Experiment 4

84

Winter 2014

Experiment 4: Preparation of Ammonium Nickel(II) Sulfate

Hexahydrate, (NH4)2Ni(SO4)2. 6H2O, from its Component Salts
Introduction
Nickel is a d-block element and a transition metal. Like most d-block elements, it exhibits
various oxidation states. Compounds are known that contain nickel in all of the oxidation states from 0
to +4. Nickel reacts with dilute mineral acids but is rendered passive by concentrated nitric acid. As it
only reacts with air or steam at high temperatures, it is often electroplated onto other metals as a
protective coating.
The most common oxidation state of nickel is nickel(II).

You will prepare a double salt

containing the nickel(II) ion. A double salt is prepared from stoichiometric amounts of its component
salts. No new complex ions result when the double salt is synthesized. The double salt has a more
stable crystal structure than the salts from which it is prepared.

Chemicals required
Ammonium sulfate

3.2 g

Nickel(II) sulfate hexahydrate

6.1 g

Procedure
Once the actual masses have been measured and recorded, transfer the ammonium sulfate,
(NH4)2SO4, and the nickel(II) sulfate hexahydrate, NiSO 4. 6H2O, into a 150 mL beaker. Mix the solids
together with a glass stirring rod. Add 30 mL of hot deionized water to the beaker. Warm (do not boil)
the resulting mixture using a hot plate-stirrer and stir gently with a stirring bar to dissolve the solids. A
fine pale blue precipitate may form immediately upon the addition of the water - continue stirring to
dissolve this solid. When all solids are dissolved, remove the beaker from the heat. Set it aside to
cool undisturbed at room temperature for about 45 minutes. Do not cover it with a watch glass!
Collect the crystalline precipitate by suction filtration using a Buchner funnel. Do NOT wash
the crystals with water! Wash the crystals once with 10 mL of 50% ethanol (prepare this yourself:
mix 5 mL of 95% ethanol with 5 mL of deionized water.) and then once with 10 mL of 95% ethanol. Air
dry your collected solid on a preweighed watch glass in a drawer for a week. Determine and record
your yield, calculate a percent yield and submit your labelled product when you submit your report.

Experiment 4

85

Winter 2014

Procedure (continued)
Two samples of the product have been provided for observation: Sample A has large crystals
but resulted in a low yield while sample B has small crystals but was obtained in a high yield. What
differences in experimental technique could account for these variations? Record a description and
a diagram of the appearance of both provided products as seen by the naked eye and under
the microscope. Which sample does your product most resemble? Include a description of your
product with the observations of samples A and B. Include the answers to the above questions in your
discussion.