Development of a diffusive sampling method for determination of methyl isocyanate in air

A diffusive sampling method for determination of methyl isocyanate in air has been developed. A glass fibre filter impregnated with 1-(2-methoxyphenyl)piperazine in a commercially available diffusive sampling device was used to collect methyl isocyanate and the derivative formed was analysed with LC-MS/MS. The sampling rate was determined to be 15.6 ml min(-1), with a relative standard deviation of 7.3%. The sampler was validated for sampling periods from 15 min to 8 h, for relative humidities from 20% to 80% and for concentrations from I to 46 microg m(-3). A field validation was also made and the diffusive sampling results showed no difference compared to a pumped reference method. The impregnated filters have to be stored apart from the diffusive sampler housing and loaded into the sampler prior to each sampling.     

A comparison of X-ray fluorescence and wet chemical analysis of air filter samples from a scrap lead smelting operation

Personal and area air samples were taken at a scrap lead smelter operation in a bullet manufacturing facility. Samples were taken using the 37-mm styrene-acrylonitrile closed-face filter cassette (CFC, the current US standard device for lead sampling), the 37-mm GSP or "cone" sampler, the 25-mm Institute of Occupational Medicine (IOM) inhalable sampler, and the 25-mm Button sampler (developed at the University of Cincinnati). Polyvinylchloride filters were used for sampling. The filters were pre- and post-weighed, and analyzed for lead content using a field-portable X-ray fluorescence (XRF) analyzer. The filters were then extracted with dilute nitric acid in an ultrasonic extraction bath and the solutions were analyzed by inductively coupled plasma optical emission spectroscopy. The 25-mm filters were analyzed using a single XRF reading, while three readings on different parts of the filter were taken from the 37-mm filters. The single reading from the 25-mm filters was adjusted for the nominal area of the filter to obtain the mass loading, while the three readings from the 37-mm filters were inserted into two different algorithms for calculating the mass loadings, and the algorithms were compared. The IOM sampler was designed for material collected in the body of the sampler to be part of the collected sample as well as that on the filter. Therefore, the IOM sampler cassettes were rinsed separately to determine if wall-loss corrections were necessary. All four samplers gave very good correlations between the two analytical methods above the limit of detection of the XRF procedure. The limit of detection for the 25-mm filters (5 microg) was lower than for the 37-mm filters (10 microg). The percentage of XRF results that were within 25% of the corresponding ICP results was evaluated. In addition, the bias from linear regression was estimated. Linear regression for the Button sampler and the IOM sampler using single readings and the GSP using all tested techniques for total filter loading gave acceptable XRF readings at loadings equivalent to sampling at the OSHA 8-hour Action Level and Permissible Exposure Limit. However, the CFC only had acceptable results when the center reading corrected for filter area was used, which was surprising, and may be a result of a limited data set. In addition to linear regression, simple estimation of bias indicated reasonable agreements between XRF and ICP results for single XRF readings on the Button sampler filters, (82% of the individual results within criterion), and on the IOM sampler filters (77% or 61%--see text), and on the GSP sampler filters using the OSHA algorithm (78%). As a result of this pilot project, all three samplers were considered suitable for inclusion in further field research studies.     

Pre-sampling contamination of filters used in measurements of airborne (1 → 3)-β-D-glucan based on glucan-specific Limulus amebocyte lysate assay

Air sampling for (1 → 3)-β-D-glucan may be a good method for assessing inhalation exposure to airborne fungi. Pre-sampling contamination of filter media used for sampling (1 → 3)-β-D-glucan may lead to substantial exposure measurement errors. Using the Limulus amebocyte lysate assay, we tested for pre-sampling levels of (1 → 3)-β-D-glucan on three types of filters-mixed cellulose ester (MCE)[1 brand], glass fiber (GF)[1 brand], and polycarbonate (PC)[5 brands]. Levels of (1 → 3)-β-D-glucan on MCE filters exceeded 4586.1 pg per filter. Levels on GF filters averaged 135.3 (± 28.9) pg per filter (range = 94.8-160.4 pg per filter) and levels on PC filters averaged 152.4 (± 236.1) pg per filter (range = non-detectable-1760.7 pg per filter). Efforts to clean MCE and GF filters were unfeasible or unsuccessful. Sonicating PC filters for two hours in ethanol, followed by a wash in pyrogen-free water, effectively eliminated measured levels of (1 → 3)-β-D-glucan on four brands of PC filters, as compared to untreated PC filters. This pretreatment process did not appear to physically damage the PC filters. Air sampling results highlighted the potentially problematic contamination of untreated PC filters. Ensuring that sampling media are free of (1 → 3)-β-D-glucan before sampling is crucial to accurately measure levels of (1 → 3)-β-D-glucan exposure, especially in environments where levels of (1 → 3)-β-D-glucan are low.     

Evaluation of a standardized method for determining soluble silver in workplace air samples

Several occupational exposure limits and guidelines exist for silver, but the values for each depend on the chemical form of the silver compound in question. In the past, it generally was not possible, without prior knowledge of the work process, to distinguish soluble silver from insoluble silver compounds collected in workplace air samples. Therefore, analytical results were historically reported as total silver. In this study, work was conducted to evaluate a method to differentiate between the quantities of water-soluble silver compounds and total silver collected on filters. The investigation entailed an evaluation of an International Organization for Standardization method to determine soluble silver in airborne particulate matter. The study design incorporated laboratory experiments to evaluate analytical figures of merit, such as selection of appropriate filter media and extraction solution, analytical recovery, and sample stability during storage. Polytetrafluoroethylene (PTFE) filters (2 microm, 37 mm) in opaque cassettes were either spiked with known amounts of silver nitrate or contained a known mass of solid silver nitrate. Results showed that over 90% of the silver was recovered from PTFE filters. Also, field studies were conducted in which workplace air samples were collected in two silver refineries. Some of these samples were analyzed only for soluble silver while others were sequentially extracted and analyzed, first, for soluble silver, then for total silver. The mass fractions of soluble silver, as compared to total silver, were approximately 2% or less. This investigation served to validate an international standard procedure for the determination of soluble silver in workplace air samples.     

Evaluation of a novel passive sampling technique for monitoring volcanogenic hydrogen sulfide

A novel, low-cost passive sampling procedure for monitoring of volcanogenic hydrogen sulfide is reported. The technique is based on absorption of H2S onto treated sections of photographic paper, which are housed in plastic film canisters during exposure. The H2S reacts with silver halide in the photographic paper, causing a colour-change reaction from white, through brown, to black, depending on concentration of atmospheric H2S. The sampler is sensitive to < 30 ppb to approximately 1000 ppb of H2S. Here we present results from a series of optimization and quantification experiments. An active sampling procedure for rapid H2S measurement is also reported, based on absorption of H2S onto Whatman No. 41 cellulose filters treated with silver nitrate, and was shown to be quantitative using a single filter at flow rates <1.0 L min(-1) for collection of <200 microg of sulfide (as H2S). Determination of sulfide collected on the substrates was performed using a rapid flow-injection technique based on the fluorescence quenching of fluorescein mercuric acetate (FMA) by sulfide. This was optimized at a FMA concentration of 8 mg L(-1), at which 100% quenching was obtained at a solution sulfide concentration of 3 mg L(-1).     

Development of a field method for measuring manganese in welding fume

Workers who perform routine welding tasks are potentially exposed to fume that may contain manganese. Manganese may cause respiratory problems and is implicated in causing the occurrence of Parkinson-like symptoms. In this study, a field colorimetric method for extracting and measuring manganese in welding fume was developed. The method uses ultrasonic extraction with an acidic hydrogen peroxide solution to extract welding fume collected on polyvinyl chloride filters. Commercially available pre-packaged reagents are used to produce a colored solution, created by a reaction of manganese(ii) with 1-(2-pyridylazo)-2-naphthol. Absorbance measurements are then made using a portable spectrophotometer. The method detection limit and limit of quantification (LOQ) were 5.2 microg filter(-1) and 17 microg filter(-1), respectively, with a dynamic range up to 400 microg filter(-1). When the results are above the LOQ for the colorimetric method, the manganese masses are equivalent to those measured by the International Organization for Standardization Method 15202-2, which employs a strong acid digestion and analysis using inductively coupled plasma-optical emission spectrometry.     

Development and validation of methods for environmental monitoring of cyclophosphamide in workplaces

Methods to monitor contamination of workplaces with antineoplastic drugs have been developed and validated. Cyclophosphamide (CP) was used as a model compound as it is one of the most commonly used antineoplastic drugs. A wipe sampling method to detect contamination with CP at surfaces was developed. A personal air sampling method to sample gas and vapour on solid sorbent tubes and particles with filters was also developed. Wipe and filter samples were extracted and sorbent samples were eluted, all with ethyl acetate. The samples were analysed with liquid chromatography tandem mass spectrometry. (2)H(6)-labelled cyclophosphamide was used as an internal standard. The between-day precision was 2-5% for wipe samples, 4-6% for sorbent samples and 3-8% for filter samples. The limit of detection was 0.02 ng CP per sample for the wipe and filter methods and 0.03 ng CP per sample for the solid sorbent method. Wipe sampling on surfaces made of different materials resulted in mean recoveries between 78-106%. The desorption recovery was between 97-102% for the wipe samples, 97% for the sorbent samples and 101% for the filter samples. Samples were stable for up to 2 months at 5 degrees C and -20 degrees C and for about 2 d at room temperature. The developed methods were applied to the measurement of contamination with CP in a hospital pharmacy. Trace amounts of CP, 1.3 and 1.4 ng, were detected on surfaces in the pharmacy.     

Sampling and analytical methodology development for the determination of primary and secondary low molecular weight amines in ambient air

In this project, a sampling device and an analytical method have been developed to simultaneously analyse the most frequently found low molecular weight amines, including aliphatic, aromatic and alcohol amines. These amines are diethanolamine, ethanolamine, methylamine, isopropylamine, morpholine, dimethylamine, and aniline. A sampling device was developed using a 37 mm cassette with glass fibre filters impregnated with sulfuric acid. Immediately after sampling, the filter was transferred to vials containing a solution of dansyl chloride. Dansyl chloride was used for derivatisation because it forms aromatic sulfonamides that are fluorescent and easy to protonate for MS detection. The effect of using an internal standard made with the dansylated derivative of 1-(2-methoxyphenyl)piperazine (MOPIP) on the uncertainty and efficiency of the method was also evaluated. This internal standard was spiked directly onto filters. The coupling of HPLC/ESI-MS was used for the simultaneous analysis of all the derivatives. This method showed detection limits of about 0.03 microg mL(-1) to 0.3 microg mL(-1) of amine with an average expanded uncertainty of 3% to 6% depending on the amine. The methodology recoveries are close to 100% for all the amines, and the overall estimated expanded uncertainties vary between 10% and 13% depending on the amine. This new strategy will be useful in evaluating workplace air since a unique sampling system will be used, independent of the amine to be quantified.     

Air sampling of fungal spores on filters. An investigation on passive sampling and viability

In this study, glycerol was tested as a collection substrate for passive bioaerosol sampling. Filters (mixed cellulose acetate and nitrate) were soaked in glycerol and exposed for an aerosol from three different fungal species: Penicillum commune, Aspergillus versicolor and Paecilomyces variotii. The passive sampling method was compared with a closed-face polycarbonate filter sampling method. Exposure was performed in an exposure chamber. The total number of spores was determined by microscopic techniques, and the cultivable number was determined by cultivation on Malt Extract Agar dishes. The glycerol soaked filter demonstrated a good correlation with the closed-face sampler with regard to the total count. Spores stored in a pumped filter cassette were not affected by storage for up to 7 days. On the other hand, the culturability of the spores was markedly decreased after 1 day when stored on glycerol soaked filters.     

Thermally induced filter bias in TEOM mass measurement

Researchers at the National Institute for Occupational Safety and Health (NIOSH) have long used stationary tapered element oscillating microbalances (TEOMs) in laboratory settings. They have served to assess the mass concentration of laboratory-generated particulates in experimental dust chambers and they provide a reference method for comparison with other particulate-measuring instruments. Current NIOSH research is focused on further adapting TEOM technology as a wearable personal dust monitor (PDM) for coal mining occupations. This investigation's goal is to help identify, quantify, and provide means for resolving certain TEOM-related error. The present research investigated bias caused by thermal effects on filter assemblies. New filters used in the PDM for 8 h tests show an average positive bias of 25.5 microg, while similar tests of equivalent filters used in two 1400A model TEOMs show an average positive bias of 34.3 microg. The derived bias values allow correction of previously collected biased data. Also, pre-heating the filters for 24 h at 46 degrees C shows significant bias reduction, with PDM pre-heated filters subsequently averaging -3.3 microg and 1400A TEOM filters averaging 5.9 microg. On a single-point comparison to gravimetric sampling, a 25.5 microg bias is only significant at low mass loadings. At 2.5 mg, this bias represents a negligible 1% of the mass measurement. If ordinary linear regression is used, the bias is still insignificant. However, if the more valid weighted linear regression is used, it gives more weight to the smaller dependent variable values, which are more impacted by the bias. Consequently, what is 1% bias on a single high-mass value can translate into a larger bias percentage at high-mass values when performing a weighted regression on data that include a large number of low-mass values.     

Diffusive sampling of methyl isocyanate using 4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole (NBDPZ) as derivatizing agent

A diffusive sampling method for the determination of methyl isocyanate (MIC) in air is introduced. MIC is collected using a glass fiber filter impregnated with 4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole (NBDPZ). The urea derivative formed is desorbed from the filter with acetonitrile and analyzed by means of high-performance liquid chromatography (HPLC) using fluorescence detection (FLD) with lambdaex = 471 nm and lambdaex = 540 nm. Additionally, a method was developed using tandem mass spectrometric (MS-MS) detection, which was performed as selected reaction monitoring (SRM) on the transition [MIC-NBDPZ + H]+ (m/z 307) to [NBDPZ + H]+ (m/z 250). The diffusive sampler was tested with MIC concentrations between 1 and 35 microg m(-3). The sampling periods varied from 15 min to 8 h, and the relative humidity (RH) was set from 20% up to 80%. The sampling rate for all 15 min experiments was determined to be 15.0 mL min(-1) (using HPLC-FLD) with a relative standard deviation of 9.9% for 56 experiments. At 80% RH, only 15 min sampling gave acceptable results. Further experiments revealed that humidity did not affect the MIC derivative but the reagent on the filter prior to and during sampling. The sampling rate for all experiments (including long term sampling) performed at 20% RH was found to be 15.0 mL min(-1) with a relative standard deviation of 6.3% (N = 42). The limit of quantification was 3 microg m(-3) (LC-MS-MS: 1.3 microg m(-3)) for 15 min sampling periods and 0.2 microg m(-3) (LC-MS-MS: 0.15 microg m(-3)) for 8 h sampling runs applying fluorescence detection.     

Elimination of ammonia interference in acidimetric determination of sulphur dioxide

Ammonia interference in acidimetric determination of sulphur dioxide can be eliminated by separate determination of ammonia in the same sample and by correction of results. However, with this addition the procedure is no longer simple.To avoid two separate determinations a selective absorption of ammonia from the air stream before it enters the absorbent solution for SO₂ has been considered. Several absorbents used to remove or to collect ammonia for subsequent determination were tested in the laboratory. Whatman No. 1 (or 41) filter papers impregnated with 3% oxalic acid solution in ethanol proved to be the most efficient for ammonia retention without an effect on SO₂. In a comparative testing over 52 days at a permanent sampling station no statistically significant difference was observed between two trains with impregnated filters and a third train where correction for ammonia, separately determined in the same sample, was performed.Regression analysis, however, showed that the results obtained in the third train are more dispersed due to accumulated errors in two analyses at low concentration levels further aggravated by conversion of ammonia to equivalent SO₂ concentrations. The removal of ammonia with impregnated filters gives better precision with less inconvenience and is therefore preferable.     

A chemosorptive cylindrical denuder designed for personal exposure measurements of isocyanates-evaluation on generated aerosols of 4,4'-methylenediphenyl diisocyanate

A denuder/filter system constructed for solvent-free personal exposure measurements was evaluated for separation of vapour and particulate 4,4'-methylenediphenyl diisocyanate (4,4'-MDI) generated from heated PUR-foam. The two different phases were collected in the denuder and on the filter, respectively, by chemosorption on a polydimethylsiloxane (SE-30)-dibutylamine (DBA) stationary phase. Both repeatability and the total mass concentration of 4,4'-MDI were similar to that obtained from the reference method, in this case an impinger/filter system. The penetration of particles through the denuder at 300 ml min(-1) was nearly 100% in the particle size range 25 to 700 nm, which fits well with the Gormley-Kennedy equation. Denuder/filter sampling of the 4,4'-MDI aerosol at 500 ml min(-1) yielded a phase distribution that was in accordance with the results from the reference method. The method limit of detection was 6 ng m(-3) and 4 ng m(-3) for the denuder and filter, respectively, when using an air sampling flow rate of 300 ml min(-1) and a sampling period of 15 min. This is well below the Swedish occupational exposure limit (OEL) of 50 and 100 microg m(-3) for an 8-hour working day and a 5-min period, respectively.     

Direct on-filter assay of subtilisin-type proteolytic enzymes for rapid analysis of analyte captured from the workplace atmosphere

A simple assay for some proteolytic enzymes has been developed which can be performed directly on the surface of a cellulose nitrate filter used to capture the analyte during workplace monitoring for health and safety purposes. Following air sampling the analysis is performed on the filter which is retained within the air sampler. This involves two steps: first, a 15 min incubation in which the captured enzyme is dissolved and then digests an alkaline-phosphatase-labelled antibody immobilised as a small dot on the surface of the filter; and second, is a 10 min incubation with substrate solution, which follows an in situ wash under a vacuum. During the incubation colour develops on the spot at the location of the immobilised enzyme antibody conjugate. The intensity of the spot can be assessed visually within the sampler to ascertain the presence or absence of captured enzyme, or alternatively quantitative results can be obtained using an optical scanner. The limit of detection is 5 ng per filter for subtilisin (20 ng for visual discrimination between this standard and the zero). The assay is stable to the effects of ambient air sampling at 31 min(-1) for 18 h.     

Solid phase extractive preconcentration of silver from aqueous samples

N,N-dibutyl-N1-benzoylthiourea (DBBT) impregnated onto a polymeric matrix, Amberlite XAD-16 was prepared. The separation and enrichment of Ag(I) from solution was investigated. Effective extraction conditions were optimized in column methods prior to determination by atomic absorption spectrometry. The optimum pH range for quantitative adsorption is 2-5. Quantitative recovery of Ag was achieved by stripping with 1 mol L(-1) thiourea in 1 mol L(-1) HCl. The sorption capacity of resin is 0.115 mmol Ag+ g(-1) resin. The relative standard deviation and detection limit was 3.1% for 1 microg Ag+ mL(-1) solution and 0.11 microg L(-1), respectively. The method was used for the determination of silver in geological water samples.     

Portable XRF analysis of occupational air filter samples from different workplaces using different samplers: final results, summary and conclusions

This paper concludes a five-year program on research into the use of a portable X-ray fluorescence (XRF) analyzer for analyzing lead in air sampling filters from different industrial environments, including mining, manufacturing and recycling. The results from four of these environments have already been reported. The results from two additional metal processes are presented here. At both of these sites, lead was a minor component of the total airborne metals and interferences from other elements were minimal. Nevertheless, only results from the three sites where lead was the most abundant metal were used in the overall calculation of method accuracy. The XRF analyzer was used to interrogate the filters, which were then subjected to acid digestion and analysis by inductively-coupled plasma optical-emission spectroscopy (ICP-OES). The filter samples were collected using different filter-holders or "samplers" where the size (diameter), depth and homogeneity of aerosol deposit varied from sampler to sampler. The aerosol collection efficiencies of the samplers were expected to differ, especially for larger particles. The distribution of particles once having entered the sampler was also expected to differ between samplers. Samplers were paired to allow the between-sampler variability to be addressed, and, in some cases, internal sampler wall deposits were evaluated and compared to the filter catch. It was found, rather surprisingly, that analysis of the filter deposits (by ICP-OES) of all the samplers gave equivalent results. It was also found that deposits on some of the sampler walls, which in some protocols are considered part of the sample, could be significant in comparison to the filter deposit. If it is concluded that wall-deposits should be analyzed, then XRF analysis of the filter can only give a minimum estimate of the concentration. Techniques for the statistical analysis of field data were also developed as part of this program and have been reported elsewhere. The results, based on data from the three workplaces where lead was the major element present in the samples, are summarized here. A limit of detection and a limit of quantitation are provided. Analysis of some samples using a second analyzer with a different X-ray source technology indicated reasonable agreement for some metals (but this was not evaluated for lead). Provided it is only necessary to analyze the filters, most personal samplers will provide acceptable results when used with portable XRF analysis for lead around applicable limit values.     

A passive sampler for hydrogen sulfide

The silver nitrate/fluorescein mercuric acetate fluorimetric method for the measurement of atmospheric hydrogen sulfide has been adapted to passive sampling. Standard samplers have been tested and used in both indoor and outdoor environments. Sampler performance was not dependent on construction materials or sunlight intensity and gave similar results to active sampling. Two case studies were carried out, one in the Horniman Museum and its associated storage and study building, London, UK, and the other in the vicinity of a pulp and paper mill and geothermal area North Island, New Zealand. The detection limit of the samplers (50 ppt average for a one-week exposure) provides the opportunity to make measurements in a variety of locations provided exposure times are sufficiently long, i.e., up to one month in areas of low hydrogen sulfide concentration.     

Indoor air sampling of organophosphate triesters using solid phase extraction (SPE) adsorbents

In this paper we demonstrate the use of SPE cartridges for sampling of organophosphate triesters in indoor air by adsorptive enrichment. The method has been optimised for the sampling and analysis of organophosphate triesters using a 25 mg aminopropyl silica SPE cartridge. The same cartridge is used for the active air sampling as well as for the subsequent extraction and clean-up of the sample. This makes the method fast and eliminates some tedious and time-consuming manual sample handling steps. Sampling and extraction efficiency was high for the investigated organophosphates, and limit of detection was in the range 0.1-0.3 ng m(-3). The method was applied to measurements of organophosphate triesters in two lecture halls and an electronics dismantling facility, and was compared with results from common filter/adsorbent sampling at each site. Analysis was made by GC with selective detection by NPD set in phosphorus mode, and by GC-MS. Thirteen organophosphate triesters (not counting isomers) were detected in the electronic dismantling facility. Chlorinated organophosphate triesters were detected in all locations with concentrations over 1 microg m(-3) in the lecture halls. This kind of adsorptive enrichment using an SPE cartridge could be adjusted to other types of analytes as well.     

固定污染源废气中硝酸雾测定方法研究

通过国内外文献调研和硝酸雾采样方法比对实验研究,提出了固定污染源废气中的硝酸雾包括硝酸气体、硝酸液滴及颗粒物中的硝酸盐。建立了固定污染源废气中硝酸雾的分析方法：使用经1 mol/L Na₂CO₃溶液浸渍的石英滤膜捕集固定污染源废气中的硝酸雾,离子色谱法进行分析。实验结果表明：当采样体积为0.4 m³时,方法检出限为0.04 mg/m³;低、中、高浓度空白加标样品相对标准偏差均在9.2%以内,加标回收率为89.9%～117%。选取4种典型硝酸雾固定污染源废气进行实际样品采集与分析,硝酸雾质量浓度分别为1.62、1.86、1.63、19.8 mg/m³。对电子元件电镀车间固定污染源废气进行不同浓度的实际样品加标回收实验,加标回收率分别为86.0%和104%。     

Preparation, certification and interlaboratory analysis of workplace air filters spiked with high-fired beryllium oxide

Occupational sampling and analysis for multiple elements is generally approached using various approved methods from authoritative government sources such as the National Institute for Occupational Safety and Health (NIOSH), the Occupational Safety and Health Administration (OSHA) and the Environmental Protection Agency (EPA), as well as consensus standards bodies such as ASTM International. The constituents of a sample can exist as unidentified compounds requiring sample preparation to be chosen appropriately, as in the case of beryllium in the form of beryllium oxide (BeO). An interlaboratory study was performed to collect analytical data from volunteer laboratories to examine the effectiveness of methods currently in use for preparation and analysis of samples containing calcined BeO powder. NIST SRM(?) 1877 high-fired BeO powder (1100 to 1200 °C calcining temperature; count median primary particle diameter 0.12 μm) was used to spike air filter media as a representative form of beryllium particulate matter present in workplace sampling that is known to be resistant to dissolution. The BeO powder standard reference material was gravimetrically prepared in a suspension and deposited onto 37 mm mixed cellulose ester air filters at five different levels between 0.5 μg and 25 μg of Be (as BeO). Sample sets consisting of five BeO-spiked filters (in duplicate) and two blank filters, for a total of twelve unique air filter samples per set, were submitted as blind samples to each of 27 participating laboratories. Participants were instructed to follow their current process for sample preparation and utilize their normal analytical methods for processing samples containing substances of this nature. Laboratories using more than one sample preparation and analysis method were provided with more than one sample set. Results from 34 data sets ultimately received from the 27 volunteer laboratories were subjected to applicable statistical analyses. The observed performance data show that sample preparations using nitric acid alone, or combinations of nitric and hydrochloric acids, are not effective for complete extraction of Be from the SRM 1877 refractory BeO particulate matter spiked on air filters; but that effective recovery can be achieved by using sample preparation procedures utilizing either sulfuric or hydrofluoric acid, or by using methodologies involving ammonium bifluoride with heating. Laboratories responsible for quantitative determination of Be in workplace samples that may contain high-fired BeO should use quality assurance schemes that include BeO-spiked sampling media, rather than solely media spiked with soluble Be compounds, and should ensure that methods capable of quantitative digestion of Be from the actual material present are used.