National Institute for Occupational Safety and Health

Name: NIOSH Manual of Analytical Methods — Vanadium Oxides (7504)
Author: National Institute for Occupational Safety and Health

NIOSH Manual of Analytical Methods… (1994)

Summary

“NIOSH Manual of Analytical Methods — Vanadium Oxides (7504)”, published in 1994, is a work by National Institute for Occupational Safety and Health. It explores elements such as filter, sample and analyte.

Quotes from NIOSH Manual of Analytical Methods… (National Institute for Occupational Safety and Health)

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Calculate and record the normalized intensity for the analyte peak on each sample and standard:
f.
For each media blank, determine the net count for the analyte diffraction peak. Calculate the average normalized intensity, Î b, for the 6 media blanks. Determine net count, I Ag, of an interference-free silver peak on the filter following the same procedure. Scan times should be shorter for the silver peak (e.g., about 5% of scan times for analyte peaks) and should be consistent throughout the method. For each media blank, determine the net count for the silver peak. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Sampling is quantitative using the two-filter technique described.
NIOSH Manual of Analytical Methods (NMAM) , Fourth Edition, 8/15/94 VANADIUM OXIDES: METHOD 7504, Issue 2, dated 15 August 1994 - Page 6 of 10 For the analytes, biases of spiked samples were determined by assuming the volume of suspension as "true." Biases of generated samples were determined by assuming that the concentration obtained from the ICP-AES analysis of monitor AAWP filters was the "true" concentration. Instrumental imprecision increases with smaller depositions. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Calibrate each personal sampling pump with a representative sampler in line. Sample at 1.7 ± 5% L/min with a nylon cyclone or 2.2 ± 5% L/min with an HD cyclone for a total sample size of 200 to 1000 L. Do not exceed 2 mg dust loading on the filter. NOTE: Do not allow the sampler assembly to be inverted at any time. Turning the cyclone to more than 90 °C from vertical may deposit over-sized material from the cyclone body onto the filter. Obtain an area high-volume bulk sample in the vicinity of the personal sampling area. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ A large positive intercept indicates an error in determining the baseline or that an impurity is included in the measured peak. NOTE 2: Poor repeatability at a given level indicates problems in the sample preparation technique and new standards should be made. Eliminate curvature with absorption corrections based on the mass absorption coefficient of the analyte (step 15, or from Tables 2 through 4) . ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Allow the solution to return to room temperature before withdrawing aliquots. Prepare a series of standard filters over the range 0.05 to 2 mg V per sample. a. Mount a filter on the filtration apparatus. Wet the filter with ca. 3 mL of acetonitrile (for V2O 5) or isopropanol (for V 2O 3 or NH 4VO 3) . b. Turn off the stirrer and shake the bottle vigorously by hand. Immediately remove the lid and withdraw an aliquot (2 to 25 mL) from the center of the suspension. Do not adjust the volume in the pipet by expelling part of the suspension. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ For low loading levels, higher counting times will increase precision, as should sample spinning. The stated lower limit of quantitation of ca. 100 μg per analyte when the recommended analytical lines were used is an estimate based on numerous spiked and generated sample experiments. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Filter: 37-mm diameter, 5.0-μm pore size, polyvinyl chloride filter supported with backup pad in a two-piece, 37-mm cassette filter holder (preferably, conductive) held together by tape or cellulose shrink band. NOTE: Test PVC filter for THF digestion (see Step 4) . b. Cyclone: 10-mm nylon or Higgins-Dewell (HD) , or equivalent. c. Sampling head holder: Holder must keep the cassette, cyclone, and coupler together rigidly so that air enters only at the cyclone inlet. 2. Bulk sampler: PVC membrane filter, 37-mm, 5-μm pore size in two-piece filter cassette. Sample closed face at 3 L/min. 3. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Dry at 110 °C for one hour. Store in desiccator. Tetrahydrofuran (THF) , reagent grade.* Isopropanol, reagent grade. Acetonitrile, reagent grade. Glue or tape for securing silver filters to XRD holders. ”

National Institute for Occupational Safety and Health

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Quotes from NIOSH Manual of Analytical Methods… (National Institute for Occupational Safety and Health)

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