Procedure of Analytical Chemistry Experiment

EXPERIMENT 4
GRAVIMETRY

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GOALS:

1. Students are able to determine Ni2+ content as Dimethyl Glyoxime (DMG) complex
with gravimetry analysis method.
2. Students are able to determine the mass of Pb(CH3CO2)2.3H2O with gravimetry
analysis method.

BASIC THEORY:

Gravimetry is one of the quantitative analysis of a compound that has been known by
measuring the weight of components (compounds) in a pure state after a separation process.
Separation process of the component is carried out by separating the component from other
undesirable components and also separating the component from the solvent that used in the
experiment. There are several conditions that must be met in gravimetric analysis, which are :

1. Solubility of the precipitate is very small.

2. The precipitate must be in the pure state.
3. The precipitate must be easily filtered and washed.
4. The precipitate that will be weighed should have a definite formula.

A. DETERMINING Ni CONTENT AS DMG COMPLEX

METHOD :

Nickel is precipitated from its hot and acidic solution with the addition of a solution
called DMG (Dimethyl Glyoxime), then followed by addition of a little excess NH4OH

Ni+2 + 2H DMG -------→ Ni ( DMG ) 2 + 2 H+

The precipitate is filtered off, washed with cold water, and then dried. The precipitate
is weighted as Ni(DMG)2 with factors : Ni/ Ni(DMG)2 = 0,2032

TOOLS AND MATERIALS:

1. Beaker Glass 400 mL

2. Sintecruss
3. Dessicator
4. Oven and water bath
5. Measuring pipette 10 mL
6. NiSO4.7H2O
7. Diluted HCl (1:1)

Analytical Chemistry Laboratory Departement of Chemical Engineering FTIRS – ITS 1

Procedure of Analytical Chemistry Experiment

8. DMG solution 1% in alcohol

9. Ammonia 1 N solution
10. AgNO3 solution

EXPERIMENT PROCEDURE:

1. Ask for task solution in beaker glass 400 mL to the assistant with stirring rod.
2. Add 5 mL of concentrated HCl (1:1) dan dilute the solution up to 200 mL.
3. Heat the solution to 70 – 80 °C, add excess DMG (30 – 35 mL), and then immediately
followed with diluted ammoniac solution drop by drop directly to the solution, while
keep stirring it, until it formed red precipitate. After that, add excess ammoniac solution
until the solution smells of NH3.
4. Put the beaker glass in the water bath for 20 – 30 minutes and try with the reagent
solution, whether the precipitation is complete or not.
5. Leave the precipitate for 1 hour.
6. Filter the precipitate through a sintercruss thas has been preheated at 110 – 120 °C and
weighed to a fixed weight, after being cooled in a dessicator.
7. Wash the precipitate with cold water until it is chloride free, and dry the precipitate at
110 – 120 °C for 45 – 60 minutes.
8. Put it in the dessicator to cool it and then weight it carefully.
9. Repeat the drying step and weight it until the weight remains.

QUESTIONS :

1. What is the formula of Ni dimethyl glyoxime?

2. What is shelat complex? Give another example of shelat complex!
3. Why the addition of reagents should not be too excessive?
4. Why should it be heated in water bath?
5. At what pH does Ni dimethyl glyoxime settle?

B. DETERMINING THE WEIGHT OF PB ACETATE

TOOLS AND MATERIALS:

1. Filter cup
2. Volumetric flask 100 mL
3. Volumetric pipette 25 mL
4. Dessicator
5. Water jet pump
6. Oven
7. Filter paper
8. Task solution Pb(CH3CO2)2.3H2O
9. K2CrO4 4% solution
10. Asbestos dust

Analytical Chemistry Laboratory Departement of Chemical Engineering FTIRS – ITS 2

Procedure of Analytical Chemistry Experiment

EXPERIMENT PROCEDURE :

Making of Filter Cup :

1. Ask for asbestos dust to the assistant, mix it with water, then stir until it becomes
powder.
2. Take a filter cup, put asbestos powder into the filter cup so that the surface of the
porcelain cup covers asbestos, then the water is sucked with water jet pump.
3. Heat it in the oven for 1 hour at 110 – 120 °C.
4. Dry the filter cup in the dessicator until it cools.
5. After it gets cold, do the weighing until the weight is constant.
6. Record the weight results.

Precipitation Analysis :

1. Ask for task solution to the assistant using volumetric flask 100 mL, dilute it up to 100
mL and shake it until homogeneous.
2. Take 25 mL of the task solution using volumetric pipette, put it in the Erlenmeyer.
Then, add K2CrO4 solution so that the solution will react with K2CrO4. Then heat it until
the main solution becomes clear and its precipitate becomes larger and accumulates.
3. Separate the precipitate from the main solution with filter paper and wash the precipitate
with aquadest or separate the precipitate from water using the crush goach above and
use a water jet pump for faster separation.
4. Put the filter cup that contain precipitates in the oven for 1 hour at 110 – 120 °C.
After that dry it in the dessicator until it cools.
5. Weight until the weight is constant.
6. Calculate the weight of precipitates that occur and calculate the weight of Pb Acetate.

Analytical Chemistry Laboratory Departement of Chemical Engineering FTIRS – ITS 3

Procedure of Analytical Chemistry Experiment

OBSERVATION

A. 1. Gravimetry Ni2+ Content Experiment Results :

No. Parameter Observation

1. Task Solution + HCl
2. Task Solution + DMG
3. ……….

Number of Sintercruss mass Sintercruss + Precipitate mass

Experiment (gram) precipitate mass (gram)
(gram)
1.

2.

3.

Average

2. Reaction that occurs :

3. Ni2+ content calculation :

Analytical Chemistry Laboratory Departement of Chemical Engineering FTIRS – ITS 4

Procedure of Analytical Chemistry Experiment

4. Discussion:

• Physical change
• Chemical change
• Hypothesis
• Comparison with literature

Analytical Chemistry Laboratory Departement of Chemical Engineering FTIRS – ITS 5

Procedure of Analytical Chemistry Experiment

B. 1. Gravimetry Pb(CH3CO2)2.3H2O Experiment Results :

No. Parameter Observation

1. Task solution + K2CrO4 4%
2. ……….

Number of Sintercruss mass Sintercruss + Precipitate mass

Experiment (gram) precipitate mass (gram)
(gram)
1.

2.

3.

Average

2. Reaction that occurs :

3. Mass of Pb(CH3CO2)2.3H2O calculation :

4. Discussion:

• Physical change
• Chemical change
• Hypothesis
• Comparison with literature

Analytical Chemistry Laboratory Departement of Chemical Engineering FTIRS – ITS 6

Procedure of Analytical Chemistry Experiment

INTERIM REPORT

ANALYTICAL AND ORGANIC CHEMISTRY EXPERIMENT

CHEMICAL ENGINEERING DEPARTMENT FTIRS - ITS

EXPERIMENT TITLE :
CLASS / DAY :
GROUP :
NAME / NRP : 1. NRP.
2. NRP.
3. NRP.

Number of Sintercruss mass Sintercruss + Precipitate mass

Experiment (gram) precipitate mass (gram)
(gram)
1.

2.

3.

Average

Knowing,

(……………………………..)

Laboratory Assistant

Analytical Chemistry Laboratory Departement of Chemical Engineering FTIRS – ITS 7