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Determination of Nickel

By gravimetric method
Procedure
 Weigh out accurately 0.3-0.4 g of Nickel
sample salt
 Rinse and pour into a 500 mL beaker
provided with a clock glass cover and
stirring rod.
 Add 5 mL of dilute hydrochloric acid (1: 1)
and dilute to 200 mL.
 Heat the solution to 70-80 OC ,
Add a slight excess of the
dimethylglyoxime reagent (30 -35 mL)
and immediately add dilute ammonia
solution drop wise, directly to the
solution and with constant stirring
until precipitation takes place, and
then in slight excess.
Allow to stand on the steam bath for 20-
30 minutes, and test the solution for
complete precipitation when the red
precipitate has settled out.
Allow the precipitate to stand for 1 hour,
cooling at the same time.
Filter the cold solution through a
sintered-glass or porcelain filtering
crucible, previously heated to 110-120
O
C and weighed after cooling in a
desiccator
 Wash the precipitate with cold water
until free from chloride, and dry it at
110-120 OC for 45-50 minutes.
 Allow to cool in a desiccator and
weigh. Repeat the drying until
constant weight is attained.
Weigh as Ni(C4H7O2N2)2
Calculate the percentage of nickel in
the sample
Discussion
Nickel is precipitated by the addition of
an ethanolic solution of
dimethylglyoxime
{CH.C(:NOH).C(:NOH).CH, referred to
in what follows as H2DMG) to a hot,
faintly acid solution of the nickel salt,
and then adding a slight excess of
aqueous ammonia solution (free from
carbonate).
The precipitate is washed with
cold water and then weighed as
nickel dimethylglyoximate after drying
at 110- 120 OC .
With large precipitates, or in work of
high accuracy, a temperature of 150
O
C should be used: any reagent that
may have been carried down by the
precipitate is volatilised.
 Ni2+(aq) + 2H2DMG(aq) Ni(HDMG)2(s) + 2H+(aq)
Formula Structure of Ni(HDMG)2

N N

Ni

N N
The precipitate is soluble in:
1.Free mineral acids (even as little
as is liberated by reaction in
neutral solution)
2.Solutions containing more than
50 per cent of ethanol by volume,
3.Hot water (0.6 mg per 100 mL),
4.Concentrated ammoniacal
solutions of cobalt salts,
The precipitate is insoluble in:
1.Dillute ammonia solution,
2.Solutions of ammonium salts
3.Dillute acetic (ethanoic) acid-
sodium acetate solutions.
 Large amounts of aqueous ammonia and
of cobalt, zinc, or copper retard the
precipitation; extra reagent must be
added, for these elements consume
dimethylglyoxime to form various soluble
compounds.
 Better results are obtained in the presence
of cobalt, manganese, or zinc by adding
sodium or ammonium acetate to
precipitate the complex;
 iron(III), aluminium, and chromium(III)
must be absent
 Dimethylglyoxime forms sparingly soluble
compounds with palladium,platinum, and
bismuth.
 Palladium and gold are partially
precipitated in weakly ammoniacal
solution;
 In weakly acid solution palladium is
quantitatively precipitated and gold
partially.
 Bismuth is precipitated in strongly basic
solution
 These elements, and indeed all the
elements of the hydrogen sulphide
group,should be absent.
 Iron(II) yields a red-coloured soluble
complex in ammoniacal solution and leads
to high results if much of it is present.
 Silicon and tungsten interfere only when
present in amounts of more than a few
milligrams.
 Iron(III), aluminium, and chromium(III) are
rendered inactive by the addition of a
soluble tartrate or citrate, with which these
elements form complex ions.
Dimethylglyoxime is almost insoluble
in water, and is added in the form of a
1 per cent solution in 90% ethanol
(rectified spirit) or absolute ethanol;
1 mL of this solution is sufficient for
the precipitation of 0.0025 g of nickel.
As already pointed out, the reagent is
added to a hot feebly acid solution of
a nickel salt, and the solution is then
rendered faintly ammoniacal.
This procedure gives a more easily
filterable precipitate than does direct
precipitation from cold or from
ammoniacal solutions.
Only a slight excess of the reagent
should be used, since dimethylglyoxime
is not very soluble in water or in very
dilute ethanol and may precipitate; if a
very large excess is added (such that
the alcohol content of the solution
exceeds 50 per cent), some of the
precipitate may dissolve.