Scribd
Upload
19 views3 pages

Gravimetric_Estimation_Nickel

The document describes the gravimetric estimation of nickel by precipitating it as nickel dimethyl glyoxime (Ni(DMG)2) using an alcoholic solution of dimethyl glyoxime and aqueous ammonia, with a pH buffered between 5 and 9 to ensure quantitative formation of the red chelate. It emphasizes the importance of controlling reagent amounts and pH to prevent dissolution of the precipitate and minimize errors due to other metals. The nickel content is calculated stoichiometrically from the weight of the precipitate after filtration and drying.

Uploaded by

William Aldrich
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
19 views3 pages

Gravimetric_Estimation_Nickel

The document describes the gravimetric estimation of nickel by precipitating it as nickel dimethyl glyoxime (Ni(DMG)2) using an alcoholic solution of dimethyl glyoxime and aqueous ammonia, with a pH buffered between 5 and 9 to ensure quantitative formation of the red chelate. It emphasizes the importance of controlling reagent amounts and pH to prevent dissolution of the precipitate and minimize errors due to other metals. The nickel content is calculated stoichiometrically from the weight of the precipitate after filtration and drying.

Uploaded by

William Aldrich
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 3

The Gravimetric Estimation of Nickel:

The nickel is precipitated as nickel dimethyl glyoxime by adding alcoholic solution of dimethyl glyoxime
C4H6(NOH)2 and then adding a slight excess of aqueous ammonia solution.

When the pH is buffered in the range of 5 to 9, the formation of the red chelate occurs quantitatively
in a solution. The chelation reaction occurs due to donation of the electron pairs on the four nitrogen
atoms, not by electrons on the oxygen atoms. The reaction is performed in a solution buffered by
either an ammonia or citrate buffer to prevent the pH of the solution from falling below 5. If the pH
does become too low the equilibrium of the above reaction favors the formation of the nickel (II) ion,
causing the dissolution of Ni (DMG)2 back into the mother liquor.

A slight excess of the reagent has no action on the precipitate, but a large excess should be avoided
because of the possible precipitation of the reagent itself. The precipitate is soluble in the free mineral
acids. It is therefore crucial to avoid the addition of too large and excess of the reagent because it
may crystallize out with the chelate. It is also important to know that the complex itself is slightly
soluble to some extent in alcoholic solutions. By adding small amount of chelating agents will minimize
the errors from these sources. The amount of the reagent added is also governed by the presence of
other metals such as cobalt, which form soluble complexes with the reagent. If a high quantity of
these ions is present, a greater amount of DMG must be added. The nickel dimethylglyoximate is a
very bulky precipitate. Therefore, the sample weight used in the analysis must be carefully controlled
to allow more convenient handling of the precipitate during the transfer to the filtering crucible. The
compactness of the precipitate is improved by adjusting the pH to 3 or 4, followed by the addition of
ammonia solution.

A slow increase in the concentration of ammonia in the solution causes a slight increase in the pH
gradually and results in the precipitation of the complex. The result is the formation of a denser
precipitate. Once the filtrate has been collected and dried, the nickel content of the solution is
calculated stoichiometrically from the weight of the precipitate.

The structure of DMG & the complex with nickel ions is given below;
DMG

1% dimethylglyoxime and 10% ammonium hydroxide in 75%


ethanol

Nickel solution

Ni-DMG Complex

Funnel and flask


Desiccator

Ref: http://amrita.vlab.co.in/?sub=2&brch=193&sim=348&cnt=1

MW of dimethylglyoxime: 116.12 g/mol

NiDMG2 complex MW: 288.9155 ± 0.0002 g/mol

Nickel MW: 58.6934 g/mol

You might also like