SIC 1011

LAB REPORT A3- GRAVIMETRIC DETERMINATION AND IR-

CHARACTERIZATION OF NICKEL COMPLEX

PREPARED FOR: ASSOCIATE PROF. DR. WOI PEI MENG

NAME SUMAYYAH BINTI LOKMAN

MATRIX NO. 22003285/1

SEMESTER 1

OCCURANCE 1

DATE OF 15th NOVEMBER 2022

EXPERIMENT
TITLE
Gravimetric determination and IR- characterization of nickel complex
OBJECTIVES
1. To understand the concept of gravimetric analysis
2. To derive the mass of nickel calculated from the mass of precipitate
METHODOLOGY

25 ml of nickel (ii) sulfate solution is pipetted into each of the two 400-ml beakers

5ml of dilute hydrochloric acid (2M) is added and the solution is diluted to 200ml with distilled
water. The solution is heated to 60-80℃.

20ml of dimethylglyoxime solution (1%) is added to the hot solution, followed by the addition
of ammonium hydroxide dropwise with stirring until precipitation occurs and the solution is
slightly basic. More dimethylglyoxime solution is added to test the completeness of
precipitation.

The precipitate is warmed for 30 minutes, cooled to room temperature and filtered through a
weighed no.4 sintered glass crucible previously dried at 110℃.

The precipitate is washed with cold water until it is free from any chloride (test with silver
nitrate solution) and is dried overnight.

The crucible is cooled in a desiccator and weighed to constant weight

From the weight of the precipitate and the knowledge of theoretical quantity of nickel in bis
(dimethylglyoximato) nickel (II), the concentration (in g𝐿−1) of nickel (II) ions in the solution is
calculated.

RESULTS AND CALCULATIONS

Weight (g) A B
Empty crucible (g) 30.2634 30.4532
Crucible + precipitate (g) 30.7243 31.0468
Weight of precipitate (g) 0.4609 0.5936
 0.4609 + 0.5936
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑝𝑟𝑒𝑐𝑖𝑝𝑖𝑡𝑎𝑡𝑒 = = 0.5273𝑔
2
Relative molecular mass of Ni(C4H7O2N2)2 = 288.922 g 𝑚𝑜𝑙 −1

0.5273
𝑚𝑜𝑙𝑒 𝑜𝑓 𝑛𝑖𝑐𝑘𝑒𝑙 (𝐼𝐼)𝑑𝑖𝑚𝑒𝑡ℎ𝑦𝑙𝑔𝑙𝑦𝑜𝑥𝑖𝑚𝑎𝑡𝑒 = = 1.825 × 10−3 𝑚𝑜𝑙
288.922
Mol ratio of nickel (II) ion to nickel (II) dimethylglyoximate = 1:1
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑁𝑖 2+ = 0.001825 × 58.69 = 0.1071𝑔
58.69
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑏𝑦 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑛𝑖𝑐𝑘𝑒𝑙 = × 100% = 20.31%
288.922
0.1071
𝑎𝑐𝑡𝑢𝑎𝑙 𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑏𝑦 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑛𝑖𝑐𝑘𝑒𝑙 = × 100% = 20.31%
0.5273
Theoretical percentage=actual percentage
0.1071
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑛𝑖𝑐𝑘𝑒𝑙 (𝐼𝐼)𝑖𝑜𝑛 = = 4.284 𝑔𝐿−1
0.025
DISCUSSION
In this experiment, the quantity of nickel (II) ions are determined. At the end of this
experiment, nickel is present as nickel dimethylglyoxime precipitate, 𝑁𝑖(𝐶4 𝐻7 𝑂2 𝑁2 )2 , which
is red in colour and insoluble in water.
The formation of red precipitate occurs in the solution when the pH buffered between the
range of 5 to 9 using ammonia. The four nitrogen atoms donate electron pairs, which causes
this reaction to happen. Buffer solution is used to prevent the pH to fall below 5.
When transferring the precipitate to sintered glass, make sure that all precipitate is free from
chloride ions which can be tested by using silver nitrate solution. If the solution turns cloudy,
it means that chloride ions are still present. Wash with cold water if there is any excess in the
beaker.
Next, IR analysis method is used where it uses infrared light to scan the test sample and
observe chemical properties. By measuring atom vibrations using IR spectroscopy, the
functional groups of molecules can be identified. 5 Usually, light atoms and stronger bonds
will vibrate with a higher stretching frequency (wavenumber).
From sample A, we can assume that:
No. Frequency (𝑐𝑚−1 ) Bonding type Functional group
1. 1789.50 C=O Conjugated acid
halide
2. 1568.47 N-O Nitro compound
3. 1422.21 O-H Carboxylic acid
4. 1364.39 O-H Alcohol
5. 1236.60 C-O Alkyl/aryl/ether
6. 1096.16 C-N amine
7. 987.42 C=C alkene
8. 879.32 C-H 1,2,4-trisubstituted
9. 811.45 C-H 1,4-disubstituted
10. 700.60 C-H Benzene derivative
11. 517.83 C-I -

SAFETY PRECAUTIONS
1. Make sure that the precipitate is free from any chloride
2. Transfer of liquids should be in as small quantity as possible
3. Make sure to pour ammonium hydroxide into the hot solution in the fume cupboard.

CONCLUSION
The weight of precipitate obtained from sample A is 0.4609g while weight of precipitate from
sample B is 0.5936g. The concept of gravimetric analysis is understood and The mass of
nickel calculated from the mass of precipitate is derived.

QUESTIONS
1.

Ni is sp2 hybridized, N is sp2 hybridized and C is sp3 hybridized

 3. The temperature of the solution must be maintained at 60-80℃ during precipitation
process because the boiling point of DMG is lower than 80℃. Therefore, if the
temperature reaches any higher, the DMG will evaporate and affect the whole
precipitation process.

REFERENCE

1. IR Spectrum Table & Chart. IR Spectrum Table. (n.d.). Retrieved December 12,
2022, from https://www.sigmaaldrich.com/MY/en/technical-documents/technical-
article/analytical-chemistry/photometry-and-reflectometry/ir-spectrum-table
2. AMRITA. (n.d.). Gravimetric Estimation of Nickel. Gravimetric estimation of nickel
(theory) : Inorganic Chemistry Virtual Lab : Chemical Sciences : Amrita Vishwa
vidyapeetham virtual lab. Retrieved December 12, 2022, from
https://vlab.amrita.edu/?sub=2&brch=193&sim=348&cnt=1