Macro and Micro Analytical Methods Development Completed
The Macro and Micro Analytical Methods Development Project (MMAMD) provides access to the expertise of highly experienced research scientists and state of the art analytical instrumentation to develop new and unique analytical capabilities to solve complex problems beyond routine analysis.
Science Issue and Relevance
Many projects funded by the Minerals Resources Program and other USGS mission areas use chemical analysis as a tool to study a variety of mineralogical, ecological, environmental, and biological processes. Routinely, the success of these projects is reliant upon access to state-of-the-art instrumentation and methods of analysis. The Macro and Micro Analytical Methods Development Project provides access to the expertise of highly experienced research scientists and state of the art analytical instrumentation to develop new and unique analytical capabilities to solve complex problems beyond routine analysis. Generally macro analytical methods examine the bulk elemental, chemical, or mineralogical composition of a sample while micro analytical methods use specialized sample introduction devices or instrumentation to examine how the elements or minerals are spatially distributed in a sample. Both macro and micro analytical methods use a variety of analytical instrumentation including: Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES), X-ray Fluorescence (XRF), X-ray Diffraction (XRD), Raman Spectroscopy, and Cavity Ring-Down Spectroscopy (CRDS). Development of new, state-of-the-art analytical methods can be applied to topical studies in energy and minerals, environmental health, ecosystems, land resources use, water quality, and natural hazards. For many projects carried out by the USGS, there are no commercial laboratories that can provide the unique types of geochemical analyses or the high quality data required to carry out the project objectives.
Methodology to Address Issue
Our scientists ascertain what types of new and emerging analytical techniques USGS will need with the next several years to support programmatic research efforts and to develop those techniques using existing instrumentation or by obtaining the necessary equipment and instrumentation. Another key goal of the project is to evaluate the need for and develop new natural matrix geochemical standard reference materials that are used by USGS and other scientists to calibrate analytical instrumentation, validate methods and models, and monitor laboratory performance. Project members also develop methods for specialized analyses via reimbursable projects for other DOI and U.S. government agencies. The Project is responsible for maintaining the availability of analytical instrumentation, laboratories, techniques and staffing for use by multiple USGS projects and for maintaining specialized in-house capabilities for use in characterization of difficult to analyze sample matrices beyond the capabilities of the contract laboratory.
New Macro Analytical Methods Development - This task provides for the coordinated research and development of new analytical methods needed to meet the needs of projects administered under the Mineral Resources Program and other USGS projects as needs arise. Project staff work on analytical techniques including inductively coupled plasma-atomic emission spectrometry (ICP-AES), inductively coupled plasma-mass spectrometry (ICP-MS), ion chromatography, liquid chromatography, hydride generation atomic absorption, and specific element instrumentation such as mercury, carbon, and sulfur analyzers. Other areas of investigation include development of new or improved sample preparation methodologies such as specialized hot plate or microwave-assisted digestions and extractions to improve efficiency and data quality.
One of the primary goals of this task is to develop and validate analytical protocols for difficult-to-analyze samples that are beyond the capabilities of routine commercial laboratories. Development of new analytical protocols is performed in anticipation of future analytical needs of USGS projects, so that state-of-the-art analytical methods will be available to project staff as they are needed. Current areas of focus include:
- Development and validation of new analytical methodologies including High Resolution Dynamic Reaction Cell (DRC) and/or Kinetic Energy Discrimination (KED) Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) for analysis of typical geological samples to improve detection limits and accuracy eliminating common interferences on elements,
- Development and validation of direct analysis of powdered samples for trace elements using Energy Dispersive X-ray Fluorescence (EDXRF),
- Development and validation of new analytical methods for interference-free analysis of rare earth elements in waters, soils, and sediments using alternative sample introduction devices, dynamic reaction cell ICP-MS, and/or high resolution (HR) ICP-MS,
- Continued development of speciation methods using the high performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP-MS) system for determination of different forms of arsenic, selenium, and chromium species in aqueous species,
- Continued investigation and validation of new methods for the preservation and extraction of inorganic species of arsenic, selenium, and chromium from a wide variety of sample types, including fire ashes, soils, sediments, and air filters, including improved or modified hexavalent chromium extraction methods,
- Investigation and development of isotope dilution methodologies for the accurate determination of elements in geochemical reference materials,
- Continued development and validation of new and improved analytical methods using dual-view ICP-AES to improve detection limits and elimination of interferences using Multicomponent Spectral Fitting (MSF) techniques,
- Further develop novel in-situ microanalytical techniques for determining trace concentrations in heavy metals in surface water environments in virtual real-time mode using field deployable instrumentation that operates in unattended mode.
Geological Reference Materials - This task develops and produces geochemical reference materials in support of USGS mineral exploration and development activities. Geological reference materials are crucial for USGS projects and laboratories to ensure the highest possible accuracy of their chemical analyses.
Geologic reference materials are developed using matrix matched geologic sample types currently under investigation. Well characterized reference materials are a key component in evaluating laboratory accuracy and precision, as these materials are routinely used in laboratory quality assurance programs. We provide reference materials for methods development on new sample types or methods of analysis, which in turn allow the transition from qualitative to quantitative analysis. We foster development of new preparation techniques to meet specific project needs and collaborate with government, private, and international partners to develop new reference materials that benefit USGS activities.
The major areas of investigation are listed below.
- Replacement of existing USGS powdered reference materials which serve as the backbone to many quality control programs.
- Development of new reference materials for microanalysis, particularly focusing on the development of a) glass materials from different alumino silicate rock types and b) pressed powders from significant geologic matrix types (phosphates, gypsum, barite, sulfides, carbonates).
- Development of new reference materials from sample types important in rare earth element source materials (carbonatite, alkaline dike).
- Develop plans for the preparation of several shale gas reference materials in collaboration with industry.
- Begin developing a series of new geologic reference materials designed to assist in the mineralogical analysis of geologic materials by X-ray diffraction (XRD).
- Prepare customized geologic reference materials for private and government customers (ex. mine waste, ore material, baseline sediments, soils, lunar simulant).
Laser Ablation ICP-MS Trace Element Microanalysis - The laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) task involves the continuing advance of in-situ methods for trace element analyses for Mineral Resource Program goals. Direct, in-situ analyses provide a detailed look at the chemical story preserved in minerals, rocks, biological and environmental samples. Our work provides broad support across numerous USGS projects and to outside collaborators. Focus areas include the direct assessment of the residence and mode of occurrence of critical metals in a variety of deposit types and waste products, utilization of trace element signatures and zoning within minerals to better decipher mineral deposit origins, and detailed examination of the role of microchemistry and complex residence of metals on the geometallurgy and processing of geologic materials for economic recoveries.
Our objectives are to maintain the laboratory as a leading analytical facility providing analyses for core USGS projects, be responsive (and proactive) to the changing needs of projects and scientists in areas where microanalyses can help solve problems, and to integrate and understand the complimentary nature of both traditional bulk chemical methods as well as the important necessary microanalytical tools. We utilize the known and newly developing potential of trace element microanalysis for the determination of trace elements in minerals and other solid media useful to attain programmatic goals. We work closely with the Geological Reference Materials task and the other microanalytical techniques in this project.
Multi-Collector ICP-MS - The objectives for the multi-collector inductively coupled plasma-mass spectrometer (MC-ICP-MS) lab are to continue the development of new methodologies for analysis and application of isotope systems in both solution and solid (laser) form for the applications in mineral and environmental research in support of Mineral Resources Program and USGS goals. The primary objective is to better understand the potential insight that non-traditional and traditional stable isotopes can provide for the Program's environmental, economic and geological studies. The infancy of multi-collectors still warrants the need for thorough method development with a focus on chromatographic separation for solution sample introduction and in situ laser ablation introduction. These new methods will have immediate application in the Mineral Resources Program and the multi-collector field. The lab will continue to establish new ties within the USGS and with other State, Federal agencies and Universities. Current research endeavors are below.
- In situ S isotope ratios by laser ablation MC-ICP-MS for geological applications
- Sr in situ laser ablation of fish otoliths and whole otolith by solution
- Development of in situ Pb isotope glass reference material
- Source correlation using multiple isotope systems
- Hg isotope systematics in mineral deposits and ecosystems
Method for Assessing the Microbial Geochemistry of Mineral Deposits and Their Impact on Surrounding Environments - The transport and fate of metals are inextricably linked to the carbon cycle. Natural organic compounds chelate metals which is key to the sequestration and transport of metals in aquatic environments. Many types of microorganisms in soil, sediment, and water environments link the oxidation of organic carbon and the reduction of metals. Others mediate the oxidation or methylation of metals. Many of the processes that release metals into the environment from mineralized deposits or mine waste are exclusively mediated or are accelerated by microbial activity. In addition, microbial activity can mitigate (e.g. Cr[VI] reduction) or exacerbate (e.g. mercury methylation) trace metal pollution. Microorganisms also respond to toxic concentrations of trace metals and changes in microbial community structure can be an indicator of impacts to ecosystem health. Organic biomarker molecules isolated from environmental matrices can indicate the types and abundances of microorganisms present. Some indicator molecules provide measures of viable microorganisms while others can integrate long-term occurrence of microbial processes.
We maintain and develop expertise in microbial biogeochemistry and associated analytical methods and instrumentation to support research on processes that distribute and sequester trace metals from mined and unmined mineralized deposits. The methods will be applied to geochemical exploration research and on environmental impacts of mining. We will develop methods that utilize gas chromatography-mass spectrometry to measure microbial abundance and characterize microbial communities.
Raman Spectroscopy for Metal Speciation in Minerals - Currently the best available method for the direct quantification of chromium(VI) in environmental solids (e.g. soils, rocks, mine wastes, manufacturing residues, and materials in the built environment) is synchrotron-based X-ray absorption near edge spectroscopy (XANES), a technique with very limited availability and no potential for application on a routine basis. Several laboratory-based techniques now exist that show promise for routine quantification of chromium(VI) in solids at trace levels: Raman spectroscopy, wavelength-dispersive X-ray fluorescence (WD-XRF), and laboratory-based XANES. The individual capabilities of each of these techniques for chromium(VI) quantification and chromium speciation in solids will be assessed in this task by analyzing selected representatives of an extensive set of samples prepared under a previous project. Raman spectroscopy is a spectroscopic technique used to observe vibrational, rotational, and other low-frequency modes in a system and is commonly used in chemistry to provide a fingerprint by which molecules can be identified. Raman spectroscopy could provide an alternative method to X-ray absorption near edge structure XANES for the determination of oxidation state of elements (e.g. arsenic and chromium) directly in the solid. This would allow studies to be performed more easily with lab-based instrumentation.
Our objectives are:
- Use microbeam techniques to identify chromium-bearing phases in soils contaminated with chromite-ore processing residue, in naturally-weathered serpentinite soils, and in primary serpentinite / peridotite rock.
- Test the feasibility of above-mentioned laboratory-based techniques to quantify chromium(VI) species in solid phases and microvolumes of solution.
Research Mineralogy - We provide research, development, and application of mineralogical analysis and support of topical projects within the USGS. The task includes x-ray mineralogy, thermogravimetric analysis coupled with quadrupole mass spectrometry, qualitative and semi-quantitative x-ray fluorescence spectroscopy and related analytical techniques for mineralogical studies in support of Mineral Resources Program and Energy Resources Program projects. The powder x-ray diffraction laboratory in Reston, VA provides qualitative and quantitative powder x-ray diffraction (XRD) and energy-dispersive x-ray fluorescence (EDXRF). Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media.
Task goals are to 1) ensure availability of state-of-the-art mineralogical analyses for scientists funded by the Mineral and Energy Resources Programs, 2) develop new methods and new applications of existing methods, and 3) minimize duplication of skills and equipment by sharing laboratory facilities with both Mineral and Energy Resources Programs.
Return to Mineral Resources Program | Geology, Geophysics, and Geochemistry Science Center
Below are other science projects associated with this project.
Below are data or web applications associated with this project.
Below are publications associated with this project.
Multi-elemental analysis of aqueous geological samples by inductively coupled plasma-optical emission spectrometry
Investigation of off-site airborne transport of lead from a superfund removal action site using lead isotope ratios and concentrations
Deep-sea coral record of human impact on watershed quality in the Mississippi River Basin
The Devonian Marcellus Shale and Millboro Shale
Mercury isotope fractionation during ore retorting in the Almadén mining district, Spain
Effects of surface applications of biosolids on groundwater quality and trace-element concentrations in crops near Deer Trail, Colorado, 2004-2010
Linking geology and health sciences to assess childhood lead poisoning from artisanal gold mining in Nigeria
Uranium quantification in semen by inductively coupled plasma mass spectrometry
Aquatic assessment of the Pike Hill Copper Mine Superfund site, Corinth, Vermont
Identification of contamination in a lake sediment core using Hg and Pb isotopic compositions, Lake Ballinger, Washington, USA
Mineralogy and environmental geochemistry of historical iron slag, Hopewell Furnace National Historic Site, Pennsylvania, USA
Arsenic-induced biochemical and genotoxic effects and distribution in tissues of Sprague-Dawley rats
Below are partners associated with this project.
- Overview
The Macro and Micro Analytical Methods Development Project (MMAMD) provides access to the expertise of highly experienced research scientists and state of the art analytical instrumentation to develop new and unique analytical capabilities to solve complex problems beyond routine analysis.
Science Issue and Relevance
Many projects funded by the Minerals Resources Program and other USGS mission areas use chemical analysis as a tool to study a variety of mineralogical, ecological, environmental, and biological processes. Routinely, the success of these projects is reliant upon access to state-of-the-art instrumentation and methods of analysis. The Macro and Micro Analytical Methods Development Project provides access to the expertise of highly experienced research scientists and state of the art analytical instrumentation to develop new and unique analytical capabilities to solve complex problems beyond routine analysis. Generally macro analytical methods examine the bulk elemental, chemical, or mineralogical composition of a sample while micro analytical methods use specialized sample introduction devices or instrumentation to examine how the elements or minerals are spatially distributed in a sample. Both macro and micro analytical methods use a variety of analytical instrumentation including: Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES), X-ray Fluorescence (XRF), X-ray Diffraction (XRD), Raman Spectroscopy, and Cavity Ring-Down Spectroscopy (CRDS). Development of new, state-of-the-art analytical methods can be applied to topical studies in energy and minerals, environmental health, ecosystems, land resources use, water quality, and natural hazards. For many projects carried out by the USGS, there are no commercial laboratories that can provide the unique types of geochemical analyses or the high quality data required to carry out the project objectives.
Methodology to Address Issue
Our scientists ascertain what types of new and emerging analytical techniques USGS will need with the next several years to support programmatic research efforts and to develop those techniques using existing instrumentation or by obtaining the necessary equipment and instrumentation. Another key goal of the project is to evaluate the need for and develop new natural matrix geochemical standard reference materials that are used by USGS and other scientists to calibrate analytical instrumentation, validate methods and models, and monitor laboratory performance. Project members also develop methods for specialized analyses via reimbursable projects for other DOI and U.S. government agencies. The Project is responsible for maintaining the availability of analytical instrumentation, laboratories, techniques and staffing for use by multiple USGS projects and for maintaining specialized in-house capabilities for use in characterization of difficult to analyze sample matrices beyond the capabilities of the contract laboratory.
New Macro Analytical Methods Development - This task provides for the coordinated research and development of new analytical methods needed to meet the needs of projects administered under the Mineral Resources Program and other USGS projects as needs arise. Project staff work on analytical techniques including inductively coupled plasma-atomic emission spectrometry (ICP-AES), inductively coupled plasma-mass spectrometry (ICP-MS), ion chromatography, liquid chromatography, hydride generation atomic absorption, and specific element instrumentation such as mercury, carbon, and sulfur analyzers. Other areas of investigation include development of new or improved sample preparation methodologies such as specialized hot plate or microwave-assisted digestions and extractions to improve efficiency and data quality.
One of the primary goals of this task is to develop and validate analytical protocols for difficult-to-analyze samples that are beyond the capabilities of routine commercial laboratories. Development of new analytical protocols is performed in anticipation of future analytical needs of USGS projects, so that state-of-the-art analytical methods will be available to project staff as they are needed. Current areas of focus include:
- Development and validation of new analytical methodologies including High Resolution Dynamic Reaction Cell (DRC) and/or Kinetic Energy Discrimination (KED) Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) for analysis of typical geological samples to improve detection limits and accuracy eliminating common interferences on elements,
- Development and validation of direct analysis of powdered samples for trace elements using Energy Dispersive X-ray Fluorescence (EDXRF),
- Development and validation of new analytical methods for interference-free analysis of rare earth elements in waters, soils, and sediments using alternative sample introduction devices, dynamic reaction cell ICP-MS, and/or high resolution (HR) ICP-MS,
- Continued development of speciation methods using the high performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP-MS) system for determination of different forms of arsenic, selenium, and chromium species in aqueous species,
- Continued investigation and validation of new methods for the preservation and extraction of inorganic species of arsenic, selenium, and chromium from a wide variety of sample types, including fire ashes, soils, sediments, and air filters, including improved or modified hexavalent chromium extraction methods,
- Investigation and development of isotope dilution methodologies for the accurate determination of elements in geochemical reference materials,
- Continued development and validation of new and improved analytical methods using dual-view ICP-AES to improve detection limits and elimination of interferences using Multicomponent Spectral Fitting (MSF) techniques,
- Further develop novel in-situ microanalytical techniques for determining trace concentrations in heavy metals in surface water environments in virtual real-time mode using field deployable instrumentation that operates in unattended mode.
Geological Reference Materials - This task develops and produces geochemical reference materials in support of USGS mineral exploration and development activities. Geological reference materials are crucial for USGS projects and laboratories to ensure the highest possible accuracy of their chemical analyses.
Geologic reference materials are developed using matrix matched geologic sample types currently under investigation. Well characterized reference materials are a key component in evaluating laboratory accuracy and precision, as these materials are routinely used in laboratory quality assurance programs. We provide reference materials for methods development on new sample types or methods of analysis, which in turn allow the transition from qualitative to quantitative analysis. We foster development of new preparation techniques to meet specific project needs and collaborate with government, private, and international partners to develop new reference materials that benefit USGS activities.
The major areas of investigation are listed below.
- Replacement of existing USGS powdered reference materials which serve as the backbone to many quality control programs.
- Development of new reference materials for microanalysis, particularly focusing on the development of a) glass materials from different alumino silicate rock types and b) pressed powders from significant geologic matrix types (phosphates, gypsum, barite, sulfides, carbonates).
- Development of new reference materials from sample types important in rare earth element source materials (carbonatite, alkaline dike).
- Develop plans for the preparation of several shale gas reference materials in collaboration with industry.
- Begin developing a series of new geologic reference materials designed to assist in the mineralogical analysis of geologic materials by X-ray diffraction (XRD).
- Prepare customized geologic reference materials for private and government customers (ex. mine waste, ore material, baseline sediments, soils, lunar simulant).
Laser Ablation ICP-MS Trace Element Microanalysis - The laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) task involves the continuing advance of in-situ methods for trace element analyses for Mineral Resource Program goals. Direct, in-situ analyses provide a detailed look at the chemical story preserved in minerals, rocks, biological and environmental samples. Our work provides broad support across numerous USGS projects and to outside collaborators. Focus areas include the direct assessment of the residence and mode of occurrence of critical metals in a variety of deposit types and waste products, utilization of trace element signatures and zoning within minerals to better decipher mineral deposit origins, and detailed examination of the role of microchemistry and complex residence of metals on the geometallurgy and processing of geologic materials for economic recoveries.
Our objectives are to maintain the laboratory as a leading analytical facility providing analyses for core USGS projects, be responsive (and proactive) to the changing needs of projects and scientists in areas where microanalyses can help solve problems, and to integrate and understand the complimentary nature of both traditional bulk chemical methods as well as the important necessary microanalytical tools. We utilize the known and newly developing potential of trace element microanalysis for the determination of trace elements in minerals and other solid media useful to attain programmatic goals. We work closely with the Geological Reference Materials task and the other microanalytical techniques in this project.
Multi-Collector ICP-MS - The objectives for the multi-collector inductively coupled plasma-mass spectrometer (MC-ICP-MS) lab are to continue the development of new methodologies for analysis and application of isotope systems in both solution and solid (laser) form for the applications in mineral and environmental research in support of Mineral Resources Program and USGS goals. The primary objective is to better understand the potential insight that non-traditional and traditional stable isotopes can provide for the Program's environmental, economic and geological studies. The infancy of multi-collectors still warrants the need for thorough method development with a focus on chromatographic separation for solution sample introduction and in situ laser ablation introduction. These new methods will have immediate application in the Mineral Resources Program and the multi-collector field. The lab will continue to establish new ties within the USGS and with other State, Federal agencies and Universities. Current research endeavors are below.
- In situ S isotope ratios by laser ablation MC-ICP-MS for geological applications
- Sr in situ laser ablation of fish otoliths and whole otolith by solution
- Development of in situ Pb isotope glass reference material
- Source correlation using multiple isotope systems
- Hg isotope systematics in mineral deposits and ecosystems
Method for Assessing the Microbial Geochemistry of Mineral Deposits and Their Impact on Surrounding Environments - The transport and fate of metals are inextricably linked to the carbon cycle. Natural organic compounds chelate metals which is key to the sequestration and transport of metals in aquatic environments. Many types of microorganisms in soil, sediment, and water environments link the oxidation of organic carbon and the reduction of metals. Others mediate the oxidation or methylation of metals. Many of the processes that release metals into the environment from mineralized deposits or mine waste are exclusively mediated or are accelerated by microbial activity. In addition, microbial activity can mitigate (e.g. Cr[VI] reduction) or exacerbate (e.g. mercury methylation) trace metal pollution. Microorganisms also respond to toxic concentrations of trace metals and changes in microbial community structure can be an indicator of impacts to ecosystem health. Organic biomarker molecules isolated from environmental matrices can indicate the types and abundances of microorganisms present. Some indicator molecules provide measures of viable microorganisms while others can integrate long-term occurrence of microbial processes.
We maintain and develop expertise in microbial biogeochemistry and associated analytical methods and instrumentation to support research on processes that distribute and sequester trace metals from mined and unmined mineralized deposits. The methods will be applied to geochemical exploration research and on environmental impacts of mining. We will develop methods that utilize gas chromatography-mass spectrometry to measure microbial abundance and characterize microbial communities.
Raman Spectroscopy for Metal Speciation in Minerals - Currently the best available method for the direct quantification of chromium(VI) in environmental solids (e.g. soils, rocks, mine wastes, manufacturing residues, and materials in the built environment) is synchrotron-based X-ray absorption near edge spectroscopy (XANES), a technique with very limited availability and no potential for application on a routine basis. Several laboratory-based techniques now exist that show promise for routine quantification of chromium(VI) in solids at trace levels: Raman spectroscopy, wavelength-dispersive X-ray fluorescence (WD-XRF), and laboratory-based XANES. The individual capabilities of each of these techniques for chromium(VI) quantification and chromium speciation in solids will be assessed in this task by analyzing selected representatives of an extensive set of samples prepared under a previous project. Raman spectroscopy is a spectroscopic technique used to observe vibrational, rotational, and other low-frequency modes in a system and is commonly used in chemistry to provide a fingerprint by which molecules can be identified. Raman spectroscopy could provide an alternative method to X-ray absorption near edge structure XANES for the determination of oxidation state of elements (e.g. arsenic and chromium) directly in the solid. This would allow studies to be performed more easily with lab-based instrumentation.
Our objectives are:
- Use microbeam techniques to identify chromium-bearing phases in soils contaminated with chromite-ore processing residue, in naturally-weathered serpentinite soils, and in primary serpentinite / peridotite rock.
- Test the feasibility of above-mentioned laboratory-based techniques to quantify chromium(VI) species in solid phases and microvolumes of solution.
Research Mineralogy - We provide research, development, and application of mineralogical analysis and support of topical projects within the USGS. The task includes x-ray mineralogy, thermogravimetric analysis coupled with quadrupole mass spectrometry, qualitative and semi-quantitative x-ray fluorescence spectroscopy and related analytical techniques for mineralogical studies in support of Mineral Resources Program and Energy Resources Program projects. The powder x-ray diffraction laboratory in Reston, VA provides qualitative and quantitative powder x-ray diffraction (XRD) and energy-dispersive x-ray fluorescence (EDXRF). Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media.
Task goals are to 1) ensure availability of state-of-the-art mineralogical analyses for scientists funded by the Mineral and Energy Resources Programs, 2) develop new methods and new applications of existing methods, and 3) minimize duplication of skills and equipment by sharing laboratory facilities with both Mineral and Energy Resources Programs.
Return to Mineral Resources Program | Geology, Geophysics, and Geochemistry Science Center
- Science
Below are other science projects associated with this project.
- Data
Below are data or web applications associated with this project.
- Publications
Below are publications associated with this project.
Filter Total Items: 74Multi-elemental analysis of aqueous geological samples by inductively coupled plasma-optical emission spectrometry
Typically, 27 major, minor, and trace elements are determined in natural waters, acid mine drainage, extraction fluids, and leachates of geological and environmental samples by inductively coupled plasma-optical emission spectrometry (ICP-OES). At the discretion of the analyst, additional elements may be determined after suitable method modifications and performance data are established. Samples aAuthorsTodor I. Todorov, Ruth E. Wolf, Monique AdamsInvestigation of off-site airborne transport of lead from a superfund removal action site using lead isotope ratios and concentrations
Lead (Pb) concentration and Pb isotopic composition of surface and subsurface soil samples were used to investigate the potential for off-site air transport of Pb from a former white Pb processing facility to neighboring residential homes in a six block area on Staten Island, NY. Surface and subsurface soil samples collected on the Jewett White Pb site were found to range from 1.122 to 1.138 for 2AuthorsMichael J. Pribil, Mark A. Maddaloni, Kimberly Staiger, Eric Wilson, Nick Magriples, Mustafa Ali, Dennis SantellaDeep-sea coral record of human impact on watershed quality in the Mississippi River Basin
One of the greatest drivers of historical nutrient and sediment transport into the Gulf of Mexico is the unprecedented scale and intensity of land use change in the Mississippi River Basin. These landscape changes are linked to enhanced fluxes of carbon and nitrogen pollution from the Mississippi River, and persistent eutrophication and hypoxia in the northern Gulf of Mexico. Increased terrestrialAuthorsNancy G. Prouty, E. Brendan Roark, Alan E. Koenig, Amanda W.J. Demopoulos, Fabian C. Batista, Benjamin D. Kocar, David Selby, Matthew D. McCarthy, Furu MienisThe Devonian Marcellus Shale and Millboro Shale
The recent development of unconventional oil and natural gas resources in the United States builds upon many decades of research, which included resource assessment and the development of well completion and extraction technology. The Eastern Gas Shales Project, funded by the U.S. Department of Energy in the 1980s, investigated the gas potential of organic-rich, Devonian black shales in the AppalaAuthorsDaniel J. Soeder, Catherine B. Enomoto, John A. ChermakMercury isotope fractionation during ore retorting in the Almadén mining district, Spain
Almadén, Spain, is the world's largest mercury (Hg) mining district, which has produced over 250,000 metric tons of Hg representing about 30% of the historical Hg produced worldwide. The objective of this study was to measure Hg isotopic compositions of cinnabar ore, mine waste calcine (retorted ore), elemental Hg (Hg0(L)), and elemental Hg gas (Hg0(g)), to evaluate potential Hg isotopic fractionaAuthorsJohn E. Gray, Michael J. Pribil, Pablo L. HiguerasEffects of surface applications of biosolids on groundwater quality and trace-element concentrations in crops near Deer Trail, Colorado, 2004-2010
The U.S. Geological Survey (USGS), in cooperation with Metro Wastewater Reclamation District (Metro District), studied biosolids composition and the effects of biosolids applications on groundwater quality and trace-element concentrations in crops of the Metro District properties near Deer Trail, Colorado, during 2004 through 2010. Priority parameters for each monitoring component included the ninAuthorsTracy J.B. Yager, James G. Crock, David B. Smith, Edward T. Furlong, Philip L. Hageman, William T. Foreman, James L. Gray, Rhiannon C. ReVelloLinking geology and health sciences to assess childhood lead poisoning from artisanal gold mining in Nigeria
Background: In 2010, Médecins Sans Frontières discovered a lead poisoning outbreak linked to artisanal gold processing in northwestern Nigeria. The outbreak has killed approximately 400 young children and affected thousands more. Objectives: Our aim was to undertake an interdisciplinary geological- and health-science assessment to clarify lead sources and exposure pathways, identify additional toAuthorsGeoffrey S. Plumlee, James T. Durant, Suzette A. Morman, Antonio Neri, Ruth E. Wolf, Carrie A. Dooyema, Philip L. Hageman, Heather Lowers, Gregory L. Fernette, Gregory P. Meeker, William Benzel, Rhonda L. Driscoll, Cyrus J. Berry, James G. Crock, Harland L. Goldstein, Monique Adams, Casey L. Bartrem, Simba Tirima, Behbod Behrooz, Ian von Lindern, Mary Jean BrownUranium quantification in semen by inductively coupled plasma mass spectrometry
In this study we report uranium analysis for human semen samples. Uranium quantification was performed by inductively coupled plasma mass spectrometry. No additives, such as chymotrypsin or bovine serum albumin, were used for semen liquefaction, as they showed significant uranium content. For method validation we spiked 2 g aliquots of pooled control semen at three different levels of uranium: lowAuthorsTodor I. Todorov, John W. Ejnik, Gustavo S. Guandalini, Hanna Xu, Dennis Hoover, Larry W. Anderson, Katherine Squibb, Melissa A. McDiarmid, Jose A. CentenoAquatic assessment of the Pike Hill Copper Mine Superfund site, Corinth, Vermont
The Pike Hill Copper Mine Superfund site in Corinth, Orange County, Vermont, includes the Eureka, Union, and Smith mines along with areas of downstream aquatic ecosystem impairment. The site was placed on the U.S. Environmental Protection Agency (USEPA) National Priorities List in 2004. The mines, which operated from about 1847 to 1919, contain underground workings, foundations from historical strAuthorsNadine M. Piatak, Denise M. Argue, Robert R. Seal, Richard G. Kiah, John M. Besser, James F. Coles, Jane M. Hammarstrom, Denise M. Levitan, Jeffrey R. Deacon, Christopher G. IngersollIdentification of contamination in a lake sediment core using Hg and Pb isotopic compositions, Lake Ballinger, Washington, USA
Concentrations and isotopic compositions of Hg and Pb were measured in a sediment core collected from Lake Ballinger, near Seattle, Washington, USA. Lake Ballinger has been affected by input of metal contaminants emitted from the Tacoma smelter, which operated from 1887 to 1986 and was located about 53 km south of the lake. Concentrations and loadings of Hg and Pb in Lake Ballinger increased by asAuthorsJohn E. Gray, Michael J. Pribil, Peter C. Van Metre, David M. Borrok, Anita ThapaliaMineralogy and environmental geochemistry of historical iron slag, Hopewell Furnace National Historic Site, Pennsylvania, USA
The Hopewell Furnace National Historic Site in southeastern Pennsylvania, which features an Fe smelter that was operational in the 18th and 19th centuries, is dominated by three slag piles. Pile 1 slag, from the Hopewell Furnace, and pile 2 slag, likely from the nearby Cornwall Furnace, were both produced in cold-blast charcoal-fired smelters. In contrast, pile 3 slag was produced in an anthraciteAuthorsNadine M. Piatak, Robert SealArsenic-induced biochemical and genotoxic effects and distribution in tissues of Sprague-Dawley rats
Arsenic (As) is a well documented human carcinogen. However, its mechanisms of toxic action and carcinogenic potential in animals have not been conclusive. In this research, we investigated the biochemical and genotoxic effects of As and studied its distribution in selected tissues of Sprague–Dawley rats. Four groups of six male rats, each weighing approximately 60 ± 2 g, were injected intraperitoAuthorsAnita K. Patlolla, Todor I. Todorov, Paul B. Tchounwou, Gijsbert van der Voet, Jose A. Centeno - Partners
Below are partners associated with this project.