Validation of the analysis of respirable crystalline silica (quartz) in foams used with CIP 10-R samplers.

Sampling the respirable fraction to measure exposure to crystalline silica is most often carried out using cyclones. However, low flow rates (<4 l min(-1)) and continuing improvement in workplace hygiene means less and less material is sampled for analysis, resulting in increased analytical uncertainty. Use of the CIP 10-R sampler, working at a flow rate of 10 l min(-1), is one attempt to solve current analytical difficulties. To check the ability of the analysis of quartz sampled on foams, known amounts of quartz associated with a matrix have been injected into foams. The results obtained show that the proposed protocol, with prior acid attack and ashing of the foams, satisfies the recommendations of EN 482 Standard [CEN. (2006) Workplace atmospheres-general requirements for the performance of procedures for the measurements of chemical agents. Brussels, Belgium: EN 482 Comité Européen de normalization (CEN).], namely an expanded uncertainty of <50% for quartz weights between 0.1 and 0.5 times the 8-h exposure limit value and <30% for quartz weights between 0.5 and 2 times the 8-h exposure limit value, assuming an exposure limit value equal to 0.1 mg m(-3). Results obtained show that the 101 reflection line allows a quartz quantity of the order of 25 µg to be satisfactorily measured, which corresponds to a 10th of the exposure limit value, assuming an exposure limit value of 0.05 mg m(-3). In this case, the 100 and 112 reflection lines with expanded uncertainties of ~50% would also probably lead to satisfactory quantification. Particular recommendations are also proposed for the preparation of calibration curves to improve the method.

Producing samples for the organization of proficiency tests. Study of the homogeneity of replicas produced from two atmosphere generation systems.

This article describes two atmosphere generation systems used for the production of replicas. The first, the Sputnic system, is based on the Sputnic air sampler developed by the National Institute of Occupational Health in Oslo (Norway). It is used to generate asbestos fibres or silica particles and allows the simultaneous production, by means of sampling on filters, of up to 114 replicas. The second is a multipurpose system that allows dust sampling on foams used with the CIP 10-R device. Twenty samples can be taken simultaneously. In total, 120 series of samples allowed characterization of the variability of the two generation systems used for the production of replicas loaded with asbestos fibres or silica dust. The coefficients of variation characterizing the dispersion of the filter loading in the Sputnic system are <10% for high densities asbestos fibre or silica dust samples. The coefficient of dispersion is on average higher when the asbestos fibre density is lower. The differences observed between the measurements taken on the different crowns of the Sputnic system are low and <2%. The results obtained with the multipurpose system show that replica dispersion is on average equal to 4%, which will allow proposal in the near future of a proficiency test dedicated to the quantitative analysis of crystalline silica on foams sampled with the CIP 10-R device.

Laboratory study of selected personal inhalable aerosol samplers.

Assessment of inhalable dust exposure requires reliable sampling methods in order to measure airborne inhalable particles' concentrations. Many inhalable aerosol samplers can be used but their performances widely vary and remain unknown in some cases. The sampling performance of inhalable samplers is strongly dependent on particle size and ambient air velocity. Five inhalable aerosol samplers have been studied in two laboratory wind tunnels using polydisperse glass-beads' test aerosol. Samplers tested were IOM sampler (UK), two versions of CIP 10-I sampler, v1 and v2 (F), 37-mm closed face cassette sampler (USA), 37-mm cassette fitted up with an ACCU-CAP insert (USA), and Button sampler (USA). Particle size-dependent sampling efficiencies were measured in a horizontal wind tunnel under a 1 m s(-1) wind velocity and in a vertical tunnel under calm air, using a specific method with Coulter(R) counter particle size number distribution determinations. Compared with CEN-ISO-ACGIH sampling criteria for inhalable dust, the experimental results show fairly high sampling efficiency for the IOM and CIP 10-I v2 samplers and slightly lower efficiencies for the Button and CIP 10-I v1 samplers. The closed face cassette (4-mm orifice) produced the poorest performances of all the tested samplers. This can be improved by using the ACCU-CAP internal capsule, which prevents inner wall losses inside the cassette. Significant differences between moving air and calm air sampling efficiency were observed for all the studied samplers.

Site comparison of selected aerosol samplers in the wood industry.

Several samplers (IOM, CIP 10-I v1, ACCU-CAP, and Button) were evaluated at various wood industry companies using the CALTOOL system. The results obtained show that compared to the CALTOOL mouth, which can be considered to be representative of the exposure of a person placed at the same location under the same experimental conditions, the concentrations measured by the IOM, CIP 10-I v1, and ACCU-CAP samplers are not significantly different (respectively, 1.12, 0.94, and 0.80 compared to 1.00), the Button sampler (0.86) being close to the ACCU-CAP sampler. Comparisons of dust concentrations measured using both a closed-face cassette (CFC) and one of the above samplers were also made. In all, 235 sampling pairs (sampler + CFC) taken at six companies provided us with a comparison of concentrations measured using IOM, CIP 10-I v1, ACCU-CAP, and Button samplers with concentrations measured using a CFC. All the studied samplers collected systematically more dust than the CFC (2.0 times more for the IOM sampler, 1.84 times more for the CIP 10-I v1 sampler, 1.68 times more for the ACCU-CAP sampler, and 1.46 times more for the Button sampler). The literature most frequently compares the IOM sampler with the CFC: published results generally show larger differences compared with the CFC than those found during our research. There are several explanations for this difference, one of which involves CFC orientation during sampling. It has been shown that concentrations measured using a CFC are dependent on its orientation. Different CFC positions from one sampling session to another are therefore likely to cause differences during CFC-IOM sampler comparisons.

Comparison of direct and indirect methods of measuring airborne chrysotile fibre concentration.

Transmission electron microscopy observations most frequently form a basis for estimating asbestos fibre concentration in the environment and in buildings with asbestos-containing materials. Sampled fibres can be transferred to microscope grids by applying either a direct [ISO (1995) Draft International ISO/DIS 10312. Ambient air. Determination of asbestos fibres. Direct transfer transmission electron microscopy procedure. Geneva, Switzerland: International Standardization Organization] or an indirect [AFNOR (1996) Détermination de la concentration en fibres d'amiante par microscopie électronique à transmission-Méthode indirecte. Cedex, France: AFNOR, p. 42; ISO (1997) Draft International ISO/DIS 13794. Ambient air. Determination of asbestos fibres. Indirect-transfer transmission electron microscopy procedure. Geneva, Switzerland: International Standardization Organization] method. In the latter case, ISO Standard 13794 recommends filtering calcination residues either on a polycarbonate (PC) filter (PC indirect method) or on a cellulose ester (CE) membrane (CE indirect method). The PC indirect method requires that fibres deposited on a PC filter be covered by a carbon layer, whereas in the CE indirect method, the CE membrane has to be directly processed using a method described in ISO Standard 10312. The purpose of this study was to compare results obtained using, on the one hand, direct preparation methods and, on the other hand, PC indirect or CE indirect methods, for counting asbestos fibres deposited on filters as a result of liquid filtration or air sampling. In direct method-based preparation, we observed that an etching time of 6-14 min does not affect the measured densities, except for fibres <1 microm deposited by liquid filtration. Moreover, in all cases, the direct method gives higher densities than the PC indirect method because of possible fibre disappearance when using the carbon evaporator implemented in the PC indirect method. The CE membrane used for sample preparation in the CE indirect method is collapsed prior to passing it through the carbon evaporator, so the fibres are less likely to disappear at this stage. We then note that the resulting fibre densities for chrysotile-loaded filters prepared using the direct method are close to those obtained with filters prepared using the CE indirect method. Our study therefore shows that, under the implemented experimental conditions, the PC and CE indirect preparation methods described in ISO Standard 13794 are not equivalent.

An International comparison of the crystallinity of calibration materials for the analysis of respirable alpha-quartz using X-ray diffraction and a comparison with results from the infrared KBr disc method.

It is important that analytical results, produced to demonstrate compliance with exposure limits are comparable, to ensure controls are monitored to similar standards. Correcting a measurement result of respirable alpha-quartz for the percentage of crystalline material in the calibration dust is good analytical practice and significant changes in the values assigned to calibration materials will affect the interpretation of results by an analyst or occupational hygiene professional. The reissue of the certification for the quartz reference material NIST 1878a in 2005 and differences in comparative values obtained by other work created uncertainty about the values of crystallinity assigned to national calibration dusts for alpha-quartz. Members of an International Organization for Standardization working group for silica measurement ISO/TC146/SC2/WG7 collaborated to investigate the comparability of results by X-ray diffraction (XRD) and to reach a consensus. This paper lists the values recommended by the working group for use with XRD analysis. The values for crystallinity obtained for some of the materials (NIST 1878, Min-U-Sil5 and A9950) were 6-7% lower than the original certification or estimates reported in other comparisons. Crystallinity values obtained by XRD gave a good correlation with BET surface area measurements (r2 = 0.91) but not with mean aerodynamic particle size (r2 = 0.31). Subsamples of two of the materials (A9950 Respirable and Quin 1 Respirable) with smaller particle size distribution than their parent material did not show any significant change in their values for crystallinity, suggesting that the area XRD measurement of these materials within the particle size range collected is more dependent on how the quartz is formed geologically or how it is processed for use. A comparison of results from laboratories using the infrared (IR) and KBr disc method showed that this method is more dependent than XRD on differences in the particle size within the respirable size range, whereas the XRD values were more consistent between the different measurement values obtained on each material. It was not possible to assign a value for percentage purity to each material for users of IR analysis. This work suggests that differences are likely to exist between the results from XRD and IR analysis when measuring 'real' workplace samples and highlights the importance of matching the particle size of the calibration material to the particle size of the workplace dust for measurements of crystalline quartz.

ALASCA proficiency testing scheme for occupational hygiene laboratories.

Nowadays, quality assurance is an important part in the environment of analytical laboratories, who need to prove their ability to perform analysis as well to handle routine control as research and development analysis. A proficiency testing scheme (PTS) is one of the possible and powerful tools to evaluate both bias and dispersion of the analysis. As far as industrial hygiene is concerned, since analytical uncertainty is insignificant with regard to sampling strategy uncertainty, laboratories could be tempted to neglect analytical uncertainty assessment as well. The department 'Métrologie des Polluants' (part of INRS) has been organising a proficiency testing scheme since 2002 with the intention of giving the most reliable performance assessment to the participant. The original features, which are also the strong points of the scheme, are: the determination of the assigned value by a method that is independent from the analytical method to be tested; the development of original tools for the fabrication of samples; the strength of the statistic model, which is based on the WASP HSL scheme model; a tool to visualize the results of participants in bias and dispersion contribution; communication with the participants; a completely computerized system to handle the participant database, the sample database, results treatment and report edition; and the use of internet facilities to allow the participant to submit the results via a secured website. All these technical and organisational points are detailed in this paper.

Occupational exposure to mineral fibres: analysis of results stored on colchic database.

The aim of this paper is to present fibre exposure data recorded on the COLCHIC database. This database consolidates all occupational exposure data collected in French companies by the Caisses Régionales d'Assurance Maladie (regional health insurance funds, CRAM) and the Institut National de Recherche et de Sécurité (national institute for research and safety, INRS). A total of 8029 concentration results, expressed in number of fibres measured by phase-contrast optical microscopy, are available for exposure to asbestos fibres, ceramic fibres and man-made mineral fibres other than ceramic fibres. Presentation of base data by activity branch, activity sector or workplace permits identification of situations, for which prevention efforts are most essential. Analysis of exposure levels during the 1986-2004 period show that these are broadly influenced by changes in the exposure limit values. Wearing of respiratory protection equipment by employees is also discussed. The data may be helpful to occupational physicians performing occupational screening of exposed workers and to epidemiologists seeking information for building job-exposures matrices. In this respect, a database (FIBREX) will be available on the INRS web site (www.inrs.fr) at the beginning of 2007. This database will provide a higher level of detail in activity and workplace description than that which was possible for practical reasons in this paper.

Effect of using a cowl when measuring the fiber number concentration by the membrane filter method.

This article compares samples taken with three different sampling heads: (1). open-faced sampling head, (2). open-faced sampling head with stainless-steel extension cowl, and (3). open-faced sampling head with graphite-impregnated extension cowl. Sampling was performed in three factories producing man-made mineral fibers (alkaline silicate fibers, refractory ceramic fibers, glass fibers). Flow rate was varied (1 L/min or 2 L/min). The average densities measured on the sampling filter for fibers of <3 microm in diameter varied from 19 to 91 fibers/mm(2). No significant difference in fiber density was observed in relation to the nature of the sampling head for fibers with a diameter of <3 microm. The deposits noted on the internal walls of the cowl were small and much less than that documented in the literature for man-made mineral fibers until now. They were greater for fibers with a diameter of >3 microm than for those with a diameter of <3 microm. For large-diameter fibers, it would appear that cowl deposit can be reduced by increasing the sampling flow rate.