Gravimetric analysis examples

The ultimate goal of any titrimetric analysis is to determine the amount of the analyte in a sample. This involves the stoichiometry calculation mentioned in the Work the Data section of the analytical strategy flow chart in Figure 4.1. This amount of analyte is often expressed as a percentage, as it was for the gravimetric analysis examples in Chapter 3. This percentage is calculated via the basic equation for percent used previously for the gravimetric analysis examples ... 

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. 

Quantitative Calculations When needed, the relationship between the analyte and the analytical signal is given by the stoichiometry of any relevant reactions. Calculations are simplified, however, by applying the principle of conservation of mass. The most frequently encountered example of a direct volatilization gravimetric analysis is the determination of a compound s elemental composition. 

In an indirect volatilization gravimetric analysis, the change in the sample s weight is proportional to the amount of analyte. Note that in the following example it is not necessary to apply the conservation of mass to relate the analytical signal to the analyte. 

When the analyte is already present in a particulate form that is easily separated from its matrix, then a particulate gravimetric analysis may be feasible. Examples include the determination of dissolved solids and the determination of fat in foods. 

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 ... 

The aryl-substituted derivatives of [Bi(SeC6H2R3-2,4,6)3] (R = Me, Pr, Bu) are the only isolated examples of selenolate complexes. They have been characterized by mp, elemental analysis, NMR spectroscopy, and thermal gravimetric analysis, and the solid-state structure of the isopropyl-substituted derivative reveals a tricoordinate environment for bismuth [Bi-Se 2.630(8)-2.711(8) A Se-Bi-Se 92.3(2)-103.3(2)°], imposed by the steric bulk of the ligands (38). 

Following are examples of gravimetric analysis when the analyte is physically separated from the matrix. 3.6.1.1 Loss on Drying... 

When analyzing for solids in liquid samples, such as water and wastewater samples, the analysis is based on a volume of the sample rather than a weight. Thus, while this is considered an example of a gravimetric analysis because the weight of the solids is determined, a volume of the sample is measured rather than a weight. There are several categories of solids that may be determined. 

It will be very much within the scope of this chapter to discuss briefly the various important details, with specific examples wherever necessary, of volumetric analysis, gravimetric analysis and biomedical analytical chemistry. 

In certain specific cases either the pure pharmaceutical substance or dosage forms are quantitatively converted to free compound. This conversion to free compound is quantitative and hence forms the basis of gravimetric analysis. A few typical examples belonging to this category are, namely progesterone suspension sterile, progesterone tablets, sodium lauryl sulphate, mephobarbital tablets and sorbitan monooleate. 

What are the advantages of gravimetric analysis over titrimetric analysis Give suitable examples to expatiate your answer. 

The principle of solubility product is the major factor in governing the gravimetric analysis. Justify the statement adequately with appropriate examples. 

On the other hand, the P—E bond is rather labile toward hydrolysis by even trace amounts of moisture in nonaqueous solvents, producing a series of corrosive products (Scheme 5). Thermal gravimetric analysis (TGA) reveals that, in a dry state, LiPFe loses 50% of its weight at >200 °C but that, in nonaqueous solutions, the deterioration occurs at substantially lower temperatures, for example, as low as 70 X. 

As an example, gravimetric analysis can be used to determine the amount of water in hydrated barium chloride. 

The classical methods for detection and quantitation of racemization require analysis of the chiral purity of the product of a peptide-bond-forming reaction. For example, the Anderson test is used to explore a variety of reaction conditions for the coupling of Z-Gly-Phe-OH to H-Gly-OEt (Scheme 6). 9 The two possible enantiomeric tripeptides are separable by fractional crystallization, so that gravimetric analysis furnishes the racemization data. This procedure has a detection limit of 1-2% of the epimerized tripeptide. A modification by Kemp,1"1 utilizing 14C-labeled carboxy components, extends the detection limit by two to three orders of magnitude by an isotopic dilution procedure. The Young test 11 addresses the coupling of Bz-Leu-OH to H-Gly-OEt, and the extent of epimerization is determined by measurement of the specific rotation of the dipeptide product. 

An example of gravimetric analysis is the determination of Cl by precipitation with Ag+ ... 

The ideal product of a gravimetric analysis should be very pure, insoluble, and easily filterable, and it should possess a known composition. Few substances meet all these requirements, but appropriate techniques can help optimize the properties of gravimetric precipitates. For example, solubility is usually decreased by cooling the solution. 

The use of organic components increases the discrimination in soils that are otherwise similar. For example, soils that have identical Munsell color values could be discriminated by subtractive FTIR. A new ancillary method using thermal gravimetric analysis in addition to IR analysis on samples prior to and after pyrolysis has been applied to soils and could give additional valuable information for the discrimination of soils (Thermo electron corporation application note 50862). 

Internal electrolysis — Internal electrolysis, also known as spontaneous electrogravimetric analysis, is the deposition of a metal in an electrochemical cell for the purpose of gravimetric analysis without an external source of electrical energy by proper selection of the anode material. For example Ag can be determined in the presence of Pb, Cu, and Bi by use of a Cu anode. (See also electrogravimetry). 

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