Gravimetric analysis steps

Another step in laboratory automation to be achieved is the conversion of standard chemical procedures such as titrations or thermal gravimetric analysis, into unit laboratory operations. A procedure could then be selected from these laboratory operations by an expert system and translated by the system to produce a set of iastmctions for a robot. The robot should be able to obey specific iastmctions, such as taking a specified sample aliquot and titrating it using a specified reagent. 

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. 

Gravimetric analysis methods proceed with the following steps 1) the weight or volume of the prepared sample is obtained, 2) the analyte is either physically separated from the sample matrix or chemically altered and its derivative separated from the sample matrix, and 3) the weight of the separated analyte or its derivative is obtained. The data thus obtained are then used to calculate the desired results. 

Conversion of the as-deposited film into the crystalline state has been carried out by a variety of methods. The most typical approach is a two-step heat treatment process involving separate low-temperature pyrolysis ( 300 to 350°C) and high-temperature ( 550 to 750°C) crystallization anneals. The times and temperatures utilized depend upon precursor chemistry, film composition, and layer thickness. At the laboratory scale, the pyrolysis step is most often carried out by simply placing the film on a hot plate that has been preset to the desired temperature. Nearly always, pyrolysis conditions are chosen based on the thermal decomposition behavior of powders derived from the same solution chemistry. Thermal gravimetric analysis (TGA) is normally employed for these studies, and while this approach seems less than ideal, it has proved reasonably effective. A few investigators have studied organic pyrolysis in thin films by Fourier transform infrared spectroscopy (FTIR) using reflectance techniques. - This approach allows for an in situ determination of film pyrolysis behavior. 

Describe the basic steps involved in gravimetric analysis. How does this procedure help us determine the identity of a compound or the purity of a compound if its formula is known ... 

Once a sample is in solution, the solution conditions must be adjusted for the next stage of the analysis (separation or measurement step). For example, the pH may have to be adjusted, or a reagent added to react with and mask interference from other constituents. The analyte may have to be reacted with a reagent to convert it to a form suitable for measurement or separation. For example, a colored product may be formed that wUl be measured by spectrometry. Or the analyte will be converted to a form that can be volatilized for measurement by gas chromatography. The gravimetric analysis of iron as FeaOa requires that all the iron be present as iron(in), its usual form. A volumetric determination by reaction with dichromate ion, on the other hand, requires that all the iron be converted to iron(II) before reaction, and the reduction step will have to be included in the sample preparatioii. 

The steps required iu a gravimetric analysis, after the sample has been dissolved, can be summarized as follows ... 

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. 

Although preliminary separations may be required, in other instances the precipitation step in gravimetric analysis is sufficiently selective that other separations are not required. The pH is important because it often influences both the solubility of the analytical precipitate and the possibility of interferences from other substances. For example, calcium oxalate is insoluble in basic medium, but at low pH the oxalate ion combines with the hydrogen ions to form a weak acid. 8-Hydroxy-quinoline (oxine) can be used to precipitate a large number of elements, but by controlling pH, we can precipitate elements selectively. Aluminum ion can be precipitated at pH 4, but the concentration of the anion form of oxine is too low at this pH to precipitate magnesium ion. 

A one step process is described using a pre-drled vinylbenzylamlne slloxane primer, overcoated with the functional monomer, in this case acrylonitrile. Infrared analysis, tape tests, and gravimetric analysis after washing and flexing have shown the electron initiated cure grafts the primer to the film surface and simultaneously causes the copolymerization of the monomer-primer system. 

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