Precipitate gravimetric analysis

A precipitation gravimetric analysis must have several important attributes. Eirst, the precipitate must be of low solubility, high purity, and of known composition if its mass is to accurately reflect the analyte s mass. Second, the precipitate must be in a form that is easy to separate from the reaction mixture. The theoretical and experimental details of precipitation gravimetry are reviewed in this section. 

Many precipitation reactions that are useful as separation techniques for gravimetric analysis fail to meet one or both of two requirements for titrimetry ... 

Solubility Considerations An accurate precipitation gravimetric method requires that the precipitate s solubility be minimal. Many total analysis techniques can routinely be performed with an accuracy of better than 0.1%. To obtain this level of accuracy, the isolated precipitate must account for at least 99.9% of the analyte. By extending this requirement to 99.99% we ensure that accuracy is not limited by the precipitate s solubility. 

In some situations the rate at which a precipitate forms can be used to separate an analyte from a potential interferent. For example, due to similarities in their chemistry, a gravimetric analysis for Ca + may be adversely affected by the presence of Mg +. Precipitates of Ca(01T)2, however, form more rapidly than precipitates of Mg(01T)2. If Ca(01T)2 is filtered before Mg(01T)2 begins to precipitate, then a quantitative analysis for Ca + is feasible. 

In a gravimetric analysis a measurement of mass or change in mass provides quantitative information about the amount of analyte in a sample. The most common form of gravimetry uses a precipitation reaction to generate a product whose mass is proportional to the analyte. In many cases the precipitate includes the analyte however, an indirect analysis in which the analyte causes the precipitation of another compound also is possible. Precipitation gravimetric procedures must be carefully controlled to produce precipitates that are easily filterable, free from impurities, and of known stoichiometry. 

Thompson, R. Q. Ghadiali, M. Microwave Drying of Precipitates for Gravimetric Analysis, /. Chem. Educ. 1993, 70, 170-171. 

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 ... 

Tetraphenylarsonium chloride (107,108) has also been used for the precipitation of the perchlorate ion in gravimetric analysis. 

The quantitative execution of chemical reactions is the basis of the traditional or classical methods of chemical analysis gravimetry, titrimetry and volumetry. In gravimetric analysis the substance being determined is converted into an insoluble precipitate which is collected and weighed, or in the special case of electrogravimetry electrolysis is carried out and the material deposited on one of the electrodes is weighed. 

Precipitation reactions have many applications. One is to make compounds. The strategy is to choose starting solutions that form a precipitate of the desired insoluble compound when they are mixed. Then we can separate the insoluble compound from the reaction mixture by filtration. Another application is in chemical analysis. In qualitative analysis—the determination of the substances present in a sample—the formation of a precipitate is used to confirm the identity of certain ions. In quantitative analysis, the aim is to determine the amount of each substance or element present. In particular, in gravimetric analysis, the amount of substance present is determined by measurements of mass. In this application, an insoluble compound is precipitated, the precipitate is filtered off and weighed, and from its mass the amount of a substance in one of the original solutions is calculated (Fig. 1.6). Gravimetric analysis can be used in environmental monitoring to find out how much of a heavy metal ion, such as lead or mercury, is in a sample of water. 

FIGURE 1.6 A step in a gravimetric analysis. An ion has come out of solution as part of a precipitate and is being filtered. The filter paper, which has a known mass, will then be dried and weighed, thereby allowing the mass of the precipitate to be determined. 

Applications The determination and quantification of oligomers from PET has been carried out using various techniques Soxhlet extraction followed by gravimetric analysis with identification by HPLC-DAD, selective precipitation of the polymer (from a trifluoroacetic acid solution), and chloroform extraction under pressure in a sealed Parr bomb [112]. Heating of a 1 g sample in 20 mL chloroform at 100 °C for 2h allows a precision of 5 %. 

For a precipitate used in gravimetric analysis magnesium ammonium phosphate has a rather high solubility (0.1 g dm 3 in water at 20°C). Hence solution volumes should be kept as low as possible and the precipitate must be filtered from cold solution. Furthermore, the solution composition must be carefully controlled to ensure the maintenance of conditions of... 

Wil Kastning of the Nebraska State Agriculture Laboratory filters barium sulfate precipitates using filtering crucibles and a vacuum system while performing a gravimetric analysis of fertilizers for sulfate content. 

Gravimetric Analysis The precipitation is guided by the concentration of the solute and of the precipitating reagent, reaction time, reaction temperature and the nature and amount of other substance(s) present in solution. 

However, it is pertinent to mention here that quite a few techniques related to measurement of pharmaceutical substances and reagents involved is more or less common to both gravimetric and volumetric analysis. Besides, in gravimetric analysis, some more additional techniques play a vital role, namely precipitation, filtration, washing of the precipitate and ignition of the precipitate. 

Theory Gravimetric analysis of proguanil hydrochloride involves the precipitation of the proguanil-cupric complex that results on the addition of ammoniacal cupric chloride solution to a solution of proguanil hydrochloride. The reaction can be expressed by the following equation ... 

Water of crystaUization in hydrated salts can be measured by thermo-gravimetric analysis. Zinc can be analyzed in an aqueous solution by AA or ICP. Sulfate can be identified by precipitation with barium chloride solution or by ion chromatography. The zinc content in the heptahydrate is determined by AA, ICP and other instrumental methods. 

Gravimetric Analysis, Inorgonic. That branch of quantitative chemical analysis.in which a desired constituent is converted (usually by precipitation) to a pure compd or element of definite, known compn, and is weighed. In a few cases, a compd or element is formed which does not contain the constituent but bears a definite mathematical relationship to it. In either case, the amount of the desired constituent can be detd from the weight and compn of the precipitate. Methods exist for the detn of all the elements by gravimetric analysis... 

In gravimetric analysis, the mass of product from a reaction is measured to determine how much unknown was present. Precipitates from gravimetric analyses are collected by filtration, washed, and then dried. Most precipitates are collected in a fritted-glass funnel (also... 

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 %. 

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