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I. Kuselman 《Accreditation and quality assurance》1998,3(3):131-133
It is argued that results of uncertainty calculations in chemical analysis should be taken into consideration with some caution
owing to their limited generality. The issue of the uncertainty in uncertainty estimation is discussed in two aspects. The
first is due to the differences between procedure-oriented and result-oriented uncertainty assessments, and the second is
due to the differences between the theoretical calculation of uncertainty and its quantication using the validation (experimental)
data. It is shown that the uncertainty calculation for instrumental analytical methods using a regression calibration curve
is result-oriented and meaningful only until the next calibration. A scheme for evaluation of the uncertainty in uncertainty
calculation by statistical analysis of experimental data is given and illustrated with examples from the author's practice.
Some recommendations for the design of corresponding experiments are formulated. 相似文献
35.
《Journal of separation science》2003,26(8):701-708
A micellar electrokinetic chromatographic and a fast reversed‐phase liquid chromatographic method have been developed for determination of the purity of phenoxymethylpenicillin. The optimized running buffer composition was 40 mM phosphate–borate–125 mM SDS–3.5% (v/v) methanol. The HPLC method employed a monolithic silica C18 column and a mobile phase composed of phosphate buffer, pH 3.5, and ACN, the flow‐rate being 3.5 mL/min. Both methods were successfully validated. Linearity, intermediate precision, limits of quantitation, accuracy, and a good correlation of the HPLC and MEKC results were demonstrated. Both methods proved to be fast and reliable and sufficiently sensitive. A combination of the two methods can be very useful in impurity profiling. 相似文献
36.
Using statistically designed experiments, 12,500 observations are generated from a 4-pieced Cobb-Douglas function exhibiting increasing and decreasing returns to scale in its different pieces. Performances of DEA and frontier regressions represented by COLS (Corrected Ordinary Least Squares) are compared at sample sizes ofn=50, 100, 150 and 200. Statistical consistency is exhibited, with performances improving as sample sizes increase. Both DEA and COLS generally give good results at all sample sizes. In evaluating efficiency, DEA generally shows superior performance, with BCC models being best (except at corner points), followed by the CCR model and then by COLS, with log-linear regressions performing better than their translog counterparts at almost all sample sizes. Because of the need to consider locally varying behavior, only the CCR and translog models are used for returns to scale, with CCR being the better performer. An additional set of 7,500 observations were generated under conditions that made it possible to compare efficiency evaluations in the presence of collinearity and with model misspecification in the form of added and omitted variables. Results were similar to the larger experiment: the BCC model is the best performer. However, COLS exhibited surprisingly good performances — which suggests that COLS may have previously unidentified robustness properties — while the CCR model is the poorest performer when one of the variables used to generate the observations is omitted. 相似文献
37.
Summary A sensitive and specific method for quantitation of the steroids betamethasone, prednisolone and cortisone acetate commonly used as adulterants in locally produced herb extracts and in certain homeopathic drugs is described. Reverse-phase liquid chromatography with UV detection has been used. 相似文献
38.
Syhi-Hwan Chen 《中国化学会会志》1997,44(2):115-121
The purpose of this investigation is to try and understand the degree of arsenic poisoning in the waste water from agricultural chemical factories which release effluents into the waterways in their vicinity. The method of determination is to use the water samples, soil, fish, clams, shell-fish, etc. found in the areas along the canals and aqueducts and those which lie upstream, midstream, and downstream and also the hair samples of people living in the contiguous areas, to check for the levels of arsenic in them by emission spectroscopy. From the analysis during a one year investigation, we find that the level of As in the water creatures of Chungkang Stream and Lu-Er-Men Stream is much higher than in the other water areas of Taiwan such as along beaches and the other rivers; the levels in the hair of the people who live nearby these water courses have a certain degree of correspondence with their eating habits and the quantity of food eaten; however, even those people who eat relatively little have almost 3% As, beyond the 2 mg/kg limit allowed for human beings. We are fully aware of the high level of food contamination on Taiwan, and this fact has been taken into consideration. The effect of As contamination in the soil on agricultural produce does not seem to have any apparent relationship. By the way, the influence of the monthly average rainfall on As contamination in the soil is not obvious. 相似文献
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The epoxy-impregnated graphite tube electrode bulk modified with 2-mercaptobenzoxazole, employed in a wall-jet configuration, was found to be useful for the continuous flow and flow injection stripping voltammetric determinations of AgI, HgII and BiIII. For continuous flow, detection limits for AgI, HgII and BiIII were 1.8 × 10−10 M, 1.9 × 10−9 M and 9.5 × 10−9 M, respectively (10 min accumulation, S/N = 3). Precisions for 5.00 × 10−9 M AgI, 1.00 × 10−8 M HgII and 1.00 × 10−7 M BiIII were 10.5%, 5.77 % and 7.90% (relative standard deviations, n = 6), respectively. In the case of flow injection stripping, with a 500 μL injection loop, detection limits of 0.59 ng, 2.0 ng and 120 ng were obtained for AgI, HgII and BiIII, respectively (S/N = 3). Selected metal ions, inorganic and organic substances were investigated for interferences. The electrode was tested with a certified sample and then applied to the determinations of the metal ions in a urine and a sea-water sample. 相似文献