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M. J. Fishman

Publications and source records attributed to M. J. Fishman.

13 recordsLinked to original sources

Indirect spectrophotometric determination of traces of bromide in water

A rapid, accurate, and sensitive indirect spectrophotometric method for the determination of bromide in natural waters is based on the catalytic effect of bromide on the oxidation of iodine to iodate by potassium permanganate in sulfuric acid solution. The method is applicable to concentrations ranging from 1 to 100 μ g. of bromide per liter, but may be modified to extend the concentration range. Most ions commonly occurring in water do not interfere. The standard deviation is 2.9 at bromide concentrations of 100 μ g. per liter and less at lower concentrations. The determination of bromide in samples containing known added amounts gave values ranging from 99 to 105% of the concentration calculated to be present.

Analytical Chemistry↗

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory-In-bottle acid digestion of whole-water samples

Water samples for trace-metal determinations routinely have been prepared in open laboratories. For example, the U.S. Geological Survey method I-3485-85 (Extraction Procedure, for Water- Suspended Sediment) is performed in a laboratory hood on a laboratory bench without any special precautions to control airborne contamination. This method tends to be contamination prone for several trace metals primarily because the samples are transferred, acidified, digested, and filtered in an open laboratory environment. To reduce trace-metal contamination of digested water samples, procedures were established that rely on minimizing sample-transfer steps and using a class-100 clean bench during sample filtration. This new procedure involves the following steps: 1. The sample is acidified with HCl directly in the original water-sample bottle. 2. The water-sample bottle with the cap secured is heated in a laboratory oven. 3. The digestate is filtered in a class-100 laminar-flow clean bench. The exact conditions used (that is, oven temperature, time of heating, and filtration methods) for this digestion procedure are described. Comparisons between the previous U.S Geological Survey open-beaker method I-3485-85 and the new in-bottle procedure for synthetic and field-collected water samples are given. When the new procedure is used, blank concentrations for most trace metals determined are reduced significantly.

Open-File Report↗

Validation of an automated fluorescein method for determining bromide in water

Surface, atmospheric precipitation and deionized water samples were spiked with ??g l-1 concentrations of bromide, and the solutions stored in polyethylene and polytetrafluoroethylene bottles. Bromide was determined periodically for 30 days. Automated fluorescein and ion chromatography methods were used to determine bromide in these prepared samples. Analysis of the data by the paired t-test indicates that the two methods are not significantly different at a probability of 95% for samples containing from 0.015 to 0.5 mg l-1 of bromide. The correlation coefficient for the same sets of paired data is 0.9987. Recovery data, except for the surface water samples to which 0.005 mg l-1 of bromide was added, range from 89 to 112%. There appears to be no loss of bromide from solution in either type of container.Surface, atmospheric precipitation and deionized water samples were spiked with mu g l** minus **1 concentrations of bromide, and the solutions stored in polyethylene and polytetrafluoroethylene bottles. Bromide was determined periodically for 30 days. Automated fluorescein and ion chromatography methods were used to determine bromide in these prepared samples. Analysis of the data by the paired t-test indicates that the two methods are not significantly different at a probability of 95% for samples containing from 0. 015 to 0. 5 mg l** minus **1 of bromide. The correlation coefficient for the same sets of paired data is 0. 9987. Recovery data, except for the surface water samples to which 0. 005 mg l** minus **1 of bromide was added, range from 89 to 112%. Refs.

Water Research↗

Pilot study for U.S. Geological Survey Standard Reference Water Samples for pesticides

The U.S. Geological Survey has been preparing and maintaining a library of standard reference water samples for inorganic constituents for 19 years. Recently, a pilot study was conducted to see if the reference-sample program could be expanded to include pesticides and other organic materials. Two samples containing organochlorine and organophosphorus insecticides, and chlorophenoxy acid herbicides were distributed to a number of laboratories in the United States. One of the samples also contained polychlorinated biphenyls. Interlaboratory data obtained from these round robin studies are presented with intralaboratory information on long-term stability.

Journal of Testing and Evaluation↗

Determination of traces of silver in waters by anion exchange and atomic absorption spectrophotometry

A method has been developed for the accurate determination of 0.1–1 μg of silver per liter of water. The method permits stabilization of silver in water without loss to container walls. Optimum conditions have been established for the complete recovery of silver from water with an anion-exchange column, for quantitative elution of silver from the resin, and for measurement of silver by atomic absorption spectrophotometry after chelation with ammonium pyrrolidine dithiocarbamate and extraction of the chelate with MIBK. Silver in the 1–10 μg 1 "> μg1 range can be determined by extraction without pre-concentration on an ion-exchange resin.

Analytica Chimica Acta↗

Catalytic determination of vanadium in water

A kinetic determination of V(V) as a catalyst was spectrophotometrically performed by using the indicator reaction of Gallamine blue (GB + ) and bromate at pH 2.0. The reaction was followed by measuring absorbance change for a fixed-time of 3 min at 537 nm. The variables such as reagent concentration, pH, buffer concentration, ionic strength and temperature were optimized to improve the selectivity and sensitivity. Under the optimized conditions, the determination of V(V) was performed in the range 1–100 μg L −1 with limits of detection and quantification of 0.31 and 0.94 μg L −1 . The developed kinetic method is sufficiently sensitive, selective and simple. It was successfully applied to the speciative determination of total V and inorganic dissolved vanadium species, V(V) and V(IV) in environmental water samples. The oxidizing property of permanganate is used to differentiate between V(IV) and V(V) species. The V(IV) content was found by subtracting the V(V) content from those of total V. The recovery is above 95% for V(V) spiked samples. Additionally, the accuracy was validated by analysis of a certified water sample, CRM TMDA-53.3, and the results were in good agreement with the certified value.

Analytical Chemistry↗