Five soil sample splitting methods (riffle splitting, paper cone riffle splitting, fractional shoveling, coning and quartering, and grab sampling) were evaluated with synthetic samples to verify Pierre Gy sampling theory expectations. Individually prepared samples consisting of layers of sand, NaCl and magnetite were left layered until splitting to simulate stratification from transport or density effects. Riffle splitting performed the best, with approximate 99% confidence levels of less than 2%, followed by paper cone riffle splitting. Coning and quartering and fractional shoveling were associated with significantly higher variability and also took much longer to perform. Common grab sampling was the poorest performer, with approximate 99% confidence levels of 100%±150% and biases of 15%±20%. Method performance rankings were in qualitative agreement with expectations from Gy sampling theory. Precision results depended on the number of increments, the type of increment, and other factors influencing the probability of selecting a particle at random, and were all much higher than Pierre Gy's fundamental error estimate of 1%. A critical factor associated with good performance for these methods is a low conditional probability of sampling adjacent particles. Accuracy levels were dominated by the sampling process rather than by the analytical method. Sampling accuracy was at least two orders of magnitude worse than the accuracy of the analytical method. Published in
The method described in this paper is a strict protocol for X-ray diffraction (XRD) analysis of mineral phases found in soils. Its application is not restricted to soils and is an attempt to standardize XRD sample preparation and analysis. The protocol requires the particle size of the < 2 mm - 0.002 mm fraction be reduced to 0.002 mm before analysis. In die qualitative section, the clay fraction ( < 0.002 mm particle size) is prepared as oriented slides. The suspended clay fraction is saturated with ethylene glycol, K +, and Mg+2; pipeted; air-dried; heat-treated at 110°C, 350°C, and 550°C; and X-rayed at each step in order to properly identify the clay minerals. In the quantitative section, the method employs a matrix-flushing agent, corundum (Al2O3). The corundum acts also as an internal standard, a calibration standard, and a reference standard. The suspended clay fraction is freeze-dried and corundum is added to each sample. Randomly oriented powder mounts are prepared from the < 2 mm - 0.002 mm fraction, and the < 0.002 mm fraction, and X-rayed. A series of reference standards are prepared based on the existing mineralogy, corundum is added, and each mixture is X-rayed. The software integrates the area under specific peaks (chosen for intensity and no overlap) in each sample, calculates the reference intensity ratios (RIRs) and calculates the percentage of each mineral based on the equation of Chung (1974). The attention to detail allows documentation and verification of the results yielding data of known quality.
This paper investigates the contributions of sample preparation to the analytical lower limits of detection and errors for the quantitative X-ray diffraction analysis of a simple, binary system of quartz and calcite. This study further demonstrates the danger of using only statistical and instrumental contributions to detection limits and analytical errors.
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