 3050A (1986).

(2) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 7000 (1986).

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Lab Name: Midwest Research Institute                     Method Code: 010

Homogenization and Moisture Determination of Tissue

Summary: Samples of tissue are homogenized by grinding the sample twice in a Hobart auger-fed grinder. A vessel is preweighed (vessel weight) and an aliquot of the homogenized tissue is weighed in the tared vessel (aliquot weight). The sample is then lyophilized and a vessel + lyophilized tissue weight is recorded. The tissue is ground to a coarse powder with a glass rod.

Percent Moisture = [1 - (vessel + lyophilized tissue - vessel weight/aliquot weight)] X 100

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Lab Name: Midwest Research Institute                     Method Code: 011

Homogenization and Moisture Determination of Sediments

Summary: A suitable vessel is preweighed (vessel weight) and an aliquot of sediment sample is added to the tared vessel (aliquot weight). The sample is allowed to dry for 24 hours in an oven at 105oC. After drying the sample is placed in a dessicator to cool. The vessel + dry sample weight is recorded.

The dried sample is transferred to a mortar and pestle for grinding. The ground sample is passed through a #10 sieve (2.0 mm mesh size).

Percent Moisture = [1 - (vessel + dry weight - vessel weight/aliquot weight)] X 100

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Lab Name: Midwest Research Institute                     Method Code: 012

Analytical Methodology for ICP Scan for Water using Microwave Digestion

Summary: A 45-mL of aliquot of water is digested in 5 mL of concentrated nitric acid in a heavy duty microwave vessel for 20 minutes using a CEM MDS 2100 microwave system (1). The contents are transferred to a 50-mL centrifuge tube for analysis. Analyses are performed using a Thermo Jarrell Ash Model 61E simultaneous inductively coupled plasma emission spectrometer (2).

Reference:

(1) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, Integrated Manual, Final Update III, June 1997, Method 3015 Revision 1.

(2) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, SW-846 Method 6010A (1986).

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Lab Name: Midwest Research Institute                     Method Code: 013

Analytical Methodology for Selenium in Water by Hydride Atomic Absorption

Summary: A 50 mL aliquot of a well-mixed, acid-preserved sample is transferred to abeaker and digested with nitric and sulfuric acids. The selenium in a 10-mL aliquot of the digestate is then converted to a volatile hydride with hydrogen produced from a sodium borohydride reaction (1). Selenium absorption is measured using a GBC 902 atomic emission/absorption spectrometer with deuterium background correction. Selenium concentration is proportional to the absorbance of the signal (2).

Reference:

(1) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, Integrated Manual, Final Update III, June 1997, Method 7741-A, Revision 1.

(2) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, SW-846 Method 7000 (1986).

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Lab Name: Midwest Research Institute                     Method Code: 014

Analytical Methodology for Selenium in Soil by Hydride Atomic Absorption

Summary: A one gram aliquot of the dried soil is transferred to a beaker and metalsare extracted using nitric acid and hydrogen peroxide (1). A 50 mL aliquot the extract is transferred to a beaker and digested with nitric and sulfuric acid. The selenium in a 10-mL aliquot of the digestate is then converted to a volatile hydride with hydrogen produced from a sodium borohydride reaction (2). Selenium absorption is measured using a GBC 902 atomic emission/absorption spectrometer with deuterium background correction. Selenium concentration is proportional to the absorbance of the signal (3).

Reference:

(1) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 3050A (1986).

(2) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, Integrated Manual, Final Update III, June 1997, Method 7741A, Revision 1.

(3) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 7000 (1986).

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Lab Name: Midwest Research Institute                     Method Code: 015

Analytical Methodology for GFAA Analysis of Arsenic, Selenium and Cadmium in Water using Microwave Digestion

Summary: A 45-mL of aliquot of water is digested with 5 mL of concentrated nitric acid in a heavy duty microwave vessel for 20 minutes using a CEM MDS 2100 microwave system (1). The contents are transferred to a 50-mL centrifuge tube for analysis. Analyses are performed using a Varian SpectrAA Graphite Furnace Zeeman Corrected single element atomic absorption spectrometer (2).

Reference:

(1) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, Integrated Manual, Final Update III, June 1997, Method 3015 Revision 1

(2) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Edition, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, SW-846 Method 7000 (1986)

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Lab Name: Midwest Research Institute                     Method Code: 016

Analytical Methodology for Total Cyanide in Sediment

Summary: Approximately 1-gram of wet sample is added to 50 mL of reagent water. Any deviation from the target weight of 1 gram is accounted for in the calculation. The cyanide, as hydrocyanic acid (HCN), is released from samples containing cyanide by means of a reflux-distillation operation under acidic conditions and absorbed in a scrubber containing sodium hydroxide solution. The cyanide concentration in the absorbing solution is then determined colorimetrically. The estimated detection limit for the method is 1 mg/Kg.

Reference:

Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, Final Update III, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 9010B (Revision 2, 1996).

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Lab Name: Midwest Research Institute                     Method Code: 017

Analytical Methodology for Total Organic Carbon in Sediment/Soil

Summary: Organic carbon is measured in sediment/soil using a carbonaceous analyzer. This instrument converts the organic carbon in a sample to carbon dioxide (CO2) by either catalytic combustion or wet chemical oxidation. Carbon is converted to CO2 by means of a high temperature combustion furnace in the sediment/soil matrix. The amount of sample will vary dependent on the total organic carbon concentration.

References:

(1) Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, Final Update III, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, U.S. Government Printing Office, Washington, DC, SW-846, Method 9060 (Revision 0, 1986).

(2) Methods for Chemical Analysis of Water and Wastes, U.S. Environmental Protection Agency, EPA-600/4-79-020 (Revised March 1983), Method 415.1.

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Lab Name: Midwest Research Institute                     Method Code: 018

Analytical Methodology for Grain Size in Sediment/Soil

Summary: This method covers the quantitative determination of the distribution of particle sizes in sediment/soil. The distribution of particle sizes larger than 75 ?m is determined by sieving, while the distribution of particle sizes smaller than 75 ?m is determined by a sedimentation process, using a hydrometer.

Reference: American Society for Testing and Materials, ASTM D422-63 (Reapproved 1998).

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Lab Name: Midwest Research Institute                     Method Code: 019

Tissue Percent Moisture Determination (Oven-Drying Method)

Summary: A suitable vessel is preweighed (vessel weight) and an aliquot of tissue sample is added to the tared vessel (aliquot weight). The sample is allowed to dry for 24 hours in an oven at 105oC. After drying the sample is placed in a desiccator to cool. The vessel plus dry sample weight is recorded.

% Moisture = [1 - ((vessel plus dry weight - vessel weight)/aliquot weight)] X 100

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Lab Name: Midwest Research Institute                     Method Code: 020

Analytical Method for Mercury in Water by FIMS CVAAS

Summary: A 25-mL aliquot is digested using sulfuric acid, nitric acid, potassium permanganate and potassium persulfate for 2 hours at 95C in a heating block. Excess permanganate is reduced with sodium chloride/hydroxylamine hydrochloride and the sample is diluted to 50 mL. Mercury is reduced with stannous chloride to elemental mercury and measured by cold vapor atomic absorption spectroscopy (CVAAS) using a Perkin Elmer FIMS mercury analyzer, or equivalent. The nominal detection limit is 0.2 ug/L

References:

Method 245.1 Determination of Mercury in Water by Cold Vapor Atomic Absorption Spectrometry. Rev 3.0, EMMC Version. Methods for the Determination of Metals in Environmental Samples, Supplement 1. United States Environmental Protection Agency, Office of Research and Development, Washington DC 20460 . EPA/600/R-94/111.

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Lab Name: Midwest Research Institute                     Method Code: 021

Analytical Method for Mercury in Sediment by FIMS CVAAS

Summary: A 0.2-g aliquot of dry sediment is digested with aqua regia at 95*C for 2 minutes. Potassium permanganate is added and the sample is digested for an additional 30 minutes. Excess permanganate is reduced with sodium chloride/hydroxylamine hydrochloride and the sample is diluted to 50 mL. Mercury is reduced with stannous chloride to elemental mercury and measured by cold vapor atomic absorption spectroscopy (CVAAS) using a Perkin Elmer FIMS mercury analyzer, or equivalent. The nominal detection limit is 0.05 ug/g on a dry weight basis.

References:

Method 245.5 Determination of Mercury in Sediments by Cold Vapor Atomic Absorption Spectrometry. Rev 2.3, April 1991. Methods for the Determination of Metals in Environmental Samples. United States Environmental Protection Agency, Office of Research and Development, Washington DC 20460 . EPA/600/4-91-010.

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Lab Name: Midwest Research Institute                     Method Code: 022

Analytical Method for Mercury in Tissue by FIMS CVAAS

Summary: A 0.2-g aliquot of dry tissue is solubilized with tetramethylammonium hydroxide (TMAH) at 60*C for 1 hour, followed by digestion with nitric acid in a heating block at 95*C for 1 hour and the sample is diluted to 50 mL. The digest is subjected to on-line oxidation with potassium permanganate followed by reduction with sodium borohydride to elemental mercury and measured by cold vapor atomic absorption spectroscopy (CVAAS) using a Perkin Elmer FIMS mercury analyzer, or equivalent. The nominal detection limit is 0.05 ug/g on a dry weight basis.

References:

Method 200.11 Determination of Metals in Fish Tissue by Inductively Coupled Plasma Atomic Emission Spectrometry. Rev 2.1, April 1991. Methods for the Determination of Metals in Environmental Samples. United States Environmental Protection Agency, Office of Research and Development, Washington DC 20460 . EPA/600/4-91-010.

Determination of Total Mercury in Biological Tissues by Flow Injection Cold Vapor Generation Atomic Absorption Spectrometry Following Tetramethylammonium hydroxide digestion. Tao,G., Willie,S.N., and Sturgeon,R.*, Analyst, June 1998, Vol.123 (1215-1218) *Institute for National Measurement Standards, National Research Council of Canada , Ottawa , Ontario , Canada , K1A 0R9

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Lab Name: Midwest Research Institute                     Method Code: 023

Analytical Method for Trace Elements in Water by ICPMS

Summary: A 50-mL aliquot of water is digested with nitric acid and hydrochloric acid in a heating block at 95 C for 3 hours and the sample is diluted to 50 mL. Determination is performed by inductively coupled plasma-mass spectrometry. Typical detection limits are in the 0.05-5 ug/L range.

References:

Method 200.8 Determination of Trace Elements in Water and Wastes by Inductively Coupled Plasma-Mass Spectrometry. Rev 5.4, EMMC Version. Methods for the Determination of Metals in Environmental Samples, Supplement 1. United States Environmental Protection Agency, Office of Research and Development, Washington DC 20460 . EPA/600/R-94/111.

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Lab Name: Midwest Research Institute                     Method Code: 024

Analytical Method for Trace Elements in Tissue by ICPMS

Summary: A 1-g aliquot of dry tissue is solubilized with tetramethylammonium hydroxide (TMAH) at 60*C for 1 hour, followed by digestion with nitric acid (and optionally hydrochloric acid) in a heating block at 95*C for 1 hour and the sample is diluted to 50 mL. Determination is performed by inductively coupled plasma-mass spectrometry on ten-fold dilutions of the digested solution. Typical detection limits are in the 0.01-5 ug/g range on a dry weight basis.

References:

Method 200.11 Determination of Metals in Fish Tissue by Inductively Coupled Plasma Atomic Emission Spectrometry. Rev 2.1, April 1991. Methods for the Determination of Metals in Environmental Samples. United States Environmental Protection Agency, Office of Research and Development, Washington DC 20460 . EPA/600/4-91-010.

Method 200.8 Determination of Trace Elements in Water and Wastes by Inductively Coupled Plasma-Mass Spectrometry. Rev 5.4, EMMC Version. Methods for the Determination of Metals in Environmental Samples, Supplement 1. United States Environmental Protection Agency, Office of Research and Development, Washington DC 20460 . EPA/600/R-94/111.

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Lab Name: Midwest Research Institute                     Method Code: 025

Analytical Method for Trace Elements in Sediment by ICPMS

Summary: A 1-g aliquot of dry sediment is digested with nitric acid and hydrochloric acid in a heating block at 95*C for 30 minutes and the sample is diluted to 50 mL. Determination is performed by inductively coupled plasma-mass spectrometry on ten-fold dilutions of the digested solution. Typical detection limits are in the 0.01-5 ug/g range on a dry weight basis.

References:

Method 200.8 Determination of Trace Elements in Water and Wastes by Inductively Coupled Plasma-Mass Spectrometry. Rev 5.4, EMMC Version. Methods for the Determination of Metals in Environmental Samples, Supplement 1. United States Environmental Protection Agency, Office of Research and Development, Washington DC 20460 . EPA/600/R-94/111.

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Lab Name: Midwest Research Institute                     Method Code: 026

Microwave Digestion and the Analysis of Trace Elements in Sediment

Summary: A 0.5-g aliquot of dry sediment is digested with nitric acid (and optionally hydrochloric acid) in a microwave oven at a temperature of 170-180*C for 20 minutes and the sample is diluted to 50 mL. Determination is performed by inductively coupled plasma-mass spectrometry on ten-fold dilutions of the digested solution or by cold vapor atomic absorption spectrometry for mercury. Typical detection limits are in the 0.01-5 ug/g range on a dry weight basis.

References:

Method 3051 Microwave Assisted Acid Digestion of Sediments, Sludges, Soils and Oils. Rev. 0, 1992. Test Methods for Evaluating Solid Wastes, Physical/Chemical Methods, SW-846, 3rd Edition. U.S. Environmental Protection Agency, Office of Solid Waste and Emergency response, U.S. Government Printing Office, Washington , D.C. 20460

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Lab Name: Midwest Research Institute                     Method Code: 027

Procedure for Moisture Determination and Homogenization of Solid Samples

Summary: A suitable vessel is preweighed, an aliquot of wet sample is added and the vessel is reweighed. The sample is freeze dried and the vessel is weighed again. After subtraction of the vessel weight, wet and dry sample mass is used to determine moisture content. For homogenization, 2 Teflon balls (0.25" diameter) are added and the vessel is shaken in a paint shaker for 30 minutes. Aliquots of the dried, homogenized samples are used for digestion and analysis.

References:

Analytical Methods for Trace Elements in Fish Liver by Atomic Absorption Spectrophotometry. NOAA Technical Memorandum NOS ORCA 71. Sampling and Analytical Methods of the National Status and Trends Program National Benthic Surveillance and Mussel Watch Projects 1984-1992 Volume III. Comprehensive Descriptions of Elemental Analytical Methods. National Oceanic and Atmospheric Administration, Silver Springs , Maryland , July 1993.

GERG Trace Element Quantitation Techniques. NOAA Technical Memorandum NOS ORCA 71. Sampling and Analytical Methods of the National Status and Trends Program National Benthic Surveillance and Mussel Watch Projects 1984-1992 Volume III. Comprehensive Descriptions of Elemental Analytical Methods. National Oceanic and Atmospheric Administration, Silver Springs , Maryland , July 1993.

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