MODULE 5.
GRAVIMETRIC ANALYSIS METHOD
5.1 Introduction
Gravimetric is the oldest and the simplest analytical technique to quantitavely measure the
amount of substance than any other chemical analysis. Gravimetric analysis is a quantitave
analysis based on constant weight of substances. In this analysis, substances must be correctly
separated from the sample matrix that could interfere the weighing process. The main part of
gravimetric analysis is to convert the substance for analysis to the other stable form, e.g., solid
precipitate as an example. Thus, this stable substance can be weighed or determined directly
by measuring its weigh or converting its chemical reaction stoichiometrically.
In the conversion process by means of calculation, the weigh of substance is calculated from the
chemical formula as well as from the molecular weight of its atoms. For example from
gravimetric analysis of substance A that based on the reaction:
xA(aq) + yB(aq) AxBy (s)
Then, complete precipitation of substance A will be reached if A is the limiting reagent in the
reaction. This means that to make all substance A is converted to precipitate, then it must have
an excess of substance B, thus the value of K will be higher than Ksp of AxBy salt. The formed
AxBy substance is then filtered and purified from all the impurities. Then it is weighed to
determine the constant weight of AxBy precipitate. Stoichiometrically, the weight of substance
A can be determined as follow:
weight of substance A (gram) = weight of AxBy (x.Ar atom A)/(Mr molecule AxBy)
When preparing substance sample using known weight of the prepared substance A, then
recovery factor (RF) can be determined using this equation:
RF (%) = (weight A (gram) from analysis / weight A preparation) x 100%
This RF value is used to calculate the real weight of substance in the sample. The real
(empirical) weight is the weight from analysis divided by RF. Some requirements need to be
fullfilled to get accurate gravimetric analysis:
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1. Separation process of substance should be done accurately so that excess substance that
can not be precipitated can be neglected due to its small amount (negligible).
2. Substance that is required for constant weight determination must be as pure as possible,
thus need to be done in appropriate purification process or recrystallisation (when
necessary).
3. The determined substance must have confirmed uniform formation of crystal or
precipitate. Otherwise, it indicates impurities dissolved in the substance.
Gravimetric analysis method is conducted through the following step:
1. Precipitation, this includes reaction of the dissolved substances. Precipitation is done by
adding excess amount of reactant/reagent so that the substance can be precipitated
completely. It should be noted that higher excess of reactant could result in unstable
precipitate and could possibly redissolve partially. As a reference, it is considered adequate
if 2 or 3 final drops of reactant may indicate that there would be no more precipitation
occurred.
2. Filtration, this should be done by utilising capiller force of solution, so that requires correct
selection of paper filter. Prevent any trapped gas between paper filter and funnel.
Sometimes, suction pump usage in filtration could slow down the filtration process,
especially when colloidal/micro particles are able to clog pore surface of paper filter.
3. Precipitate washing, this is to get pure crystal/solid precipitate by using small amount of
appropriate solvent (sometimes by using acid, base, warm water, alcohol, etc. Based on
charateristic of the crystal and its impurities). Other techniques may include
reacrystallisation or other purification methods.
4. Drying, warming/heating up inside hot surface, to make sure that the precipitates are
completely dried.
5. Weighing process of precipitate to get constant weight (completely dried). It should be
verified by conducting several times of drying/heating up and weighing until 2 values with
maximum deviation of 0.0002 gram is obtained consecutively.
5.2 Objectives
1. Students are able to weigh the material accurately
2. Students are able to correctly filter the sample solution
3. Students are able to fully understand the concept of simple gravimetic analysis
procedure
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4. Students are able to determine the recovery factor of a method/analysis
5.3 Experiment I (Determination TSS and Pb using Chromate solution)
5.3.1 Apparatus and Materials
1. Apparatus:
a. Beaker glass 100 mL
b. Spatulas
c. Funnel
d. Erlenmeyer flask
e. Evaporating dish
f. Wash bottle
g. Crucible tongs
h. Oven
i. Analytical balance
j. Desiccator
2. Materials:
a. Suspended solid solution: dissolved 2 g of Ca(OH)2 into 100 mL of aquadest
b. Sampel containing PbCl2
c. NaOH solution
d. Buffer acetate solution containing acetate acid 6 M and sodium acetate 0,6 M
(1:1)
e. Chromium Nitrate solution: 2,4 g / 100 mL
f. Pottasium Bromate solution: 2 g / 100 mL
g. Aquadest
h. Nitric acid 1%
i. Paper filter
5.3.2 Procedure of Experiments
5.3.2.1 Experiment I (Determination of Total Suspended Solid)
1. Prepare 10-15 mL of suspended solid solution
2. Filter the solution using paper filter, and wash the precipitate with a few drops of
aquadest
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3. Put the paper filter with precipitate in the evaporating dish, and dried in the oven at
120°C for 1 hour
4. Cool down for 2 minutes, then put the evaporating dish into desiccator for 15 minutes
until it reach room temperature
5. Weigh the precipitate with analytical balance
6. Repeat the procedure 3-5 until the deviation between measurement is 0.0002 g
7. Calculate the amount of precipitate recovered from this analisis!
5.3.2.2 Experiment II (Determination of Pb using Chromate solution)
1. Prepare sample solution containing 0.1-0.2 g of Pb (can be made from the solid of
PbCl2).
2. Netralise the solution using NaOH, until the precipitate has occured
3. Add 10 mL of buffer acetate solution, 10 mL of Chromium Nitrate solution, and
Potassium Bromate solution, respectively
4. Heat the solution at 90 – 95°C, until fully precipitate (about 45 minutes of heating) and
reach a clear supernatant.
5. Cool down the solution and filter. Wash the precipitate using a few drops of 1% nitric
acid
6. Dried the precipitate in the oven at 120°C for 1 hour
7. Cool down for 2 minutes, then put the evaporating dish into desiccator for 15 minutes
until it reach room temperature
8. Weigh the precipitate of PbCrO4 with analytical balance
9. Repeat the procedure 6-8 until the deviation between measurement is 0.0002 g
10. Calculate the amount of Pb recovered from this analysis!
5.4 Percobaan II (Penetapan Kalsium sebagai Oksalat)
5.4.1 Apparatus and Materials
1. Apparatus:
a. Beaker glass 400 mL
b. Spatula
c. Funnel
d. Erlenmeyer flask
e. Evaporating dish
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f. Wash bottle
g. Oven
h. Analytical balance
i. Desiccator
2. Materials:
a. Suspended solid solution: dissolved 2 g of Calcium into 100 mL of aquadest
b. Aquadest
c. Ammonium oxalate
d. HCl solution
e. Methyl red indicator
f. Filter paper
5.4.2 Procedure of Experiments
1. Prepare sample solution by dissolving 0.3 g of Ca into 60 mL of aquadest, then put
the solution into watch glass
2. Add 10 mL of aquadest followed by 15 mL of weak HCl (1:1)
3. Heat the watch glass until the Ca is fully dissolved, then boil for a few minutes until
CO2 has gone
4. Wash the glass, and dilute the solution until 200 mL and add 2 drops of methyl red
5. Boil the solution, then slowly add warm solution of ammonium oxalate (made
from 2 g of ammonium oxalate and 50 mL of aquadest)
6. Slowly add a few drops of diluted ammonium solution and stirred, until the pH of
solution is neutral or a bit of base (the colour of the solution turn into yellow)
7. Settle down the solution for 1 hour (minimum)
8. Filter the supernatant using paper filter, and wash it with a few drops of
ammonium oxalate solution
9. Put the precipitate into evaporating dish and heat the dish for 15 minutes using
Bunsen burner, then put in the furnace at 550oC about 30 minutes
10. Dried the precipitate in the oven at 120°C for 1 hour. Cool it down for 2 minutes,
then put the evaporating dish into desiccator for 15 minutes until it reach room
temperature
11. Weigh the precipitate with analytical balance
12. Repeat the procedure 10-11 until the deviation between measurement is 0.0002 g
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13. Calculate the amount of Ca recovered from this analysis!
5.5 In-depth Knowledge
1. In experiment I and II, why 100% of recovery can not be obtained?
2. Explain why procedure of heating/drying, cooling down, and weighing must be
repeated until the deviation of two consecutive procedures reaching maximum of
0.0002 gram?
3. What is the meaning of recovery analysis/method?
4. Explain factors that lead to potential errors in gravimetric analysis, and how to deal
with it?
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