Final Report: Preconcentration, Speciation and Determination of Dissolved Heavy Metals in Natural Waters, using Ion Exchange and Graphite Furnace Atomic Absorption Spectrometry

EPA Grant Number: R825511C049
Subproject: this is subproject number 049 , established and managed by the Center Director under grant R825511
(EPA does not fund or establish subprojects; EPA awards and manages the overall grant for this center).

Center: HSRC (1989) - Northeast HSRC
Center Director: Sidhu, Sukh S.
Title: Preconcentration, Speciation and Determination of Dissolved Heavy Metals in Natural Waters, using Ion Exchange and Graphite Furnace Atomic Absorption Spectrometry
Investigators: Ososkov, Victor K. , Kebbekus, Barbara B.
Institution: New Jersey Institute of Technology
EPA Project Officer: Hahn, Intaek
Project Period: January 15, 1995 through January 14, 1997
RFA: Hazardous Substance Research Centers - HSRC (1989) RFA Text |  Recipients Lists
Research Category: Hazardous Substance Research Centers , Land and Waste Management


The goal of this research is to develop rapid, simple and accurate methods for the preconcentration and determination of trace amounts of heavy metals in drinking water, groundwater, and fresh surface water. Speciation, or determination of the analytes in each of the several forms in which they can exist (sorbed on particles, in colloids, in various oxidation states) is also desired. The initial studies focus on lead and chromium, and cadmium is also being examined. These metals are generally toxic, and may be bioaccumulated. Therefore their measurement is imperative.

Summary/Accomplishments (Outputs/Outcomes):

Rationale: The metals exist in various forms in water and the particular species in which they are found often has a serious bearing on their environmental impact. The ions readily exchanged with the resins are those of the most bioavailable form, and are therefore of most interest. In addition, heavy metals are present in very low concentrations in natural waters, and a preconcentration technique is usually needed before analysis can be carried out. The ion exchange and chelating resins provide some speciation, as well separation of the analytes from the bulk of the sample and many interferences contained therein.

Approach: The metal ions in water are sorbed on appropriate ion exchange or chelating resins, and separated from the bulk water sample. The sample loaded beads are slurried in a small volume of nitric acid and the slurry or the supernatant acid, after the resin has settled, is injected into the GFAAS or ICP-MS for quantitation of the metal of interest. The sorption can be done in the field, and the water discarded. This reduces the volume of sample to be transported to the laboratory, and concentrates the analytes.

Status: Dissolved cadmium and lead in water have been studied. Metals were preconcentrated on resin or by evaporation to a much smaller volume before GFAAS analysis. It was found that in drinking water and in lake water, the Cd content was identical by either the evaporation or the sorption method. Levels of 0.02 ppb were measurable. The Cd concentration in unfiltered lake water was found to be higher, indicating that in this sample, about 75% of the Cd content was present in solid particles which did not pass through the filter. Lead, like Cd, was found to exist primarily (80%) in filterable particulate, with 30% of the dissolved lead being not sorbable on the resin. This is assumed to be complexed with dissolved organic or other soluble chelating agents.

In contrast, the chromium content of lake water was found to exist entirely as dissolved Cr(VI). No significant difference was found between the filtered and unfiltered samples, or between the total Cr and the Cr(VI) levels as done using sorption on anion exchange beads.

The methods for separation of lead, cadmium and chromium into dissolved and particulate species and further distinguishing between dissolved free ions and dissolved complexed ions are developed and tested, and further work is being carried out to extend the work to other aqueous matrices. The methods will also be applied to the analysis of sediments and their associated waters this summer, in cooperation with Dr. J. Weis at Rutgers, who is studying the effects of pollutants on the behavior of fish exposed to these sediments.

Clients/Users: Researchers investigating water contamination with heavy metals and their effects on the biosphere. Experts involved in monitoring pollution of natural waters and risk assessment.

Journal Articles on this Report : 3 Displayed | Download in RIS Format

Other subproject views: All 3 publications 3 publications in selected types All 3 journal articles
Other center views: All 131 publications 39 publications in selected types All 39 journal articles
Type Citation Sub Project Document Sources
Journal Article Chou CC, Ososkov V, ZhangL, Somasundaran P. Removal of nonvolatile hydrophobic compounds from artificially and naturally contaminated soils by column flotation. Journal of Soil Contamination 1998;7(5):559-571. R825511C049 (Final)
not available
Journal Article Ososkov VK, Chou CC, Kebbekus BB. Speciation, preconcentration and determination of lead in natural waters using chelating resin and direct GFAAS. International Journal of Environmental Analytical Chemistry 1998;69(1):1-12. R825511C049 (Final)
not available
Journal Article Zhang L, Zeng J, Somasundaran P, Ososkov V, Chou C. Removal of nonvolatile hydrophobic compounds from soil by flotation. 1. Laboratory investigation using mechanically agitated machine. Advances in Environmental Research 1997;1(2):157-165. R825511C049 (Final)
not available

Supplemental Keywords:

Speciation, Heavy Metals, Ion Exchange, Graphite Furnace, Atomic Absorption, Spectrometry., RFA, Scientific Discipline, INTERNATIONAL COOPERATION, Water, POLLUTANTS/TOXICS, Environmental Chemistry, Physics, Chemistry, Chemicals, Engineering, Chemistry, & Physics, Drinking Water, metal-chelate complexes, chelating exchanger, graphite furnace atomic absorption spectrometry, lead, chemical composition, chemical detection techniques, metal speciation, treatment, physicochemical, other - risk management, drinking water contaminants, cadmium, heavy metals, ion exchange

Progress and Final Reports:

Original Abstract
  • 1995

  • Main Center Abstract and Reports:

    R825511    HSRC (1989) - Northeast HSRC

    Subprojects under this Center: (EPA does not fund or establish subprojects; EPA awards and manages the overall grant for this center).
    R825511C001 Development of Mechanisms and Kinetic Models on Formation of Polychlorinated Dibenzo-p-Dioxins and Dibenzofurans from Aromatic Precursors
    R825511C002 Real-Time Monitoring and Control of Emissions from Stationary Combustors and Incinerators
    R825511C003 Development of Sampling Systems for Continuous Monitoring of Volatile Organic Compounds (VOCs)
    R825511C004 Investigation into the Effectiveness of DNAPL Remediation Strategies in Fractured Media
    R825511C005 Advanced Leak Detection and Location Research: Extending the SERDP-funded Technical Base
    R825511C006 Three-Dimensional Geostatistical Site Characterization with Updating
    R825511C007 Anaerobic Biodegradation of PAHs in Soils and Dredged Sediments: Characterizing, Monitoring and Promoting Remediation
    R825511C008 Substrate Accelerated Death and Extended Lag Phases as Causes of the Recalcitrance of Halogenated Compounds in Anoxic Environments
    R825511C009 Fate and Transport of Nonionic Surfactants
    R825511C010 In Situ Degradation of Petroleum Hydrocarbons and PAHs in Contaminated Salt Marsh Sediments
    R825511C011 Design and Operation of Surfactant-Enhanced Bioslurry Reactors
    R825511C012 Experimental Study of Overland Transport of Cryptosporidium parvum Oocysts
    R825511C013 Development of a Framework for Evaluation of Leaching from Solid Waste
    R825511C014 Use of a New Leaching Test Framework for Evaluating Alternative Treatment Processes for Mercury Contaminated Mixed Waste (Hazardous and Radioactive)
    R825511C015 Field Pilot Test of In Situ Ultrasonic Enhancement Coupled With Soil Fracturing to Detoxify Contaminated Soil
    R825511C016 Development of Sampling Systems for Continuous Monitoring of Volatile Organic Compounds (VOCs)
    R825511C017 Field Demonstration of the Use of Reactive Zero-Valence Iron Powder to Treat Source Zone Sites Impacted by Halogenated Volatile Organic Chemicals
    R825511C018 Technology Transfer of Continuous Non-Methane Organic Carbon (C-NMOC) Analyzer
    R825511C019 Field Sampling and Treatability Study for In-Situ Remediation of PCB's and Leachable Lead with Iron Powder
    R825511C020 Experimental and Modeling Studies of Chlorocarbon Incineration, PIC Formation, and Emissions Control
    R825511C021 Experimental Studies and Numerical Modeling of Turbulent Combustion During Thermal Treatment of Hazardous Wastes: Applied Research for the Generation of Design and Diagnostic Tools
    R825511C022 Electrochemical Sensor for Heavy Metals in Groundwater - Phase IV
    R825511C023 Novel Molecular Tools for Monitoring In-Situ Bioremediation
    R825511C024 Surfactant-Enhanced Bioremediation of Soils in the Presence of an Organic Phase
    R825511C025 Enhanced Microbial Dechlorination of PCBs and Dioxins in Contaminated Dredge Spoils
    R825511C026 Toward A Risk-Based Model for Bioremediation of Multicomponent NAPL Contaminants
    R825511C027 Removal and Recovery of VOCs and Oils from Surfactant-Flushed Recovered Water by Membrane Permeation
    R825511C029 Field Pilot Test of In-Situ Ultrasonic Enhancement Coupled With Soil Fracturing to Detoxify Contaminated Soil in Cooperation with McLaren/Hart Environmental Engineers at the Hillsborough, NJ Site
    R825511C030 In-Situ Field Test of Electroremediation of a Chromate-Contaminated Site in Hudson County, New Jersey
    R825511C031 Electrokinetic Removal of Heavy Metals and Mixed Hazardous Wastes from Partially and Fully Saturated Soils
    R825511C032 Effects of Clay Charge and Confining Stresses on Soil Remediation by Electroosmosis
    R825511C033 Assessment of Surfactant Enhanced Bioremediation for Soils/Aquifers Containing Polycyclic Aromatic Hydrocarbons (PAHs)
    R825511C034 In-Situ Bioremediation of Organic Compounds: Coupling of Mass Transfer and Biodegradation
    R825511C035 Investigation into the Effectiveness of DNAPL Remediation Strategies in Fractured Media
    R825511C036 Field Pilot Scale Demonstration of Trench Bio-Sparge: An In-Situ Groundwater Treatment Technology
    R825511C037 In-Situ Reductive Dehalogenation of Aliphatic Compounds by Fermentative Heterotrophic Bacteria
    R825511C038 The Effect of Carbon-Nitrogen Ratios on Bacterial Transport and Biodegradation Rates In Soils
    R825511C039 Ultrasonic Enhancement of Soil Fracturing Technologies for In-Situ Detoxification of Contaminated Soil
    R825511C040 Full Field Demonstration of Integrated Pneumatic Fracturing and In-Situ Bioremediation
    R825511C041 Determination of Adsorption and Desorption Behavior of Petroleum Products on Soils
    R825511C042 Evaluation of the Potential for Complete Bioremediation of NAPL-Contaminated Soils Containing Polycyclic Aromatic Hydrocarbons (PAHs)
    R825511C043 Characterization of Subsurface NAPL Distributions at Heterogeneous Field Sites
    R825511C044 Development of a Thermal Desorption Gas Chromatograph/Microwave Induced Plasma/Mass Spectrometer (TDGC/MIP/MS) for On-site Analysis of Organic and Metal Contaminants
    R825511C045 Using Trainable Networks for a Three-dimensional Characterization of Subsurface Contamination
    R825511C046 Application of Advanced Waste Characterization to Soil Washing and Treatment
    R825511C047 Electrochemical Sensor for Heavy Metals in Groundwater Phase III
    R825511C048 Improved Luminescence Sensors for Oxygen Measurement
    R825511C049 Preconcentration, Speciation and Determination of Dissolved Heavy Metals in Natural Waters, using Ion Exchange and Graphite Furnace Atomic Absorption Spectrometry
    R825511C050 Experimental and Modeling Studies of Chlorocarbon Incineration and PIC Formation
    R825511C051 PIC Emission Minimization: Fundamentals and Applications
    R825511C052 Project Title: Development of a Two Stage, Pulse Combustion, VOC Destruction Technology
    R825511C053 Development of Sampling Systems for Continuous Monitoring of Volatile Organic Compounds (VOCs)
    R825511C054 FTIR Analysis of Gaseous Products from Hazardous Waste Combustion
    R825511C055 Toxic Metals Volatilization for Waste Separation and Real-time Metals Analyses
    R825511C056 Mixed Metal Removal and Recovery by Hollow Fiber Membrane-Based Extractive Adsorber
    R825511C057 Removal of Volatile Organic Compounds (VOCs) from Contaminated Groundwater and Soils by Pervaporation
    R825511C058 Simultaneous SO2/NO Removal/Recovery by Hollow Fiber Membrane
    R825511C059 Superfund Sites and Mineral Industries Method
    R825511C060 Soil Washing of Mixed Organics/Metal Contamination
    R825511C061 Removal of Cesium, Strontium, Americium, Technetium and Plutonium from Radioactive Wastewater
    R825511C062 Development of a Method for Removal of Nonvolatile Organic Materials from Soil using Flotation
    R825511C063 Recovery of Evaporative Fuel Losses by Vapor Permeation Membranes
    R825511C064 Surfactant Selection Protocol for Ex Situ Soil Washing
    R825511C065 Biofiltration for the Control of Toxic Industrial VOCs Emissions
    R825511C066 Catalytic Oxidation of Volatile Organic Compounds in Water
    R825511C067 Soil Washing for Remediating Metal Contaminated Soils
    R825511C068 Aqueous Absorption and Kinetics of NO by Strong Oxidizing Agents
    R825511C069 Remediation of Dredging Spoils
    R825511C070 Freeze Concentration for Zero-Effluent Processes
    R825511C071 Life Cycle/Pollution Prevention Response to Executive Order 12856
    R825511C072 Faster Better, Cheaper Hazardous Waste Site Characterization and Cleanup: an Adaptive Sampling and Analysis Strategy Employing Dynamic Workplans
    R825511C073 Development of a Comprehensive Computer Model for the Pneumatic Fracturing Process
    R825511C074 Technology Demonstration and Validation of CFAST Field Analytical Instrumentation for Use in Hazardous Waste Site Characterization, Clean-up and Monitoring
    R825511C075 XFLOW: Training Software Simulating Contaminant Site Characterization and Remediation