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Methods of Analysis by the U.S Methods of Analysis by The U.S. Geological Survey National Water Quality Laboratory—Determination of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water with Cold Vapor–Atomic Fluorescence Spectrometry Water-Resources Investigations Report 01-4132 U.S. Department of the Interior U.S. Geological Survey Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water with Cold Vapor–Atomic Fluorescence Spectrometry By John R. Garbarino and Donna L. Damrau _______________________________________________________ U.S. GEOLOGICAL SURVEY Water-Resources Investigations Report 01-4132 Denver, Colorado 2001 U.S. Department of the Interior Gale A. Norton, Secretary U.S. Geological Survey Charles G. Groat, Director The use of trade, product, or firm names in this report is for descriptive purposes only and does not imply endorsement by the U.S. Government. For additional information write to: Copies of this report can be purchased from: Chief, National Water Quality Laboratory U.S. Geological Survey U.S. Geological Survey Branch of Information Services Box 25046, Mail Stop 407 Box 25286 Federal Center Federal Center Denver, CO 80225-0046 Denver, CO 80225-0286 CONTENTS Abstract 1 Introduction 1 Analytical method 2 1. Application 2 2. Summary of method 2 3. Sample collection and storage 3 4. Quality-control samples, sampling methods, sample-collection equipment, and cleaning procedures 3 5. Contamination and interferences 4 6. Apparatus and instrumentation 5 7. Reagents and calibration standards 5 8. Sample preparation 6 9. Analytical procedure 7 10. Calculations 7 11. Reporting of results 7 Discussion of results 8 Conclusions 14 References cited 15 FIGURES 1-3. Box plots showing: 1. Results for a series of solutions based on a National Institute of Standards and Technology standard reference material preserved with acid dichromate or hydrochloric acid 9 2. Results for U.S. Geological Survey standard reference water samples Hg24 and Hg26 and two dilutions of a Baker Instra-Analyzed standard preserved in acid dichromate 11 3. The effects of using argon instead of nitrogen as the purge gas in cold vapor–atomic fluorescence spectrometry 12 4. Graph showing linear regression analysis of results for sample solutions based on two reference standards (experimental) and National Institute of Standards and Technology standard reference material (theoretical) 13 TABLES 1. Method detection limit and analytical precision for the determination of mercury by cold vapor–atomic fluorescence spectrometry 3 2. Typical instrument operating conditions 7 3. Average percent spike recoveries for mercury in reagent-water, filtered and unfiltered surface-water, and filtered and unfiltered ground-water matrices 14 Contents III CONVERSION FACTORS Multiply By To obtain Length micrometer (µm) 3.94 x 10-5 inch millimeter (mm) 3.94 x 10-2 inch nanometer (nm) 3.94 x 10-8 inch Mass gram (g) 3.53 x 10-2 ounce, avoirdupois milligram (mg) 3.53 x 10-5 ounce, avoirdupois nanogram (ng) 3.53 x 10-11 ounce, avoirdupois Volume liter (L) 2.64 x 10-1 gallon microliter (µL) 2.64 x 10-7 gallon milliliter (mL) 2.64 x 10-4 gallon Pressure kilopascal (kPa) 1.45 x 10-1 pounds per square inch Degrees Celsius (oC) may be converted to degrees Fahrenheit (oF) by using the following equation: oF = 9/5 (oC) + 32. ABBREVIATED WATER-QUALITY UNITS mg/L milligrams per liter µg/L micrograms per liter µg/mL microgram per milliliter ng/L nanograms per liter mL/min milliliters per minute L/min liters per minute IV Contents ABBREVIATIONS AND ACRONYMS ASTM American Society for Testing and Materials CASRN Chemical Abstract Service Registry Number CV–AAS cold vapor–atomic absorption spectrometry CV–AFS cold vapor–atomic fluorescence spectrometry HCl hydrochloric acid M Molar (moles per liter) LT–MDL long-term method detection level MDL(s) method detection limit(s) MRL method reporting level HNO3 nitric acid N Normal (acid equivalents per liter) NIST National Institute of Standards and Technology NWQL National Water Quality Laboratory s second sp. gr. Specific gravity SRM standard reference material SRWS(s) U.S. Geological Survey standard reference water sample(s) USEPA U.S. Environmental Protection Agency USGS U.S. Geological Survey < less than ± plus or minus GLOSSARY MDL — The method detection limit (MDL) is defined as the minimum concentration of an element that can be measured and reported with 99-percent confidence that the element concentration is greater than zero and is determined from analysis of a sample in a given matrix that contains the element of interest (U.S. Environmental Protection Agency, 2000). Contents V Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water with Cold Vapor – Atomic Fluorescence Spectrometry By John R. Garbarino and Donna L. Damrau Abstract nanograms per liter (ng/L) of mercury, and the short-term method detection limit is about An analytical method using cold vapor– 5 ng/L. The analytical variability at 50 ng/L atomic fluorescence spectrometry was is about 10 percent. developed by the U.S. Geological Survey in 2001 for the determination of organic plus This report describes the method and inorganic mercury in filtered and unfiltered compares the use of hydrochloric acid to acid natural water. This method was developed to dichromate as a field preservative. Ambient eliminate the use of acid dichromate mercury concentrations in hydrochloric acid- preservative and to provide capability to preserved samples stored in borosilicate-glass measure ambient mercury concentrations in bottles with fluoropolymer-lined caps are natural water. Dissolved mercury includes all shown to be stable for at least 30 days. oxidizable mercury species present in natural Mercury concentrations are stable for at least water that has been filtered through a 0.45- 5 months after bromine monochloride is micrometer pore size capsule filter. Whole- added to the sample bottles in the laboratory. water recoverable mercury includes dissolved The long-term average percent recoveries at mercury species and mercury species 20, 45, and 75 ng/L in reagent water, filtered adsorbed to particulate matter in unfiltered and unfiltered ground water, and filtered and natural water. Mercury species can include unfiltered surface water range from 89 to 108, elemental mercury, mercury (II), mercury (II) 96 to 103, and 94 to 98 percent, respectively. complexes, various alkyl- and phenyl- mercury compounds, and other forms of INTRODUCTION mercury. In this method, samples are collected and processed according to standard The ambient concentration for dissolved U.S. Geological Survey protocols. Samples and whole-water recoverable mercury is are preserved onsite with 6N hydrochloric generally at the parts-per-trillion level acid in a ratio of 1 to 100 in a borosilicate- (nanograms-per-liter, ng/L) for natural-water glass bottle with fluoropolymer-lined cap. samples. Measurement at this concentration Mercury species are oxidized to mercury (II) level is important because mercury by using bromine monochloride; excess bioaccumulates in living organisms. The oxidation reagent is neutralized with previous method (Fishman and Friedman, hydroxylamine hydrochloride. Elemental 1989, p. 289–291) that used cold vapor– mercury produced after adding stannous atomic absorption spectrometry (CV–AAS) chloride is purged from the solution with was not capable of measuring such low ultrapure argon gas into a cell in which the concentrations. Cold vapor–atomic mercury concentration is measured by atomic fluorescence spectrometry (CV–AFS) is fluorescence emission at 253.7 nanometers. capable of measuring 5 ng/L mercury directly, The analytical response is linear up to 125 without sample preconcentration. By Introduction 1 eliminating sample preconcentration, analysis samples. It was developed by the U.S. throughput is increased while maintaining the Geological Survey (USGS) for use in the capability to determine mercury National Water Quality Laboratory (NWQL). concentrations at levels typically regulated by It is rapid, more efficient, and can detect water-quality standards. The mercury lower concentration levels compared to concentration, organic plus inorganic species, previous USGS methods (Fishman and is determined in filtered and unfiltered Friedman, 1989, p. 289–291). This method natural-water samples by using a brominating supplements other methods of the USGS for digestion procedure that minimizes the determination of mercury that are interferences. Samples are preserved with described by Fishman and Friedman (1989) hydrochloric acid instead of acid dichromate and by Fishman (1993). The new method was solution, which has previously been used. implemented at NWQL in April 2001. This change was necessary because shipment of samples preserved with dichromate This report provides a detailed solution is restricted, and the cost of disposing description of all aspects of the method, of chromium waste is expensive. In addition, including the instrumentation, the reagents, hydrochloric acid sample preservation has the analytical procedure, and the quality- been shown as effective as sample control procedures. Mercury concentration is preservation with acid dichromate solution. reported by NWQL in micrograms per liter instead of nanograms per liter, the This report describes a method for concentration
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