Gravimetric analysis precipitation conditions

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... 

If there is introduced into the solution from some other source an ion that is in common with an ion of the insoluble solid, the chemical equilibrium is shifted to the left, and the solubility of that solid will be greatly decreased from what it is in pure water. This is called the 11 common-ion effect." This effect is important in gravimetric analysis, where one wishes to precipitate essentially all of the ion being analyzed for, by adding an excess of the "common-ion" precipitating reagent. There is a practical limit to the excess, however, which involves such factors as purity of precipitate and possibility of complex formation. You can calculate the solubility under a variety of conditions, as illustrated in the following problem. 

The first step in perfonning gravimetric analysis is to prepare the solution. Some form of preliminary separation may be necessary to eliminate interfering materials. Also, we must adjust the solution conditions to maintain low solubility of the precipitate and to obtain it in a form suitable for filtration. Proper adjustment of the solution conditions prior to precipitation may also mask potential interferences. Factors that must be considered include the volume of the solution during precipitation, the concentration range of the test substance, the presence and concentrations of other constituents, the temperature, and the pH. 

TG has been applied extensively to the study of analytical precipitates for gravimetric analysis [9]. One example is calcium oxalate, as illustrated in Figure 2. Information such as extent of hydration, appropriate drying conditions, stability ranges for intermediate products, and reaction mechanisms can all be deduced from appropriate TG curves. Figure 2 also includes the first derivative of the TG curve, termed the DTG cmve, which is capable of revealing fine details more clearly. 

Gravimetric analysis was performed on Pr-powders precipitated from solvated Pr Oj and PrC030H and PitOH)j to determine the effects of particle size/powder preparation on the solubility of each species (Fig. 6.6). The Pr-powder precipitated at atmospheric conditions at 85 °C was the most soluble followed by the powder precipitated in the presence of at ambient temperature, and Ar at 85 °C, which were not statistically different as calculated by a t-test. The Pr-powder precipitated with COj at ambient temperature, Ar at ambient temperature, at 85 °C, CO ... 

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