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Analytical Services, Ltd. (AXYS) Laboratory Methods Select one of the links below to display the method descriptions associated with AXYS.
Lab Name: Analytical Services, Ltd. Method Code: 001 Dissection of Tissue Samples The animal is dissected frozen. Muscle tissue is carefully removed from the bones and skin of the animal with a clean, solvent-rinsed scalpel. Organs are excised from the animal using a solvent rinsed scalpel. Dissected tissue and/or organ is stored frozen. Lab Name: Analytical Services, Ltd. Method Code: 002 Homogenization of Tissue Samples Tissue samples are thawed then homogenized using clean, solvent rinsed homogenization apparatus suitable to the size of the sample. Small quantities of sample, including organs and bivalves, are homogenized with a Virtis blender. Muscle tissue is homogenized with an Oster blender. Whole samples are ground by passing the sample three times through a commercial meat grinder. Homogenized samples are stored frozen. Lab Name: Analytical Services, Ltd. Method Code: 003 Homogenization of Vegetation Vegetation samples are homogenized frozen. Grass, leaves, and stalks are cut into small pieces with solvent rinsed scissors and homogenized with a clean Waring Blender. Large quantities of vegetation are homogenized using a solvent rinsed meat grinder. Homogenized samples are stored frozen. Lab Name: Analytical Services, Ltd. Method Code: 004 Decantation of Water from Sediments Samples are thawed. Free standing water is carefully decanted without disturbing the sediment. If fine particles are decanted with the free water, they are separated by centrifugation and added back to the sample. Decanted water is discarded. Lab Name: Analytical Services, Ltd. Method Code: 005 Homogenization of Soil and Sediment Samples Soil and sediment samples are thawed. The sample is transferred to a clean solvent rinsed stainless steel bowl and manually broken up. Rocks larger than 0.5 cm are removed and discarded. If dry, the sample is passed through a 0.4 cm sieve to remove rocks. The sample is stirred with a clean spatula until homogeneous. The homogenized sample is stored frozen. Lab Name: Analytical Services, Ltd. Method Code: 006 Homogenization by Stirring Samples which are received as homogenates are homogenized by stirring with a clean, solvent rinsed spatula just prior to subsampling. Lab Name: Analytical Services, Ltd. Method Code: 007 Subsampling of Aqueous Samples Aqueous samples which need to be subsampled for analysis are homogenized by shaking vigorously and immediately poured into a graduated cylinder. Lab Name: Analytical Services, Ltd. Method Code: 008 Homogenization of Blood Samples Blood samples are thawed and mixed thoroughly by shaking prior to subsampling. Lab Name: Analytical Services, Ltd. Method Code: 011 Soxhlet Extraction of Tissue, Sediment and Soil Samples Animal and plant tissue, soil and sediment samples are extracted by grinding the sample with anhydrous sodium sulphate, spiking with surrogate standards, and refluxing in a soxhlet apparatus for 16 to 20 hours. The cooled extract is concentrated by rotary evaporation. Lab Name: Analytical Services, Ltd. Method Code: 012 Solvent Extraction of Water Samples Aqueous samples are spiked with surrogate standards and extracted by shaking three times with dichloromethane. The extract is dried over anhydrous sodium sulphate and concentrated in a Kuderna-Danish concentrator. Lab Name: Analytical Services, Ltd. Method Code: 013 Solvent Extraction of Blood Samples Blood samples, to which surrogate standards have been added are extracted by shaking with an ethanol/ammonium sulphate/hexane mixture, followed by shaking with hexane. The combined hexane extracts are washed with water and dried over anhydrous sodium sulphate. The extract is filtered and the solvent removed by rotary evaporation. Lab Name: Analytical Services, Ltd. Method Code: 014 Soxhlet Extraction of XAD Columns XAD resin, from XAD water sampling columns, is dried by filtration through a Millipore filtration apparatus. The resin is placed in a soxhlet thimble and spiked with surrogate standards. The sample is soxhlet extracted with dichloromethane. The extract is concentrated by rotary evaporation. Lab Name: Analytical Services, Ltd. Method Code: 015 Soxhlet Extraction of Particulate Filters Particulate filters from XAD water sampling columns are air-dried. The filters are placed in a soxhlet thimble and spiked with surrogate standards. The sample is soxhlet extracted with dichloromethane. The extract is concentrated by rotary evporation. Lab Name: Analytical Services, Ltd. Method Code: 021 Gel Permeation Column Chromatography Concentrated extracts are loaded onto a calibrated gel permeation column (Biobeads SX-3) to remove high molecular weight interferences. The column is eluted with 1:1 dichloromethane and the second fraction collected. This fraction is concentrated by rotary evaporation, prior to additional chromatographic cleanup procedures. Lab Name: Analytical Services, Ltd. Method Code: 022 Chromatographic Cleanup of PCBs, Pesticides and Toxaphene on Florisil The extract is loaded onto a Florisil column (2.1% deactivated) which is eluted with hexane followed by 15:85 dichloromethane:hexane. The eluates are collected together (F1). This fraction contains chlorinated pesticides, toxaphene, and PCB congeners. The fraction is concentrated, an aliquot of recovery standard added and the extract transferred to an autosampler vial in preparation for instrumental analysis. However, for the analysis of non-ortho-substituted congeners, the fraction is first split, and one half is subject to additional cleanup on carbon/Celite to isolate the non-ortho-substituted PCBs. The Florisil column is then eluted with 1:1 dichloromethane:hexane and the eluate collected (F2). This fraction contains polar chlorinated pesticides. The fraction is concentrated, an aliquot of recovery standard added and the extract transferred to an autosampler vial in preparation for instrumental analysis. Lab Name: Analytical Services, Ltd. Method Code: 023 Chromatographic Cleanup of Non-ortho-substituted PCBs on Carbon/Celite and Alumina The first fraction from the Florisil cleanup procedure is eluted through a 4.75% carbon on Celite chromatography column. The column is eluted with 1:1 cyclohexane:dichloromethane (discard) followed by ethylacetate (discard). The non-ortho-substituted PCB congeners are eluted with 1:1 toluene:ethylacetate. The concentrated extract is loaded onto an alumina column (1% deactivated) which is eluted with hexane (discard) followed by 1:1 dichloromethane:hexane (retain). The eluate is concentrated and an aliquot of recovery standard added in preparation for instrumental analysis. Lab Name: Analytical Services, Ltd. Method Code: 024 Chromatographic Cleanup of PCB Congeners on Florisil The extract is loaded onto a Florisil column (2.1% deactivated) which is eluted with hexane followed by 15:85 dichloromethane:hexane. The eluates are collected together (F1). This fraction contains PCB congeners. The fraction is concentrated, an aliquot of recovery standard added and the extract transferred to an autosampler vial in preparation for instrumental analysis. Lab Name: Analytical Services, Ltd. Method Code: 025 Chromatographic Separation and Cleanup of Dioxins, Furans, Non-ortho-substituted PCBs, Ortho-substituted PCBs, Pesticides and Toxaphene on Carbon/Celite The extract is loaded onto a pre-eluted 4.5% carbon on Celite chromatography column which is eluted with 1:1 cyclohexane:dichloromethane followed by 10:1 ethylacetate:toluene. The eluates are collected together and concentrated (Fraction E1). This fraction contains ortho-substituted PCBs, pesticides and toxaphene and requires additional cleanup on Florisil. The column is inverted, eluted with toluene and the eluate collected (Fraction E2). This fraction contains dioxins, furans and non-ortho-substituted PCBs and requires further cleanup on alumina. Lab Name: Analytical Services, Ltd. Method Code: 026 Chromatographic Cleanup of Dioxins, Furans and Non-ortho-substituted PCBs on Alumina The concentrated extract is loaded onto an alumina column (1% deactivated) which is eluted with hexane. This fraction is added to the F1/F2 fraction from a Florisil column, if pesticides are part of the analysis. Otherwise, this fraction is discarded. The column is then eluted with 1:1 dichloromethane:hexane (retain). The eluate is concentrated and an aliquot of recovery standard added in preparation for instrumental analysis. Lab Name: Analytical Services, Ltd. Method Code: 027 Chromatographic Cleanup on Layered Silica The concentrated extract is loaded onto a layered silica column (layers: neutral, basis, neutral, acidic, acidic). The column is eluted with hexane. The eluate is collected and concentrated in preparation for additional chromatographic cleanup procedures. Lab Name: Analytical Services, Ltd. Method Code: 028 Chromatographic Cleanup on PCB Congeners on Florisil, Alumina and Layered Silica The extract is loaded onto a Florisil column (2.1% deactivated) which is eluted with hexane followed by 15:85 dichloromethane:hexane. The eluates are collected together (F1). The concentrated fraction is loaded onto an alumina column (1% deactivated) which is eluted with hexane (discard) followed by 1:1 dichloromethane:hexane (retain). The concentrated fraction is loaded onto a layered silica column (layers: neutral, basic, neutral, acidic, acidic). The column is eluted with hexane. The eluate is concentrated and an aliquot of recovery standard added in preparation for instrumental analysis. Lab Name: Analytical Services, Ltd. Method Code: 029 Chromatographic Cleanup of PAHs on Layered Silica The concentrated extract is loaded onto a layered silican column (layers: neutral, basic, neutral, acidic, acidic). The column is eluted with pentane, and the eluate discarded. The column is eluted with dichloromethane. The eluate is collected and concentrated in preparation for additional chromatographic cleanup procedures. Lab Name: Analytical Services, Ltd. Method Code: 030 Chromatographic Cleanup of PCDD/F on Florisil and Alumina Columns The extract is loaded onto a Florisil column (2.1% deactivated) which is eluted with hexane followed by 15:85 dichloromethane:hexane. The eluates are collected together (F1). The concentrated fraction is loaded onto an alumina column (1% deactivated) which is eluted with hexane (discard) followed by 1:1 dichloromethane:hexane (retain). The column is eluted with hexane. The eluate is concentrated and an aliquot of recovery standard added in preparation for instrumental analysis. Lab Name: Analytical Services, Ltd. Method Code: 031 HRGC/MS Analysis of PCB Congeners High resolution analysis of PCB congeners is carried out using a either a VG 70SE or VG Ultima mass spectrometer. Each instrument is equipped with a Hewlett Packard 5890 GC, a CTC autosampler and a VAX 3100 data system. Data are acquired in the Selected Ion Monitoring mode to enhance sensitivity. The MS is operated at mass resolution 10000. Chromatographic separation is achieved with a DB-5 capillary column (60 m, 0.25 mm i.d., 0.1 æm film thickness). A splitless/split injection sequence is used. A calibration solution is run every 12 hours and response factors of PCB congeners are determined. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 032 HRGC/MS Analysis of Non-ortho-substituted PCB Congeners High resolution analysis of non-ortho-substituted PCBs is carried out using a VG 70SE mass spectrometer equipped with a Hewlett Packard 5890 GC, a CTC autosampler and a VAX 3100 data system. Data are acquired in the Selected Ion Monitoring mode to enhance sensitivity. The MS is operated at mass resolution 10000. Chromatographic separation is achieved with a DB-5 capillary column (60 m, 0.25 mm i.d., 0.25 æm film thickness). A splitless/split injection sequence is used. A calibration solution is run every 12 hours and response factors of PCBs are determined. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 033 HRGC/MS Analysis of Chlorinated Pesticides High resolution analysis of pesticides is carried out using a VG 70SE mass spectrometer equipped with a Hewlett Packard 5890 GC, a CTC autosampler and a VAX 3100 data system. Data are acquired in the Selected Ion Monitoring mode to enhance sensitivity. The MS is operated at mass resolution 10000. Chromatographic separation is achieved with a DB-5 capillary column (60 m, 0.25 mm i.d., 0.25 æm film thickness). A splitless/split injection sequence is used. A calibration solution is run every 12 hours and response factors of pesticides are determined. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 034 LRGC/MS Analysis of Chlorinated Pesticides, PCBs (Aroclors), Toxaphene, and PCB Congeners Analysis of pesticides, PCBs (Aroclors), Total PCBs, toxaphene and individual PCB congeners is carried out using a Finnigan INCOS 50 mass spectrometer equipped with a Varian 3400 GC, a CTC A200S autosampler and a DG10 data system running Incos 50 (Rev 11) software. The MS is operated at unit mass resolution in the Multiple Ion detection mode. Chromatographic separation is achieved with a DB-5 capillary column (60 m, 0.25 mm i.d., 0.10 æm film thickness). A splitless/split injection sequence is used. A calibration solution is run every 12 hours and response factors are determined. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 035 GC/MS/ECNI Analysis of Toxaphene Toxaphene is analyzed using a Finnigan INCOS 50 mass spectrometer equipped with a Varian 3400 GC, a CTC A200S autosampler and a DG10 data system running Incos 50 (Rev 11) software. The MS is operated in the electron capture negative ionization mode. Chromatographic separation is achieved with a DB-5 capillary column (60 m, 0.25 mm i.d., 0.10 æm film thickness). A splitless/split injection sequence is used. A calibration solution is run every 12 hours and response factors are determined. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 036 GC/ECD Analysis of Polar Chlorinated Pesticides The most polar chlorinated pesticides are analyzed using a Hewlett Packard 5890A gas chromatograph equipped with a 63Ni electron capture detector. Chromatographic separation is achieved using a DB-5 capillary column (60 m, 0.25 mm i.d., 0.10 æm film thickness). A splitless/split injection sequence is used. A calibration solution is run every 12 hours and response factors of pesticides are determined. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 037 HRGC/MS Analysis of Dioxins, Furans and Non-ortho-substituted PCBs High resolution analysis of polychlorinated dioxins and furans and non-ortho-substituted PCBs is carried out using a VG Ultima mass spectrometer equipped with a Hewlett Packard 5890 GC, a CTC autosampler and a VAX 3100 data system. Data are acquired in the Selected Ion Monitoring mode to enhance sensitivity. The MS is operated at mass resolution 10000. Chromatographic separation is achieved with a DB-5 capillary column (60 m, 0.25 mm i.d., 0.1 æm film thickness). A splitless/split injection sequence is used. A calibration solution is run every 12 hours and response factors of authentic dioxins, furans and non-ortho-substituted PCBs are determined. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 038 HRGC/MS/ECNI Analysis of Toxaphene Toxaphene is analyzed using a VG Autospec mass spectrometer equipped with a Hewlett Packard 6890 GC, a A200S CTC autosampler and an Alpha data station. Data are acquired in the Selected Ion Monitoring mode to enhance sensitivity. The MS is operated at mass resolution 10000 and in the electron capture negative ionization mode. Chromatographic separation is achieved with a BC-5 capillary column (60 m, 0.25 mm i.d., 0.10 (m film thickness). A splitless/split injection sequence is used. A calibration solution is run every 12 hours and response factors are determined. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 039 HRGC/MS analysis of PCB Congeners (EPA Method 1668) High resolution analysis of PCB congeners is carried out using a VG 70SE mass spectrometer equipped with a Hewlett Packard 5890 GC, a CTC autosampler and an Alpha workstation. Data are acquired in the Selected Ion Monitoring mode to enhance sensitivity. The MS is operated at mass resolution 10000. Chromatographic separation is achieved with a SPB-Octyl capillary column (30 m, 0.25 mm i.d., 0.25 um film thickness). A splitless/split injection sequence is used. Initial calibration is established using a series of calibration solutions encompassing the working concentration range. Calibration is verified every 12 hours by analysis of a mid-range calibration solution. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 040 LRGC/MS Analysis of PAHs Analysis of PAHs is carried out using a Finnigan INCOS 50 mass spectrometer equipped with a Varian 3400 GC, a CTC A200S autosampler and a Pentium workstation running manufacturer software. The MS is operated at unit mass resolution in the Multiple Ion detection mode. Chromatographic separation is achieved on a Restek Rtx-5 chromatography column (30 m, 0.25 mm i.d., 0.25m film thickness), coupled directly to the MS source. A splitless/split injection sequence is used. A calibration solution is run every 12 hours and response factors are determined. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 041 HRGC/HRMS Analysis of Polybrominated Diphenylethers (PBDE) Polybrominated diphenylethers are analyzed by high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS) using a Micromass Ultima or VG70 mass spectrometer (MS) equipped with a Hewlett Packard 5890 or 6890 gas chromatograph, running Micromass software. A DB-5HT capillary chromatography column (30 m, 0.25 mm i.d. x 0.1 um film thickness) is coupled to the MS source. The mass spectrometer is tuned to have a static mass resolution of 5,000. Data are acquired in the Selected Ion Monitoring mode to enhance sensitivity. Initial calibration is established using a series of calibration solutions encompassing the working concentration range. Calibration is verified every 12 hours by analysis of a mid-range calibration solution. Analytes are quantified using the internal standard method of quantification, comparing the area of analyte peak to that of the corresponding surrogate standard and correcting for response factors. Lab Name: Analytical Services, Ltd. Method Code: 051 Determination of Percent Moisture A weighed subsample is dried for at least 16 hours at 105øC and then reweighed. Percent moisture is calculated as the percent difference between the dry weight and the wet weight. Lab Name: Analytical Services, Ltd. Method Code: 052 Determination of Percent Lipid Percent lipid determination is carried out on extracts by drying two weighed subsamples of extract at 105øC for 30 minutes. The extracts are re-weighed. The percent lipid is calculated as the percent lipid of wet sample weight. Lab Name: Analytical Services, Ltd. Method Code: 053 Determination of Grain Size To determine particle size distribution, samples are pre-treated to remove organic matter, carbonates, soluble salts, and iron oxides. The percent gravel, sand, silt and clay is determined by a combination of dry sieving, wet sieving and pipetting techniques. Reference: "Methods of Soil Analysis, Part 1 - Physical and Mineralogical Methods" (Gee and Bauder, 1986) Method 15-4. Lab Name: Analytical Services, Ltd. Method Code: 054 Determination of Total Organic Carbon Total organic carbon is determined by high temperature oxidation of carbon to carbon dioxide which is then measured by means of a nondispersive infrared analyzer. Total organic carbon is calculated as the percent difference between total and inorganic carbon. Reference: USEPA Method 9060A Lab Name: Analytical Services, Ltd. Method Code: 055 Determination of Percent Lipid The concentration of triglycerides, cholestrol and phospholipids are determined enzymatically using Technicon RA-500 Analyser. |
