Peter M. Eller

Proficiency Analytical Testing (PAT) Silica Variability, 1990–1998

Industrial hygiene laboratories use one of three analytical techniques (X-ray diffraction spectrometry, infrared absorption spectrometry, and colorimetric spectrophotometry) for the quantitative determination of crystalline silica. Interlaboratory variability historically has been high for these analyses (∼25–35% relative standard deviation). Agreement between laboratories, as measured by the American Industrial Hygiene Association Proficiency Analytical Testing program over the period April 1990 through April 1998, was studied. Analysis of over 11,000 data points (laboratory/sample/round combinations) showed some significant differences between analytical methods in their relative recovery and precision, although overall mean recoveries were similar for the three techniques. Relative recovery of colorimetric results (but not those of the X-ray or infrared results) was significantly affected by sample loading in the range 40–170 µg silica per sample. Differences on the order of 5–10% were produced in some...

A study of methods for the determination of lead and cadmium

This paper describes laboratory comparisons of precision and accuracy of some widely used methods for the determination of lead in blood and for lead and cadmium on filters. With the exception of the tantalum boat atomic absorption technique, the methods studied were found to be rugged for a variety of minor procedural changes. Recovery of cadmium from spiked filters was quantitative over a wide range of dilutions and for a variety of instrumental readout and calculation combinations.

Measurement of Multiple Inorganic Arsenic Species

While multiple species of inorganic arsenic can coexist in industrial environments, traditional air sampling methods and analysis by atomic absorption spectrometry quantify only total inorganic arsenic. The National Institute for Occupational Safety and Health (NIOSH) recently conducted laboratory experiments and field studies to develop a technique to separate mixtures of particulate inorganic arsenic compounds and arsine, and to detect and quantify arsenic trioxide vapor. A field study in a lead-acid battery manufacturing plant showed airborne particulate arsenic in Post Burn, Element Battery Repair, and Salvage and Remelt operations; measured widespread low levels of arsine; and suggested that both particulate arsenic and arsine were transported between work areas by in-plant air currents. Arsenic trioxide vapor contributed to the total airborne arsenic collected and was most prevalent in torching or welding areas. This finding suggests that, in the presence of heated arsenic sources, monitoring solely...

Summary of the NIOSH guidelines for air sampling and analytical method development and evaluation

Suggested guidelines for the development and evaluation of sampling and analytical methods for industrial hygiene monitoring have recently been published in a NIOSH technical report. These guidelines are based in part on various published approaches for method development and evaluation and serve as an attempt at a more unified experimental approach. This paper presents some salient features of this unified approach for method development and evaluation. The basic goal of the approach is to determine if the method under study meets the criterion to produce a result that fell within 25% of the true value 95 times out of 100 on average, although other factors of method performance are evaluated. The experiments proposed for the evaluation of method performance include determination of analytical recovery from the sampler, sampler capacity, storage stability of samples and effect of environmental factors. Evaluation criteria for the experimental data and procedures for the calculation of method bias, precision and accuracy are also included.

A Qualitative Sampling Device for Use at Hazardous Waste Sites

A device to draw air through up to 10 direct reading indicator tubes simultaneously has been developed. The qualitative results obtained can be used to obtain a rapid preliminary classification of the unknown chemical substances at spill scenes or at hazardous waste sites, and to devise protocols for laboratory sample analysis.

Determination of 1,3-Butadiene down to Sub-part-per-million Levels in Air by Collection on Charcoal and High-Resolution Gas Chromatography

Abstract The need for a more sensitive method for the determination of 1,3-butadiene in air led to the development of NIOSH Method 1024, in which samples are collected on tandem 400- and 200-mg coconut-shell charcoal samplers; desorbed in dichloromethane; separated by gas chromatography on an aluminum oxide, porous-layer, open-tubular, fused silica capillary column fitted with a backflushable precolumn; and detected by flame ionization. This article reports the development of the method and an assessment of its performance based on laboratory evaluations and field use. A sample volume of 25 L is recommended for 1,3-butadiene concentrations up to 100 ppm. Samples stored in a freezer are stable; a loss of 1.5 percent per day occurs at ambient temperature. The lower quantitation limit, based on maintaining desorption efficiency ≥ 75 percent, is about 40 μg/sample. The estimated limit of detection is 0.2 μg/sample. The estimated precision of the total sampling and analytical method is 6 percent relative stand...

Sampling and analytical imethods for antimony and its compounds — a review

A review of sampling and analytical procedures for antimony and its compounds is presented. Emphasis has been placed on those methods which have application to personal air or biological samples in industrial hygiene. Two analytical techniques in particular have been used most frequently--colorimetric and atomic absorption. A need for research to develop satisfactory solid sorbent sampling techniques for stibine and other volatile antimony compounds is evident.

Corrections to the Target and Critical Values for the National Institute for Occupational Safety and Health Validation Tests

In 1974 the National Institute for Occupational Safety and Health (NIOSH) and the Occupational Safety and Health Administration joined to complete exposure standards promulgated by federal regulations. In that effort NIOSH scientists developed an accuracy criterion (AC) and a statistical protocol for evaluating its fulfillment. That AC and those procedures have been widely used ever since. This article presents corrections to the target and critical coefficients of variation published as part of the statistical protocol.

Determination of Nickel Carbonyl by Charcoal Tube Collection and Furnace Atomic Absorption Spectrophotometry

Abstract A method for the determination of nickel carbonyl has been developed using acid-washed coconut shell charcoal for sample collection and graphite furnace atomic absorption spectrophotometry for measurement. The estimated relative standard deviation of the method is 0.099 and recoveries averaged 93.0%. The working range is 2 to 50 μg Ni(CO)4/m3 (0.4 to 7 ppb) for a 20-L air sample taken at 0.2 Ipm or less. Eller, P. M.: Determination of nickel carbonyl by charcoal tube collection and furnace atomic absorption.

Solid sorbent sampler for white phosphorus in air

A solid sorbent sampling tube packed with Tenax-GC is used with a personal sampling pump to collect samples of white (yellow) phosphorus vapor from air. The phosphorus is leached from the exposed sorbent into xylene and quantitated by gas chromatographic analysis. The capacity of the sorbents is in the range 10 to 20 microgramP4per100 mg of sorbent, which allows for up to 4 hrs of sampling at the OSHA Standard, 0.1 mg/m3. No interferences from red phosphorus, phosphine, water vapor, or other common gases are significant. The effects on the method of variations in temperature, pressure, humidity, sample storage and shipping conditions, and chromatographic parameters were determined.