Gravimetrical methods

Two parameters must be measured to apply the BET equation, the pressure at the sample and the amount adsorbed at this pressure. There are tlnee conmron methods for measuring the amount of gas adsorbed, called the volumetric method, the gravimetric method and the dynamic method, of which the volumetric method is the connnonest [21],... 

With gravimetric methods, the magnitude of the buoyancy correction should be assessed. Particular attention must be paid to the adsorbent temperature because of the unavoidable gap between the sample and the balance case (cf. Section 6.2). 

Before we look more closely at specific gravimetric methods and their applications, let s take a moment to develop a broad survey of gravimetry. Later, as you read through the sections of this chapter discussing different gravimetric methods, this survey will help you focus on their similarities. It is usually easier to understand a new method of analysis when you can see its relationship to other similar methods. 

A gravimetric method in which the signal is the mass of a precipitate. 

In the previous section we used four examples to illustrate the different ways that mass can serve as an analytical signal. These examples also illustrate the four gravimetric methods of analysis. When the signal is the mass of a precipitate, we call the method precipitation gravimetry. The indirect determination of by precipi-... 

Specific details, including worked examples, are found in the sections of this chapter covering individual gravimetric methods. 

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. 

Representative Method The best way to appreciate the importance of the theoretical and practical details discussed in the previous section is to carefully examine the procedure for a typical precipitation gravimetric method. Although each method has its own unique considerations, the determination of Mg + in water and waste-water by precipitating MgNH4P04 6H2O and isolating Mg2P20y provides an instructive example of a typical procedure. 

Selected Gravimetric Method for Inorganic Cations Based on Precipitation... 

Sensitivity For any precipitation gravimetric method, we can write the following general equation relating the signal (grams of precipitate) to the absolute amount of analyte in the sample... 

Unlike precipitation gravimetry, which is rarely used as a standard method of analysis, gravimetric methods based on volatilization reactions continue to play an important role in chemical analysis. Several important examples are discussed in the following sections. 

The determination of silicon is commonly encountered in metallurgical and mining laboratories responsible for the analysis of ores, slags, and alloys. The volatilization gravimetric method, which is appropriate for samples containing high concentrations of silicon, was described earlier in Method 8.2. 

Volatilization gravimetric methods are time- and labor-intensive. Equipment needs are few except when combustion gases must be trapped or for a thermogravi-metric analysis, which requires specialized equipment. 

Gravimetric methods based on precipitation or volatilization reactions require that the analyte, or some other species in the sample, participate in a chemical reaction producing a change in physical state. For example, in direct precipitation gravimetry, a soluble analyte is converted to an insoluble form that precipitates from solution. In some situations, however, the analyte is already present in a form that may be readily separated from its liquid, gas, or solid matrix. When such a separation is possible, the analyte s mass can be directly determined with an appropriate balance. In this section the application of particulate gravimetry is briefly considered. 

A number of gravimetric methods, such as the determination of Ct in a soluble salt, have been part of the standard repertoire of experiments for introductory courses in analytical chemistry. Listed here are additional experiments that may be used to provide practical examples of gravimetry. 

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