Error analysis gravimetric

The statistical uncertainty arising from the analytical measurement is derived from the automatic data collection procedure noted before. The AGAS computer performs a standard error analysis and produces both a mean and the standard error of the mean associated with that value. A computer program is used to combine the uncertainties from the primary gravimetric process with the uncertainties produced from the standard deviation of the instrument s response for each of the gas mixtures. 

GENERAL ERROR ANALYSIS - COMMON TO BOTH VOLUMETRIC AND GRAVIMETRIC... 

Determine the uncertainty for the gravimetric analysis described in Example 8.1. (a) How does your result compare with the expected accuracy of 0.1-0.2% for precipitation gravimetry (b) What sources of error might account for any discrepancy between the most probable measurement error and the expected accuracy ... 

If several fundamentally different methods of analysis for a given constituent are available, e.g. gravimetric, titrimetric, spectrophotometric, or spectrographic, the agreement between at least two methods of essentially different character can usually be accepted as indicating the absence of an appreciable systematic error in either (a systematic error is one which can be evaluated experimentally or theoretically). 

All reagents and solvents that are used to prepare the sample for analysis should be ultrapure to prevent contamination of the sample with impurities. Plastic ware should be avoided since these materials may contain ultratrace elements that can be leached into the analyte solutions. Chemically cleaned glassware is recommended for all sample preparation procedures. Liquid samples can be analyzed directly or after dilution when the concentrations are too high. Remember, all analytical errors are multiplied by dilution factors therefore, using atomic spectroscopy to determine high concentrations of elements may be less accurate than classical gravimetric methods. 

Taylor PDF, Maeck R, De Bievre P (1992) Determination of the absolute isotopic composition and Atomic Weight of a reference sample of natural iron. Int J Mass Spectrom Ion Processes 121 111-125 Taylor PDF, Maeck R, Hendrickx F, De Bievre P (1993) The gravimetric preparation of synthetic mixtures of iron isotopes. Int J Mass Spectrom Ion Processes 128 91-97 Thirlwall MF (2002) Multicollector ICP-MS analysis of Pb isotopes using a Pb- Pb double spike demonstrates up to 4000 ppm/amu systematic errors in Tl-normalization. Chem Geol 184 255-279... 

In a gravimetric analysis, plan to have enough precipitate for a low relative uncertainty. If weighing precision is 0.3 mg, a 100-mg precipitate has a relative weighing error of 0.3% and a 300-mg precipitate has an uncertainty of 0.1 %. 

The frozen-drop and the wax methods eliminate the tedious and time-consuming operations of microscopic counting of the larger droplets, and sampling errors are less likely because all of a large increment of spray can be collected and handled by employing screens and gravimetric methods of analysis. The chief limitation is that screens are not available to obtain data on particles smaller than 75 microns. Some form of microscopic count or air elutriation procedure is necessary for the smaller droplets. 

The flame must dry, vaporize, and atomize the sample in a reproducible manner with respect to both space and time. Unlike titrimetric and gravimetric analysis, atomic absorption spectrometry is a secondary analytical technique. Concentrations are determined by comparing the absorbance values obtained for samples with those obtained for standards of known determinant concentrations. It is very important, therefore, that samples and standards are always atomized with the same efficiency to produce a cloud of atomic vapour of highly reproducible geometry. If samples and standards behave differently, errors will result. 

Hence, the weight fraction oversize is calculable by measurement of P for different values of S at constant W and Q. The quickest analytical procedure is to ealculate P from gravimetric or chemical analysis of feed and overflow suspensions. Choice of flowrate and speed can be made in accordance with prior knowledge of approximate size and use of derived theoretical expressions, or by trial and error to establish the rate at which P approaches unity with maximum S. 

Sample preparation of pharmaceutical products is an important step in the analysis methodology and must be carefully carried out to avoid contamination, loss of metal(s) or addition of interferences that could result in errors in the measurements. Modem versions of the international pharmacopoeias contain methods involving atomic emission methods, and some replace tedious titration, spectrophotometer or gravimetric methods. 

The effect of a constant error becomes more serious as the size of the quantity measured decreases. The effect of solubility losses on the results of a gravimetric analysis, shown in Example 5-2, illustrates this behavior. 

The demands for accuracy frequently dictate the procedure chosen for an analysis. For example, if the allowable error in the determination of aluminum is only a few parts per thousand, a gravimetric procedure is probably required. If an error of 50 ppt can be tolerated, however, a spectroscopic or electroanalytical approach may be preferable. 

Most of the methods in use in clinical chemistry laboratories involve colorimetric analysis in fewer instances volumetric or gravimetric procedures are still retained. It is not the purpose of this review to enter into a discussion of the errors inherent in colorimetric, volumetric, and gravimetric analysis as such for a treatment of this subject the reader is referred to standard works on chemical analysis (e.g., V3). Instead, the review will be confined to those sources of error that are particularly likely to affect the work of a clinical laboratory. These errors arise mainly from the need to perform many analyses on large numbers of samples with a variable degree of urgency, and from the fact that most of these analyses have to be conducted on plasma or semm, which are viscous protein-rich fluids available only in restricted quantities (M12). 

Gravimetric analysis is a highly accurate technique, since the mass of a sample can be measured accurately. However, this procedure is applicable only to reactions that go to completion, or have nearly 100 percent yield. Thus, if AgCl were slightly soluble instead of being insoluble, it would not be possible to remove all the Cl ions from the NaCl solution and the subsequent calculation would be in error. 

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