Quartz Analysis in Bulk Samples: Sample Preparation Procedures

"The potential health effects of quartz-bearing airborne dust in mine and mill atmospheres point to the need for the quantification of quartz content in the source material for determining the source-sink relationships and for choosing applicable control measures. While a standard method exists from a regulatory point of view for the sampling of coal mine atmospheres for determining (i) respirable dust concentrations and (ii) the amount of quartz in the samples, there is no generally accepted standard method for quartz analysis in bulk samples of coal and host rocks. Generally, the bulk sample is reduced to a powder for producing quartz analysis samples. Extensive controls arc necessary to ensure representativeness of the analysis samples when these are very minute fractions of the bulk samples. Since the amount of analysis sample is not limited, alternative methods for quartz analysis may also be tried. It is, however, necessary to adopt a procedure which will satisfy several statistical requirements to guarantee representativeness of the quartz analysis samples.In this paper, the important factors in the preparation of quartz analysis samples from the host rocks and bulk samples are discussed. The method developed to prepare the analysis samples is outlined. The results of application of the procedures are presented. The procedure developed for quartz analysis sample preparation is based on sound statistical foundations. The procedure has been validated for reproducibility and homogeneity.The current methods used for quartz analysis in powders are the P-7 infrared spectrometry and quantitative X-Ray Diffraction (XRD). Both have similar restrictions concerning the sample characteristics and operational problems, which arc intrinsic to radiation beams, device geometry, mechanics and controls of the radiation behavior. Although improvements can be made in the spectrometers and diffractometers, some of the most important steps are the procedures for analysis sample preparation from bulk samples and for calibration of the instruments. The sample preparation process is often referred to as one of grinding and sizing the bulk sample to generate the powder for the scanning devices. The particle sizes are referred to and their influence emphasized but the representativeness of the sample is assumed. Assuring sample representativeness during the sample preparation procedures is critical.For the sampling of airborne respirable dust in coal mines, the collection devices, the collection procedures and the analysis procedures are defined. This is not true for bulk samples where weights must be reduced thousands of times to generate the analysis samples for the scanning devices. The specifications to be developed may include bulk sample amount, sample reduction procedures, sample particle size distribution and sample amounts. However, the common problem of insufficient sample amount which is often encountered with mine airborne dust samples need not exist for bulk samples. Further, the same bulk sample can yield analysis samples for several experiments. The latter, of course, requires sample homogeneity.Three concepts are important in the selection of any procedure for sample preparation and analysis. These arc accuracy, reproducibility and representativeness. The adopted procedure has to guarantee a homogeneous sample representative of the population, a defined level of accuracy and reproducibility. Important statistical concepts are embedded in these requirements, particularly with respect to estimation and dispersion errors. Accuracy and reproducibility are totally different though not independent concepts. Estimation is related to accuracy and the true value. Dispersion is related to reproducibility and is measured by the classical statistical standard deviation of the distribution of a series of measurements or analysis performed over the same lot or analysis sample. The dispersion variance (or dispersion error) does not tell a"