Analysis of Flue Gas Desulfurization wastewaters b y Agilent 7700x ICP-MS

Application Note

Authors:
Richard Burrows – TestAmerica Laboratories Inc. USA
Steve Wilbur – Agilent Technologies Inc. USA

The U.S. Environmental Protection Agency (USEPA) is in the process of revising effluent guidelines for the steam electric power generating industry, due to increases in wastewater discharges as a result of Phase 2 of the Clean Air Act amendments. These regulations require SO2 scrubbing for most coal-fired plants resulting in “Flue Gas Desulfurization” (FGD) wastewaters. The revised effluent guidelines will apply to plants “primarily engaged in the generation of electricity for distribution and sale which results primarily from a process utilizing fossil-type fuel (coal, oil or gas) or nuclear fuel in conjunction with a thermal cycle employing the steam water system as a thermodynamic medium. “ [1]. This includes most large scale power plants in the United States. Effluents from these plants, especially coal-fired plants, can contain several hundred to several thousand ppm of calcium, magnesium, manganese, sodium, boron, chloride, nitrate and sulfate. Measurement of low ppb levels of toxic metals (including As, Cd, Cr, Cu, Pb Se, Tl, V and Zn) in this matrix presents a challenge for ICP-MS, due to the very high dissolved solids levels and potential interferences from matrix-based polyatomic ions. Furthermore, FGD wastewater can vary significantly from plant to plant depending on the type and capacity of the boiler and scrubber, the type of FGD process used, and the composition of the coal, limestone and make-up water used. As a result, FGD wastewater represents the most challenging of samples for ICP-MS; it is very high in elements known to cause matrix interferences, and also highly variable. To address this difficult analytical challenge, in 2009 the EPA commissioned the development of a new ICP-MS method specifically for FGD wastewaters. This method was developed and validated at TestAmerica Laboratories Inc. using an Agilent 7700x ICP-MS equipped with an Agilent ISIS-DS discrete sampling system.

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Petroleum Biomarker Analysis to Support Forensic and Risk Investigations

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July 21, 2011
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This presentation provides an introduction into the analytical methodologies used to detect petroleum biomarkers and a review of their utilization in supporting petroleum release forensics.

Nothing sparks concerns about contaminates in the environment quite like a petroleum release. Unfortunately, the events of 2010 served to heighten the awareness and need to have the capability to monitor and characterize the extent and breadth of the impact of these events.

Using Petroleum Biomarker analysis it is possible to accurately identify the source of contaminates back to the specific origin, as well as determining the absolute concentrations of priority pollutant PAHs. Both of these capabilities are important in assessing the human health risk and potential liability.

TestAmerica Laboratories has developed a suite of analytical methods to support petroleum release evaluations and the experience to analyze for petroleum biomarkers in all applicable matrices (water, soil/sediment, and bulk oils/waste).

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What curve types are permitted by the EPA to generate calibration curves?

Ask the Expert Question:
We run several instruments like IC, ICP, GCMS, etc, for water analysis. What curve types are permitted (by EPA) to generate calibration curves. For example, EPA 300.1 ask for linear least squares fit. Can weighted models be use along with this?

Experts Response:
Tthe EPA method 300.1 does not allow any other calibration method other than linear regression. However, the EPA has been known to grant Alternative Test Protocol (ATP) status to use quadratic fit calibration models, but that is only granted on a case by case basis. You would need to apply for an ATP approval from EPA in order to use anything other than linear regression for method 300.1.

ICP, GCMS allow for linear regression models, as well as other calibration models. For GCMS it is most common to use Relative Percent Difference (RPD), weighted linear regression, and quadratic curves. I suggest that you read SW846 method 8000c for an explanation of the various calibration models acceptable for organic analysis.

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Will pink coloration cause interference with analysis of wastewater when testing for Phenol?

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An industrial permittee has a wastewater that has a slight pink coloration after the pretreatment process. The samples need to be analyzed for Phenol in accordance with 40 CFR 403 and 40 CFR 136. Will the pink coloration cause interference with the analysis?

Experts Response:
The pink color will probably be removed in the distillation, but one way of being sure would be to conduct the test without the addition of the 4-aminoantipyrene color reagent. This should give a result of close to zero if there is no interference. If there is interference, the phenolics result could be approximated by subtracting the value obtained without adding the reagent to the value obtained with adding the reagent.

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Detection, Quantification and Calibration: Impacts on Data Quality in Environmental Chemistry

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June 23, 2011
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Over the last 20-30 years there have been tremendous advances in analytical instrumentation - enabling faster analysis with better precision and accuracy than ever before. We are also responding to needs for ever lower reporting limits. Adoption of The NELAC Institute (TNI) standards has also helped to improve and standardize quality control procedures across the board.

However, when we look at the fundamental techniques that we use to translate instrument response into data of "known and documented quality" - calibration, detection and quantification - nothing much has changed. This webinar will examine the current state of the art for establishing these critical method properties, and will propose some possible avenues for improvement.

The presenter is Chair of the TNI Environmental Monitoring Methods Expert Committee, currently tasked with developing new standards pertaining to detection, quantification and calibration techniques.

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Collecting and Reporting Quality Data for Vapor Intrusion

TestAmerica Ask the Expert Webinar Series
June 16, 2011
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The process of systematically evaluating the indoor inhalation risk from sub-surface vapors began with the EPA's publishing of "OSWER Draft Guidance for Evaluating the Vapor Intrusion to Indoor Air Pathway from Groundwater and Soils (Subsurface Vapor Intrusion Guidance)" in 2002. That document served as the genesis for the multitude of regulations, programs and methods that are being employed in this arena today.

As these regulations and programs have developed and matured, the clarity to the overall process of collecting and reporting quality data has become a difficult highway to navigate. This presentation will focus on clearing the landscape to facilitate navigation through the sample collection and data reporting process in support of these regulations and programs.

The presentation will be given from the perspective of an environmental testing laboratory and our 10 years of experience supporting Vapor Intrusion investigations.

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TestAmerica has a new Air, Vapor and Gas Resources Page

TestAmerica Laboratories, Inc., with over 25 years of specialized experience in air analysis, is one of the nation's largest providers of analytical support services dedicated to air, vapor and gas testing.

TestAmerica routinely shares our knowledge base of information on our broad range of method capabilities, regulatory requirements, sample collection and handling procedures, achieving defensible data and data management practices with our clients. Supported by one of the largest inventories of sampling media in the nation, TestAmerica is ready to support you with your next sampling project.

The information provided in the Air, Vapor and Gas section will assist you in your initial navigation of the complex arena of air, vapor and gas analysis.

Contact a TestAmerica Air Expert, for additional assistance with your projects, please visit TestAmerica's Air, Vapor and Gas Resource Page