Analysis of a Nickel Coordination Compound  

A Laboratory Report for CHEM 2140 

Performed by: Alexandria Parks 

Date Performed: March 21, 2019, March 28, 2019, and April 4, 2019 

Date Submitted: April 25, 2019 

 
 
 
Abstract 
A nickel coordination compound was generated using nickel(II) chloride hexahydrate and 

ethylenediamine and then analyzed to determine its chemical formula. A standard curve was created and 

utilized to derive the concentration of N i2+ within the compound, the mass percent of nickel was then 

determined to be 16.04%. The amount of chlorine within the coordination compound was found via 

gravimetric analysis, resulting in a mass percent of 17.53%. To test for the mass of ethylenediamine 

within the compound volumetric analysis was conducted titrating the compound with HCl, resulting in a 

mass percent of 47.14%. These mass percents were them combined in order to determine the amount of 

water within the compound, its mass percent was found to be 19.28%. Combining these percentages the 

formula for the generated compound was found to be N i(en)3 Cl2 · 4 H 2 O or 

tris(ethylenediamine)nickel(II)chloride hydrate.

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Introduction 
 
A coordination compound is a compound made up of at least one complex ion [1]. Complex ions 

have metal ions in their center with other molecules or ions surrounding them connected by coordinate 

covalent bonds. These surrounding ions are known as ligands which function as Lewis bases since they 

have lone pairs of electrons in their outer energy shell, a prime example being chlorine [2]. In this 

experiment, the ion nickel(II) chloride hexahydrate, N iCl2 · 6 H 2 O , was combined with the ligand 

ethylenediamine, N H 2 CH 2 CH 2 N H 2 , to form the coordinate compound shown in equation 1.  

N iCl2 · 6 H 2 O (s) + x N H 2 CH 2 CH 2 N H 2 (aq) → N ix ( N H 2 CH 2 CH 2 N H 2 )y Clz · aH 2 O (s) (1) 

 
The variables in the equation can be determined through gravimetric, volumetric and 

spectrophotometric analysis. Using gravimetric analysis the chloride within the compound will be 

dissolved as shown in equation 2 and precipitated as silver chloride allowing the amount of the ion 

present to be determined. 

N ix (en)y Clz · aH 2 O (s) + 2y H + (aq) → x N i2+ (aq) + z Cl− (aq) + a H 2 O (l) (2) 

H 2 N CH 2 CH 2 N H 2 + 2 H + → + H 3 N CH 2 CH 2 N H 3 + (3)  

Through a series of titrations, the amount of ethylenediamine in the compound can be determined 

using stoichiometry in combination with the reaction shown in equation 3. In order to deduce the amount 

of nickel(II) within the compound, a standard curve can be made and compared with a series of 

spectrophotometric analyses at a certain wavelength. Using Beer’s Law, shown in equation 3, where ​A​ is 

the absorbance and​ C i​ s the molar concentration the two factors can be compared. By generating a 

standard curve of ​A​ versus ​c​ the slope of the line can be used to find the concentration of unknown 

compounds [3]. Through these methods, the chemical formula for the generated nickel coordination 

compound will be found.  

A = εbc (4) 

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Experimental  

A quantity of 5 grams of nickel (II) chloride hexahydrate was measured and transferred into a 150 

mL beaker and dissolved in 10 mL of deionized water. The solid was dissolved completely and cooled in 

an ice bath along with a beaker containing 50 mL of ethanol. In a fume hood, 10 mL of ethylenediamine 

was added to the nickel compound followed by the addition of 25 mL of the cooled ethanol while 

continuously stirring. The mixture was cooled until it turned into a bright violet and became a slushy 

consistency. Using a Büchner funnel, filtration flask, a crucible, and vacuum, the mixture was filtrated 

occasionally using a stirring rod to break up large clumps and ensure all of the liquid was drawn off the 

precipitate. Cold ethanol was used to ensure all of the solid was removed from the beaker into the crucible 

and to rinse the solid, multiple times. The precipitate was then transferred from the crucible to a clean 

labeled vial that had been previously weighed. After drying for a week the vial containing the solid was 

weighed, it was later determined that the nickel complex had a percent yield of 84.45.%. 

A wash solution of nitric acid was created by mixing 4 mL of 6 M nitric acid to 300 mL of water. 

A sample of 0.5 g of the generated coordinate compound was transferred into a 150 mL Erlenmeyer flask 

and dissolved in 20 mL of 6 M nitric acid, turning the solution from purple to a blue or green shade. Then 

20 mL of 0.250 M silver nitrate was added to the solution precipitating silver chloride. A crucible and 

filter were then weighed and used in combination with a Büchner funnel, filtration flask, and vacuum to 

collect the solid within the solution. Several small portions of nitric acid were used to rinse the beaker to 

ensure that all of the solid had been transferred. To test that all of the chloride had been reacted a drop of 

silver nitrate was added to the clear filtrate resulting in no further precipitation meaning all of the ions had 

reacted. The solid was then rinsed with three series of 5 mL of the nitric acid wash solution through the 

discussed filtration apparatus. To begin drying the precipitate was rinsed with two 5 mL portions of 

acetone and pulled through the filtration set up for about four minutes. During the rinses and filtration, the 

crucible containing the solid was loosely covered with a paper towel to protect the white solid from 

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reacting with any light. The compound was then allowed to dry for a week and then was weighed in the 

preweighed crucible.  

A sample of 0.514 grams of the nickel compound was dissolved in 10 mL of water and 8 drops of 

Bromocresol green indicator were added to the solution. The solution was then titrated using a burette 

filled with 0.5112 M HCl to a yellow endpoint. The same steps were used to analyze two more trials of 

the compound weighing 0.619 and 0.504 grams. The solutions all turned a shade of yellow that was 

similar to a light green color and was ensured to reach the endpoint by adding an extra drop of the titrant 

and observing that the color remained constant.  

In order to generate a standard curve to determine the amount of nickel in the compound, about 2 

mL of 0.1840 M N i2+ was added to a 10 mL volumetric flask and combined with 1 M nitric acid to the 10 

mL mark. The absorbance of this solution was found three times using spectrometry, this was then 

combined with class data to form a standard curve. To analyze the generated compound a mass of 0.208 

grams of the compound was diluted in a 10 mL flask and analyzed using a spectrovis plus and the logger 

pro computer program. The cuvette was rinsed carefully between each analyzation with 1.5 mL of 1 M 

nitric acid as well as rinsing off the weighing boat with nitric acid when transferring the compound into 

the flask. The same procedure was used to analyze samples of 0.300 and 0.405 grams and the absorbance 

of each trial was recorded at 725 nm.  

Results and Discussion 

 

4
  
Figure 1: The absorbance spectrum for a 0.300-gram sample of the generated compound. 
 
The absorbance spectrum was found using spectrophotometry by dissolving a 0.300-gram sample 

of the generated coordination compound in nitric acid. Similar spectrums were obtained for the other two 

quantities of the compound and the absorption at 725 nm was recorded. The absorbance at this 

wavelength can be used in combination with the equation of the line of best fit of a standard curve in 

order to derive the concentration of N i2+ within the compound.  

 
2+
Figure 2: Standard curve relating the absorbance of a known stock solution of N i at 725 nm to its 
concentration. 

5
 
Using the equation of the line of best fit and the absorbance found at 725 nm the concentration of 

the nickel ion can be solved for. The found concentration can then be used to find the mass of the nickel 

in the coordination compound. Sample calculations can be found in the appendix. 

  Mass Percent (%)  Standard Deviation  

Nickel  16.04  6.37 

Chlorine  17.53  5.09 

Ethylenediamine  47.14  10.44 

Table 1: Mass percent of elements within the generated coordination compound derived from class data as 

well as the standard deviation among those values. 

The mass percent of nickel in the compound was found to be 16.04% with a standard deviation of 

6.37. Meaning that the values for the percent of nickel throughout the class were around the same amount 

with only a little variation. The mass percent reveals that nickel is the least abundant element in the 

compound. The mass percent of chlorine was determined to be 17.53% with a standard deviation of 5.09. 

The values among the class data for the amount of chlorine within the compound were the most consistent 

with the lowest standard deviation revealing less variation in the values. Within the compound, 

ethylenediamine was the most abundant with a mass percent of 47.14% and a standard deviation of 10.44. 

The large value for the standard deviation reveals that among all of the elements in the compound 

ethylenediamine showed the greatest variation in the individual values. These values can be used to 

determine the empirical formula of the generated compound.  

Using the determined mass percentages the formula of the nickel coordination compound was 

determined to be N i(en)3 Cl2 · 4 H 2 O . The formed coordination compound is 

tris(ethylenediamine)nickel(II)chloride hydrate. This was determined by finding the moles of each 

element within the compound and dividing by the smallest mole to ensure the smallest ratio of the 

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elements was obtained. It must be noted that the mole ratio of each element within the compound was 

rounded to the nearest whole number with the exception of nickel since it had the smallest number of 

moles present. The mole ratios that are not whole numbers indicate that there may have been errors within 

the procedure. The loss of chlorine may be explained by errors that occurred during the filtration of the 

solid. If not all of the chloride had reacted with silver during the filtration and the experimenter had not 

noticed the precipitate would have been lighter making the chlorine present in the compound appear 

lower. This also could have occurred when rinsing the precipitate with nitric acid, if the filter lifted during 

this process and some of the solid were lost the amount of chlorine found would decrease. Regarding 

ethylenediamine, this value could have been low due to errors in titration. If the experimenter did not 

reach the endpoint and stopped titration prematurely, the moles of ethylenediamine would be lower 

causing the compound to appear less abundant in the compound. The amount of H 2 O in the compound 

was found by using the rest of the mass of the compound and determining the number of moles of water 

present. Once this was found it was divided by the moles of nickel and rounded up to four. 

Summary and Conclusions  

An unknown nickel coordination compound was generated and analyzed using gravimetric, 

volumetric, and spectrophotometric analysis. The mass percents of each element within the compound 

were then determined through stoichiometric calculations. Using these percentages the equation of the 

compound was derived and found to be N i(en)3 Cl2 · 4 H 2 O or tris(ethylenediamine)nickel(II)chloride 

hydrate. The mole ratio for the provided equation had to be rounded to the nearest whole number 

revealing possible error within the experimental procedure. 

References 
[1] Gilbert, Kirss, Foster, Bretz. ​Chemistry an Atoms-Focused approach​ 2nd ed.; W.W. Norton: New 
York, 2018 

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[2] What is a Complex Ion?, Chemistry LibreTexts, 
https://chem.libretexts.org/Bookshelves/Inorganic_Chemistry/Supplemental_Modules_(Inorganic_Chemi
stry)/Coordination_Chemistry/Structure_and_Nomenclature_of_Coordination_Compounds/What_is_a_C
omplex_Ion%3F (Accessed Apr 14, 2019) 
[3]​Chemistry IV Laboratory Manual.​ Stockton University Chemistry Program, 2019.