Experiment 6

Colorimetric Estimation of Cu in brass

Dr. Suni Vasudevan

Dr. Mausumi Chattopadhyaya
Assistant Professors
Department of Chemistry
mausumi@nitc.ac.in; suniv@nitc.ac.in
+919433710271; 9037582625
 Briefing about brass…..
 Brass is an alloy of Cu and Zn.

 The relatively low melting point of brass and its flow

characteristics make it a relatively easy material to cast.

 By varying the % of Cu and Zn, the properties of brass can be

changed, allowing “HARD” and “SOFT” brasses.

 Brass will corrode in the presence of moisture, chloride, acetates,

ammonia and certain acids.

2
 Colorimetric Estimation of Cu in brass
Principle of Colorimeter: A colorimeter is based on the photometric
technique. When a beam of electromagnetic radiation of intensity I0
passes through a solution, it is observed that a part of the incident
light is reflected (Ir), a part is absorbed (Ia) and the rest of the light is
transmitted (It). So it can be represented as:

I0=Ir+Ia+It

I0
It
Ia

Ir

Schematic representation of the principle statement

3
 Instrumentation

Absorption laws
Lambert’s Law : (Absorbance ∝ Path length)
Beer’s Law : (Absorbance ∝ Concentration)
 Beer–Lambert law: Combination of both the laws (A ∝ cx)
4
 Fundamental Laws of photometry
Lambert’s Law: When a beam of monochromatic radiation is
passed thru’ a transparent medium, the rate of decrease of
intensity of radiation with the thickness of absorbing medium is
directly proportional to the intensity of the incident radiation.
dI
- µI I is the intensity of the radiation
dx and x=thickness of the medium
Beer’s Law: When a beam of monochromatic radiation passed
thru’ a transparent medium, the rate of decrease of intensity of
radiation with the thickness of absorbing medium is directly
proportional to the concentration of the solution.
dI
- µc c is the concentration of the solution
dx
I0
Beer-Lambert Law: A = log = e cx ε is molar absorptivity
It
5
 Colorimetric Estimation of Cu in brass

In order to estimate the amount of copper, the brass sample is weighed and treated with 1:1
nitric acid and boiled gently for 10 minutes until the evolution of brown gas NO2 ceases.
Excess HNO3 is removed by boiling with urea and the blue color is developed by
mixing with ammonia, by the formation of cuprammonium complex. The absorbance of
the blue solution is proportional to the concentration of copper in it.

6
 Colorimetric Estimation of Cu in brass
Procedure:
 Weight out accurately 0.12 g of brass and transfer it into a 100 ml conical
flask.

 Add 10 ml of 1:1 nitric acid and boil gently for 10 minutes until the
evolution of brown gas ceases completely.

 To the above solution add 10 ml of water, 1gm (one spatula) of urea and
boil for few minutes.

 Cool the resultant solution to room temperature, transfer quantitatively into

a 50 ml standard flask and make up to the mark.

 Pipette out 5 ml of this solution into a 25 ml standard flask containing 5 ml

of 1:1 ammonia solution, mix it well and make up to 25 ml.

 Measure the absorbance of this solution using a 610 nm filter. 7

 Colorimetric Estimation of Cu in brass
Procedure (Contd.):
 From the given stock solution (CuSO4 solution), pipette out 1, 2, 3, 4 and
5ml into 5 different 25ml standard flasks and add 5ml of 1:1 NH3 solution
in each of them and make up to the mark. Mix well.

 Also prepare a blank solution without CuSO4.

 Measure the absorbance of each of these solutions using the same 610 nm
filter.

 Tabulate the readings and draw a calibration graph with the above readings
(X-axis=> Concentration in mg; Y-axis=> Absorbance)

 Determine the Cu content in unknown brass sample from the graph.

8
Colorimetric Estimation of Cu in brass

Calculations for the calibration curve:

Concentration of the given stock solution = 19.65 mg/cc

249.68 mg of CuSO4.5H2O contains 63.55 mg of Cu

i.e., 1 mg of CuSO4.5H2O contains (63.55/249.68) mg of Cu

So 19.65 mg of CuSO4.5H2O=> (63.55/249.68)x 19.65 = 5 mg Cu

Concentration of Cu in V ml of stock solution (col. 3 in the data

tables in slides 10 to 12) = V x 5 mg

9
 Colorimetric Estimation of Cu in brass
Observation Table:

Weight of brass sample taken: 0.13 g

TABLE 1: With “UNKNOWN (A)”

Sl no. Volume of stock solution (in ml) Concentration of Cu (mg) Absorbance (A)
1 1 5 0.1
2 2 10 0.2
3 3 15 0.3
4 4 20 0.4
5 5 25 0.5
6 UNKNOWN (A) ? 0.19

10
 Colorimetric Estimation of Cu in brass
Observation Table:

Weight of brass sample taken: 0.12 g

TABLE 2: With “UNKNOWN (B)”

Sl no. Volume of stock solution (in ml) Concentration of Cu (mg) Absorbance (A)
1 1 5 0.1
2 2 10 0.2
3 3 15 0.3
4 4 20 0.4
5 5 25 0.5
6 UNKNOWN (B) ? 0.18

11
 Colorimetric Estimation of Cu in brass
Observation Table:

Weight of brass sample taken: 0.11 g

TABLE 3: With “UNKNOWN (C)”

Sl no. Volume of stock solution (in ml) Concentration of Cu (mg) Absorbance (A)
1 1 5 0.1
2 2 10 0.2
3 3 15 0.3
4 4 20 0.4
5 5 25 0.5
6 UNKNOWN (C) ? 0.17

12
Colorimetric Estimation of Cu in brass
Data plotting:

13
 Colorimetric Estimation of Cu in brass
Calculations for the unknown concentration.:

Concentration of Cu (in 5ml) = ……….mg (calculate it from the

plot)

Concentration of Cu (in 50ml) = ………..mg = X

% of Cu = (X mg/Weight of brass in mg) x 100

% of Cu = …………..%

14
 Note as Important
Q1. What is the role of urea in the experiment?

Ans1. Here, urea is used to destroy the excess acid and to expel the oxides of
Nitrogen, which can interfere with the determination.

Q2. What is the role of NH3 in the experiment?

Ans2. We are adding 5 ml of NH3 with the solutions. The cupric ion, Cu2+
forms a deep blue “cuprammonium complex” as follows:

Cu + 4NH3 = éëCu ( NH3 ) 4 ùû ( deepbluecolor )

2+ 2+

Q3. Why we are using 610 nm filter?

Ans3. The absorbance of the solutions is measured at 610 nm since the

complex shows maximum absorbance at this wavelength.

15
16