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# Assaying Nickel Determination Methods

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❶The precipitate is collected, dried and ignited to high red heat which converts it entirely to calcium oxide. Weigh and measure a sample so that not over mg.

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The Q is the concentration of reactants before precipitation, S is the solubility of precipitate in the medium from which it is being precipitated.

Therefore, to get particle growth instead of further nucleation we must make the relative supersaturation ratio as small as possible.

The optimum conditions for precipitation which make the supersaturation low are:. Precipitation using dilute solutions to decrease Q b.

Slow addition of precipitating agent to keep Q as low as possible c. Stirring the solution during addition of precipitating agent to avoid concentration sites and keep Q low d. Increase solubility by precipitation from hot solution e.

Adjust the pH to increase S, but not too much increase np as we do not want to lose precipitate by dissolution f. Usually add a little excess of the precipitating agent for quantitative precipitation and check for completeness of the precipitation. Digestion of the precipitate: The precipitate is left hot below boiling for 30 min to one hour for the particles to be digested. Digestion involves dissolution of small particles and reprecipitation on larger ones resulting in particle growth and better precipitate characteristics.

This process is called Ostwald ripening. An important advantage of digestion is observed for colloidal precipitates where large amounts of adsorbed ions cover the huge area of the precipitate. Digestion forces the small colloidal particles to agglomerate which decreases their surface area and thus adsorption. You should know that adsorption is a major problem in gravimetry in case of colloidal precipitate since a precipitate tends to adsorb its own ions present in excess, Therefore, forming what is called a primary ion layer which attracts ions from solution forming a secondary or counter ion layer.

Individual particles repel each other keeping the colloidal properties of the precipitate. Particle coagulation can be forced by either digestion or addition of a high concentration of a diverse ions strong electrolytic solution in order to shield the charges on colloidal particles and force agglomeration.

Usually, coagulated particles return to the colloidal state if washed with water, a process called peptization. Washing and Filtering the Precipitate: It is crucial to wash the precipitate thoroughly to remove all adsorbed species that would add to the weight of the precipitate. One should be careful nor to use too much water since part of the precipitate may be lost. Also, in case of colloidal precipitates we should not use water as a washing solution since peptization would occur. In such situations dilute nitric acid, ammonium nitrate, or dilute acetic acid may be used.

Usually, it is a good practice to check for the presence of precipitating agent in the filtrate of the final washing solution. The presence of precipitating agent means that extra washing is required. Filtration should be done in appropriate sized Gooch or ignition filter paper.

The purpose of drying heating at about oC in an oven or ignition in a muffle furnace at temperatures ranging from oC is to get a material with exactly known chemical structure so that the amount of analyte can be accurately determined. Precipitation from Homogeneous Solution: To make Q minimum we can, in some situations, generate the precipitating agent in the precipitation medium rather than adding it. For example, to precipitate iron as the hydroxide, we dissolve urea in the sample.

Heating of the solution generates hydroxide ions from the hydrolysis of urea. Hydroxide ions are generated at all points in solution and thus there are no sites of concentration.

We can also adjust the rate of urea hydrolysis and thus control the hydroxide generation rate. This type of procedure can be very advantageous in case of colloidal precipitates.

As expected from previous information, diverse ions have a screening effect on dissociated ions which leads to extra dissociation. Solubility will show a clear increase in presence of diverse ions as the solubility product will increase. Reaction of the coin with the nitric acid oxidizes both the nickel and copper atoms and releases various oxides of nitrogen: The precipitate Ni DMG 2 initially produced by adding DMG consists of very small crystals which cannot be filtered, as they penetrate or clog the filter mat.

A more tractable precipitate is generated if the solution is simmered for an hour or more to encourage the growth of larger crystals. Such simmering of a precipitate to encourage flocculation a common technique is known as digestion. The digested precipitate is filtered and washed extensively with distilled water to remove adsorbed impurities. Extensive washing will not cause a loss of precipitate, as the Ni DMG 2 complex is extremely insoluble less than 1.

This lab requires two weeks to complete, during the first week the nickel samples will be prepared and the Ni DMG 2 will be precipitated. Between the two weeks, this precipitate will be allowed to digest, so that it can be filtered, dried and weighed during the second week. Stir to dissolve the tartaric acid and then add ammonia until slightly alkaline.

The solution should remain clear. If much iron is present it will assume a deep red color. Heat to boiling, add an excess of dimethylglyoxime solution and the ammonia until the solution has a slight odor of the reagent. Stir, allow to stand on the steam plate for 1 hr. Wash six times with hot water, dry on steam plate for one hour; cool and weigh.

## Main Topics

Experiment: Gravimetric Determination of Nickel The purpose of this experiment is to determine the % nickel (by weight) in an unknown nickel-containing ore by means of gravimetric methods. INTRODUCTION The separation of nickel from other ions in a sample is a good example of specificity in.

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The Gravimetric Determination of Nickel INTRODUCTION Nickel(II) forms a precipitate with the organic compound dimethylglyoxime, C4H6(NOH)2. The formation of the red chelate occurs quantitatively in a solution in which the pH is buffered in the range of 5 to 9. The chelation reaction that occurs is illustrated below.