USGS-NWQL: I-3055: Antimony, total, water, hydride _AA
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Official Method Name
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Antimony, atomic absorption spectrometric, hydride |
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Current Revision
| Revised 1985 |
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Media
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WATER |
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Instrumentation
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Gaseous Hydride Method with Atomic Absorption Detection |
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Method Subcategory
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Inorganic |
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Method Source
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Citation
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Methods for the Determination of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the United States Geological Survey, Book 5, Chapter A1 Edited by Marvin J. Fishman and Linda C. Friedman |
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Brief Method Summary
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Organic antimony-containing compounds are decomposed by adding sulfuric and nitric acids and by repeatedly evaporating the sample to fumes of sulfur trioxide. The antimony so liberated, together with inorganic antimony originally present, is subsequently reacted with potassium iodide and stannous chloride, and finally with sodium borohydride to form stibine. The stibine is removed from solution by aeration and swept by a flow of nitrogen into a hydrogen diffusion flame, where it is determined by atomic absorption at 217.6 nm. |
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Scope and Application
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This method may be used to analyze water and water-suspended sediment containing at least 1 ug/L of antimony. Samples containing more than 15 ug/L need to be diluted. Total antimony in water-suspended sediment may be determined after each sample has been thoroughly mixed by vigorous shaking and a suitable sample portion has been rapidly withdrawn from the mixture. |
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Applicable Concentration Range
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1-15 ug/L |
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Interferences
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Since the stibine is freed from the original sample matrix, interferences in the flame are minimized. Selenium and arsenic, which also form gaseous hydrides, do not interfere at concentrations of 100 ug/L. Greater concentrations were not tested. |
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Quality Control Requirements
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Calibrate instrument using calibration standards (CAL). Quality control samples (QCS) and laboratory blanks (LB) analyzed at a minimum of I each after every 10 samples. (Reference OFR 95-443). |
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Sample Handling
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Container Description: 250 mL Polyethylene bottle, acid-rinsed. Treatment and Preservation: Use unfiltered sample to rinse bottles, then acidify collected sample with HNO3 to pH < 2. |
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Maximum Holding Time
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180 days |
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Relative Cost
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Less than $50 |
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Sample Preparation Methods
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