UNIVERSITY OF BAHRAIN

COLLAGE OF SCIENCE
DEPARTMENT OF CHEMSTRY

Experiment #4
Gravimetric Analysis
of a Copper salt
Fatema Saleem
E-mail: [email protected]
Aim
1. To use Gravimetric analysis to determine the percentage
of Copper by mass in a copper salt of unknown identity.
Analytical methods

Gravimetric Analysis Volumetric Analysis

A process of determining the A process of determining the
amount of an analyte by measuring amount of an analyte by measuring
its mass in an insoluble ppt the volume of a reagent
e.g. Precipitation e.g. Titration

Gravimetric analysis is potentially one of the most precise techniques of analytical

methods since weight can be measured more accurately than practically any
other fundamental property like volume of liquid and gases.
Gravimetric Analysis: Precipitation gravimetry
• Principle
A process that separates the ion from its constituent by dissolving a
known amount of an ion-containing compound in a solvent and then
precipitating it as insoluble solid.

1. Conversion to a sparingly soluble precipitate by precipitation agent

2. Filtration (Get the solid form)
3. Heating (Drying)
4. Weighing

This process can be used to calculate the amount of an ion in the original solution.
Precipitation gravimetry

1. Preparation of a solution containing a known weight of the

analyte’s sample (Analyte and solvent).
2. Precipitate the analyte using excess of precipitation agent
3. Separation of the desired constituent by filtration and drying.
4. Weighing the isolated constituent.
5. Calculating the constituent’s amount in the original sample
using the isolated analyte’s weight as a starting point.
Precipitation gravimetry

This analysis has to meet few requirements in order to be useful

1. The ion of interest must fully precipitate from its solution.

2. The precipitate must be a pure compound.
3. It must be possible to filter the precipitate.
In this Experiment..
The aim is to get the mass of a copper ion in a copper salt compound
CuSO4 is a soluble salt, in order to get the mass of the Copper in it, it should be insoluble

According to the following ionic equation

CuSO4(aq) + Zn(s) → Cu(s) + ZnSO4(aq)
Cu2+(aq) +SO42-(aq) + Zn(s) → Cu(s) + Zn2+(aq) + SO42-(aq)
Cu2+(aq) + Zn(s) → Cu(s) + Zn2+(aq)

• Since Zn is more reactive than Cu; displacement reaction occurs, and Copper ions
may be quantitatively precipitated from a solution by the addition of Zinc metal
Oxidation - Reduction reaction

2-0= +2 (Oxidation)

Cu2+(aq) + Zn(s) → Cu(s) + Zn2+ (aq)

0-2= -2 (Reduction)

Cu2+(aq) is blue in solution, but Zn2+(aq) is colorless in solution

• As Cu2+ is reduced to Cu(s), and Zn(s) is oxidized to Zn2+, the solution containing the
Copper salt will slowly change from blue to colorless.
• When the reaction is finished, the solid elemental Copper will be at the bottom of the
reaction beaker and can be recovered using gravity filtering.
Materials & Apparatus

Glass Ware & Apparatus Chemical Used

1. Conical Flask 1. Unknown Copper Salt Sample
2. Beaker 2. Zinc Powder
3. Funnel 3. 2M HCl
4. Watch glass 4. Distilled Water
5. Filter paper
6. Balance
7. Oven
8. Measuring Cylinder
9. Spatula
Procedure
STEP1: Preparation of a solution containing a known weight of the analyte’s sample

1. Weigh out 0.7xxx g

2. Measure 20mL of distilled water, add to the Copper salt
of Copper salt sample
and stir until all the powder is fully dissolved
Procedure
STEP2: Precipitate the analyte using excess of precipitation agent

3. Weigh out 0.3xxxg 4. Add the Zinc to the solution and

of Zinc powder Stir the mixture to allow the reaction

Why Zinc powder is added to the Copper salt?

It is a precipitation agent, that will precipitate the Copper metal by displacement reaction
Procedure
STEP2: Precipitate the analyte using excess of precipitation agent

Why 2M of HCl is added?

To react with the excess of Zinc (Get rid of the extra Zn
solid) because Zn will interfere the solid of Copper.

How ?
H2 gas bubbles

When unreacted Zinc metal is reacted with HCl, it will

produce H2 as gas bubbles and a soluble salt which is ZnCl2
Zn(s) + 2HCl(aq) → ZnCl2 (aq) + H2 (g)
Since ZnCl2 is a soluble salt, it will be totally dissolved in the
5. Add drops of 2M HCl solution forming an aqueous salt solution, so it is no longer
until the solution becomes clear in the solid form, as a result, Copper metal now is purified
form the solid unreacted Zinc.
and no bubbles is evolved
Procedure
STEP3: Separation of the desired constituent by filtration.

6. Weigh out a 7. Set up the filtration 8. Once filtration is done, place

folded Filter paper apparatus and start filtration filter paper above a watch glass

Why filtration process has been done?

To get the Copper ion precipitate as solid only without the solution
Procedure
STEP4: Drying and Weighing the isolated constituent

9. Place the filter paper 10. Weigh out the dry

in the oven at 100°C sample and filter paper
Why drying process has been done?
To get rid of any water molecules in the precipitate.
Data & results example

Trial 1 Trial 2 Trial 3

1. Mass of sample (g) 0.7029 0.7120 0.7040
2. Mass of filter paper (g) 1.058 1.112 1.069
3. Mass of filter paper and copper ppt (g) 1.357 1.397 1.290
Calculation example
Trial 1 Trial 2 Trial 3
4. Mass of copper precipitate (g)
1.357-1.058 = 0.299 1.397-1.112= 0.285 1.290-1.069= 0.282
Ans 3 – Ans 2
5. Percent of Copper in original sample (%)
0.299 0.285 0.282
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐶𝑢 (𝐴𝑛𝑠4) × 100 = 42.54% × 100 = 40.03% × 100 = 40.05
× 100 0.7028 0.7120 0.7040
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑆𝑎𝑚𝑝𝑙𝑒 (𝐴𝑛𝑠1)

6. Average percent of Cu in original sample

42.54% + 40.03% + 40.05%
𝑇1 + 𝑇2 + 𝑇3 = 40.86%
3 3
Accuracy and Precision
Accuracy Precision
Describes how much the results are Describes how much the results are
close to the actual or true value. close to each other regardless the
actual or true value.
e.g. Percentage error e.g. Standard Deviation
Standard Deviation (s)
Type of measurements that gives a description of how much the data is precise

WHERE:
X = value of the data observed
𝑥=
ҧ The mean value of the data set
n= number of data points in the data set

• Small Standard deviation value: Data is close to the mean value.

• Large Standard deviation value : Data is more spread out.
Standard Deviation Calculation
7. Standard deviation
Step 1: Calculate the mean 𝑥ҧ (add all samples divided by the number of samples).
Step 2: Subtract each data from mean.
Step 3: Square each subtracted value (step2).
Step 4: Sum the squared deviations.
Step 5: Divide that sum from step 4 by (N-1).
Step 6: Take the square root of the number in step 6.
Standard Deviation Calculation
7. Standard deviation
Percentage of copper
𝑥ҧ |𝑥 − 𝑥|ҧ |𝑥 − 𝑥|ҧ 2
ion in original sample
42.54% 42.54% + 40.03% + 40.05%
42.54 − 40.86 = 1.68 1.682 = 2.8224
3
40.03% = 40.86% 40.03 − 40.86 = 0.83 0.832 = 0.6889

40.05% 40.05 − 40.86 = 0.81 0.812 = 0.6561

∑|𝑥 − 𝑥|ҧ 2 2.8224 + 0.6889 + 0.6561

𝑠= , where n is number of samples 𝑠= = 1.44
𝑛−1 3−1
Relative Standard Deviation Calculation
Measures the degree of standard deviation, whether it is small or large
High value of (RSD) = Poor results
Low value of (RSD) = Good results

8. Relative Standard deviation (S / mean)

1.44
𝑅𝑆𝐷 = = 0.035
40.86

9. Reported percentage of copper ion (mean ± S)

40.86 ± 1.44 %
Assignment (Must be included in the report)
An experiment has been done to get the percentage of the mass of an
ion in a salt, and the results were 35.25%, 35.16% and 35.29%. Calculate
the Standard deviation (s) and Relative Standard deviation (RSD) and
Report the value.