9578

• UCREFRP Catalog Number: 9578
• Author: Hamilton, S. J. and e. al.
• Title: The Evaluation of Contaminant Impacts on Razorback Sucker Held in Flooded Bottomland Sites Near Grand Junction, Colorado - 1997.
• USFW Year: 2001.
• USFW - Doc Type: CAP6-WW,
• Copyright Material: NO

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Inorganic element analyses

All samples collected for selenium analysis were analyzed at the Yankton FRS, SD, using
a Perkin-Elmer model 3300 atomic absorption spectrophotometer equipped with a model
MHS-I0 hydride generator (AA-HG). The spectrophotometer was standardized with National
Institute of Standards and Technology (NIST) standard reference material 3149 (water).
Water samples were digested using a persulfate digestion technique and total selenium
determined by a modification of the method of Presser and Barnes (1984). Quality
assurance/quality control measures included determination of limit of detection, procedural
blanks for background equivalent concentration, percent relative standard deviation of triplicate
sample preparation and analysis, recovery of elements from reference material, and recovery of
digested-spiked sample solutions, and analysis-spiked samples at the AA-HG. The limit of
detection (LOD) ranged from 0.5 to 3.9 IlgfL (mean 1.4, SE 0.1, n=27). The procedure blanks
had background concentrations less than the LOD, which indicated no contamination from
reagents or sample handling. The percent relative standard deviation (triplicate sample
preparation and analysis) ranged from 0 to 8.2% (mean 4.6, SE 2.1, n=27), which indicated
consistent sample handling during preparation, digestion, and analysis. Recoveries of selenium
from NIST reference material1643c water and NIST reference material 1643d were within
Columbia Environmental Research Center (CERC) recommended ranges, which indicated the
digestion and analysis procedure accurately measured selenium concentrations. The
digested-spiked sample solutions had percent recoveries ranging from 86 to 116% (mean 101, SE
8.4, n=27), which indicated the digestion procedure did not alter the amount of spiked seleIlium
in the sample, i.e., suggested no loss of selenium in water samples during digestion procedure.
Analysis of analysis-spiked samples analyzed for matrix suppression or enhancement had.,
selenium recoveries ranging from 82 to 118% (mean 101, SE 9,0=27), which indicated no
interference from other water components.
All sediment, fish, fish egg, zooplankton, brine shrimp, commercial fish food, tadpole,
and aquatic plant samples were prepared for analyses of selenium concentrations by first
lyophilizing the sample to a constant dry weight using a Virtis Vacu-Freezer. Fish samples were
then homogenized with a food processor. Animal and plant tissue, fish food, and sediment
samples were digested using a combination nitric acid wet digestion and magnesium nitrate dry
ash technique (Pettersson et al. 1986). The dry ash procedure was accomplished in a
Thermolyne model FA1730 muffle furnace. Total selenium was determined by a modification of
the method of Presser and Barnes (1984). Quality controVquality assurance measures were the
same as for water analyses, and the results are summarized in Table 1.
Analyses of water, sediment, zooplankton, and fish egg samples collected for ICP
analysis of inorganic elements were performed at the Environmental Trace Substances Research
Center (University of Missouri), Rolla, MO. The list of elements and LOD are given in Table 2.
For water, the procedure blank had background equivalent concentrations less than the LOD for
all elements except calcium, silicon in one blank, and antimony, calcium, and titanium in a
second blank; the mean percent relative standard deviation (duplicate sample preparation and
analysis) was 3.4%; the mean spike recovery was 97%; and the recovery of trace elements in
Environmental Resources Associates reference water ERA9969TM was within recommended
ranges except for arsenic, selenium, and thallium in one analysis, and aluminum, arsenic, and
thallium in a second analysis.

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