UNIVERSITY OF GUYANA

FACULTY OF NATURAL SCIENCES

DEPARTMENT OF CHEMISTRY

CHM 3202- Analytical Chemistry I

LECTURER: Dr. Dawn Fox

Lab # 1
Gravimetric estimation of Iron (III) oxide
2014/02/27

Parbatie Ramotar
13/0705/2232
Group Members:
Claude Fraser
Date submitted: 24th March, 2014
Abstract

This lab is based on the estimation of iron (III) oxide from 25 ml iron alum, by the gravimetric

analysis. The experiment proceeds as follows:

2ml of concentrated nitric acid was added to 25ml iron alum solution. The solution was brought

to a boil, and was diluted to 150ml of solution. The solution was then heated to boiling and 5M

NH4OH solution was added in excess. This solution was boiled for 1-2 minutes and the

precipitate was allowed to settle. The supernatant liquid was decanted through the filter paper,

and washing of the precipitate was repeated three more times, with 100ml 1% ammonium nitrate

solution for each wash. After washing, the precipitate in the filter paper was transferred to the

silica crucible which was placed in the oven and heated for 10 mins. The crucible was heated

gently to dry the filter paper, the charred then finally heated to redness for 30 mins. The crucible

was allowed to cool in the desiccator for the mass to be obtained. The final masses obtained for

the sample were 1.060g, 1.057g and 1.057g.

Introduction

By gravimetric analysis, iron (III) oxide, also known as rust, was estimated from 25 ml iron alum

solution. Iron (III) oxide has molecular formula Fe3O4, molar mass of 159.60g/mol, and it is

mined as hematite. The iron in this state has a +3 oxidation state. Naturally, iron (III) oxide is

produce by the corrosion of iron. Here, the iron combines with both oxygen and water to form

hydrated iron oxide.

Theory

To find mean:

∑ xi
i=1
x=
n

Where:

Xi = each individual measurement

n = total # of measurements

To find standard deviation:

s=
√ ∑ ( x i−x )2
n−1

Where:

Xi = each individual measurement

n = total # of measurements

To calculate variance:

Square standard deviation (S2).

Procedure

Refer to lab handout

Results

Type of Statistical Thursday Friday Results

Treatment

Questionable Value 0.891

Total 16.278 9.293

Number of Observations 15 12

Mean 1.0852 0.7744166

7

Standard dev. 0.0356494 0.1036291

8 1

95% Confidence Interval 0.0197439 0.0641679

9 9

[X1-X2] 0.31078333
3

tsp((/N1+N2)/(N1*N2)) 0.0559726

[X1-X2]> tsp((/N1+N2)/(N1*N2)) TRUE

Fc 8.45000640
4
Ft 1
Fc>Ft TRUE

Qc 0.11111111
1
96% Qt 0.48
Qc > Qt FALSE
Table 1 Showing Results
Discussion

Data set 1 refers to Thursday lab group

Data set 2 refers to Friday lab group

Data set 1 has 15 measurements, which give an average (mean) of 1.0852. Data set 2 on the other

hand had 12 measurements, which give an average (mean) of 0.7744. The standard deviation of

dataset 1 was 0.0356, while for dataset 2, it was 0.1036. Standard deviation is used to show how

much difference exists from the mean.

A confidence interval is a range of values about the mean within which true value can be found.

Dataset 1 had CI of 0.0197, and dataset 2, 0.0642. After a comparison of the two means, the null

hypothesis was rejected, since

[X1-X2]> tsp((/N1+N2)/(N1*N2))

This means there was a significant difference between the two means.

The precisions of the results were also calculated, and Fc was found to be greater than Ft . This

implies that the null hypothesis is rejected, and there is a significant difference between the two

precisions.

From dataset 2, an outlier was identified. The value was questionable; hence the Q test was used

to determine if it was an outlier. Qc was found to be greater than Qt , which implies that the null

hypothesis is rejected and there is a significant difference between the values. Due to this, the

questionable value is now an outlier and can be discarded.

Some of the possible sources of error for this lab include:

i) Some of the precipitate remained on the glass rod after stirring, and some also

remained in the beaker after decanting and washing.

ii) There was an incomplete washing of precipitate, since some precipitate was

accidentally poured onto the filter paper before time.

An improvement to the lab is to filter using the bruchner funnel and suction pump. This would

decrease the filtration time.

Conclusion

To conclude, 1.057g of Iron (III) oxide was produced by group 4 on Thursday.

References

Skoog et al. (2004), Fundamentals of Analytical Chemistry, 8th Edition, Brooks Cole Thomas

Learning): USA
Appendix 1

Type of Statistical Thursday Friday Results

Treatment
1.083 0.603
1.082 0.604
1.078 0.61
1.05 0.805
1.05 0.806
1.05 0.806
1.086 0.828
1.093 0.828
1.089 0.828
1.06 0.858
1.057 0.858
1.057 0.859
1.148
1.148
1.147

Questionable Value 0.891

Total 16.278 9.293

Number of Observations 15 12

Mean 1.0852 0.774416667

Standard dev. 0.035649484 0.10362911

95% Confidence Interval 0.01974399 0.064167991

[X1-X2] 0.310783333

sp 0.073735017

t 1.96
Sqrt((N1+N2)/(N1*N2)) 0.387298335

tsp((/N1+N2)/(N1*N2)) 0.0559726

[X1-X2]> tsp((/N1+N2)/(N1*N2)) TRUE

Fc 8.450006404

Ft 1

Fc>Ft TRUE

Qc 0.111111111

96% Qt 0.48

Qc > Qt FALSE