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Gravimetric analysis

physical science Maturity 9-11 Next article →

Gravimetric analysis is a highly precise method used in analytical chemistry. It is used for the quantitative determination of an analyte. An analyte is the specific ion being analyzed within a mixture. This method works by determining the mass of the analyte. To do this, the analyte must first be turned into a unique, pure compound. Once the mass of this compound is known, scientists can calculate the mass of the original analyte. This is possible as long as the quantities of other parts in the mixture are known.

Potassium hexachloroplatinate(IV)
Potassium hexachloroplatinate(IV)

The core mechanism of gravimetry involves changing the phase of the analyte. A phase change means moving from one state, like a liquid, to another, like a solid or a gas. By changing the phase, the analyte can be separated from the original mixture in its pure form. This process allows for extremely accurate measurements. In fact, gravimetric analysis was once used to determine the atomic masses of many elements. These measurements reached a precision of six figures. Because it relies on mass, it provides very little room for instrument error. It also does not require a series of standards to calculate an unknown amount.

There are four main types of gravimetric analysis. The first is precipitation, where a solid forms from a liquid solution. The second is volatilization, which involves turning a substance into a gas. The third type is electro-analytical, and the fourth is a miscellaneous physical method. Precipitation is a very common approach. For a precipitation reagent to work well, the resulting precipitate should be nonhygroscopic. This means its weight does not change based on the humidity in the air. The product should also have a high molecular weight. This makes it easier to measure even very small quantities of the analyte.

Ammonium 12-molybdophosphate
Ammonium 12-molybdophosphate

Precipitation can be a complex process with certain challenges. One problem is impurities in the solid. These impurities can be caused by occlusions or surface adsorption. Adsorption happens when other ions stick to the surface of the precipitate. To avoid this, scientists sometimes use homogeneous precipitation. This is the formation of a precipitate from a single, uniform solution. An example of this is the formation of barium sulfate. Another challenge is that the solubility of a precipitate can be affected by other ions. For instance, the solubility of silver chloride can increase significantly in the presence of certain anions.

Different chemical agents can be used to target specific elements. To quantify potassium, scientists use hexachloroplatinic acid as a precipitating agent. This creates potassium hexachloroplatinate, which is easy to weigh. To find phosphate, ammonium molybdate is added to a solution. This results in a precipitate called ammonium phosphomolybdate.

Ammonium 12-molybdophosphate
Ammonium 12-molybdophosphate

Scientists also use organic ligands to find specific metal ions. For example, treating nickel ions with dimethylglyoxime creates a bright red precipitate. Similarly, 8-hydroxyquinoline can be used to find aluminium by creating aluminium tris(8-Hydroxyquinolinate).

Tris(8-hydroxyquinolinato)aluminium
Tris(8-hydroxyquinolinato)aluminium

Volatilization methods use thermal or chemical energy to isolate a substance. In these methods, the analyte is removed by heating or chemical decomposition. This turns the analyte into a volatile species, which is a gas. One example involves determining the calcium content in water. Scientists add oxalic acid to precipitate calcium oxalate. This precipitate is then ignited at a high, red heat in the air. This heat converts the calcium oxalate into calcium oxide. By weighing the substance before and after this process, the mass of the analyte lost can be revealed. This allows scientists to calculate the percent concentration of the analyte in the original mix.

Another example of volatilization is isolating sodium bicarbonate from a mixture. This is the main ingredient in many antacid tablets. Scientists add dilute sulfuric acid to the solution. Then, nitrogen gas is bubbled through the flask. The gas carries carbon dioxide out of the solution. The gas passes through a drying agent like calcium sulfate to remove water vapor. It then passes through a mixture of sodium hydroxide on a silicate base. This mixture absorbs the carbon dioxide. By measuring the increase in mass of this absorbent, the mass of the carbon dioxide is found.

Tris(8-hydroxyquinolinato)aluminium
Tris(8-hydroxyquinolinato)aluminium

While gravimetric analysis is incredibly accurate, it has some limitations. It usually only allows for the analysis of one or a few elements at a time. The methods can also be quite convoluted, meaning they involve many steps. Because of this, gravimetric analysis has been partly displaced by spectroscopic methods. Spectroscopy is often faster and requires less intervention. However, gravimetry remains so reliable that it is used to calibrate other instruments. Instead of using separate reference standards, scientists use the high accuracy of gravimetry to ensure other machines are working correctly.

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🖼️ Images & Media (3)
File:Potassium hexachloroplatinate(IV).jpg
Potassium hexachloroplatinate(IV).jpg
File:Ammonium 12-molybdophosphate.jpg
Ammonium 12-molybdophosphate.jpg
File:Tris(8-hydroxyquinolinato)aluminium.jpg
Tris(8-hydroxyquinolinato)aluminium.jpg
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