CHAPTER I

PREFACE

1.1. Objectives
1. Able to weigh the material accurately
2. Able to correctly filter the sample solution
3. Able to ensure that the precipitate is fully dried
4. Able to perform the precipitation technique and fully understand the concept of
simple gravimetic analysis procedure
5. Able to determine the recovery factor of a method/analysis
1.2. Principle
In this experiment, students dissolved anions and cation from the sample
solution can react to each other and salt of dissolved cation-anion. Salts of dissolved
cation-anion pairs can be interchanged with other cation-anion pairs, thus forming a
precipitated salt (marked with a smaller Ksp value). This precipitated salt is then
purified from all impurities that interfere with analysis such as moisture content, the
presence of other substances, and so on. The cation or anion analyte can be calculated
by comparison of the composition of the analyte ion in the salt deposit.
1.3. Basic Theory
The gravimetric method is one of the most commonly used quantitative and
accurate volume determination methods in research laboratories and in industry.
Gravimetric volumetric calibration standards like ASTM E542 and ISO have been
established over 20 years to calibrate volumetric apparatus and liquid-handling devices
with the capacity from 100μl to 2 l (Liang et al, 2012).

Gravimetric analysis or quantitive analysis by weiht is the process of isolating

and weighing an element or a definite compund of the element in as pure a form as
possible. (Jeffery et all, 1989)

Precipitation gravimetry is based on the formation of an insoluble compound

following the addition of a precipitating reagent, or precipitant, to a solution of the
analyte. In most methods the precipitate is the product of a simple metathesis reaction
between the analyte and precipitant; however, any reaction generating a precipitate can
potentially serve as a gravimetric method. Most precipitation gravimetric methods were
developed in the nineteenth century as a means for analyzing ores. Many of these
methods continue to serve as standard methods of analysis. (Harvey, 2000).

The substance that is measured, such as calcium in a aquadest sample or

trans,trans-muconic acid measured in blood as evidence of occupational exposure to
toxic benzene, is called the analyte (Manahan, 2001).
 Product recovery has traditionally been viewed as an economically beneficial
alternative to the ordering of new products. Product recovery is interpreted as a superior
concept that involves concepts like reuse and recycling. The aim with product recovery
is to retrieve a product’s inherent value when the product no longer fulfills the user’s
desired needs. A product is in this context interpreted as an artifact produced to fulfill a
user’s desired needs. This also implies that material is interpreted as a product (Lindahl,
2006).
 CHAPTER II
WORK SCHEME

2.1. Work Scheme

1. Experiment: Determination of Total Suspended Solid

Suspended Solid Solution (CaCO3)

Prepare 10 mL of suspended solid solution.

Filter the solution using paper filter and vacuum pump,

and wash the precipitate with a few drops of aquadest.
Paper Filter

Put the paper filter with precipitate in the evaporating

dish, and dried in the oven at 105°C for 1 hour.

Cool down for 2 minutes, then put the evaporating dish

into desiccator for 15 minutes until it reach room
temperature.
Dry Precipitate

Weigh the precipitate. Repeat the procedure 3 times until

the deviation between measurement is 0.0002 g.

Calculate the amount of precipitate recovered from this

method.

2. Experiment: Determination of Ca using Oxalate solution

Solution containing 0.3 g Calcium ( CaCO3)

Prepare sample solution by dissolving 0.1 g of Ca into 10

mL or 60 mL of aquadest, then put the solution into
watch glass

Add 10 mL of aquadest, followed by 2 mL of weak HCl

(1:1)

Heat the watch glass until the Ca is fully dissolved, then

boil for a few minutes until CO2 has gone

Wash the glass, and dilute the solution until 100 mL and
add 3 drops of methyl red
Dilute Solution

Boil the solution, then slowly add warm solution of

ammonium oxalate 10 mL

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).

Settle down the solution for 1 hour (minimum).

Supernatant

Filter the supernatant using paper filter, and wash it with

a few drops of ammonium oxalate solution.

Dried the precipitate in the oven at 105°C for 15 minutes.

(Weigh the mass)

Cool it down for 2 minutes, then put the evaporating dish

into desiccator for 15 minutes until it reach room
temperature.

Put the precipitate into evaporating dish and heat the dish
for 1 hour using Furnace (550o C).
Dry Precipitate (CaO)

Weigh the precipitate. Repeat the procedure until the

deviation between measurement is 0.0002 g

Calculate the amount of Ca recovered from this method

 CHAPTER III
DISCUSSION

3.1. Observation Result

1. Experiment: Determination of Total Suspended Solid

No. Observation Treatment Description/Reaction

1. Weigh the  Use Analytical Balance
filter paper  Put the watch glass, and calibrate
 Put the filter paper
 Result: 0.1652 g (Petri Dish: 34.7377 g)

2. Filtration in  Stir the CaCO3 to get the precipitate and put

Vacuum into cylinder glass 10 mL
Pump  Put the solution into Bekker Glass and rinse
the Cylinder Glass with aquadest
 Put the filter paper in Buchner Funnel
 Turn on the vacuum, and pour aquadest and
10 mL CaCO3.

3. Dry the  Put the paper filter with precipitate

filter paper  Dried in the oven at 105°C for 1 hour
 Cool down for 2 minutes, then put into
desiccator for 15 minutes until it reach
room temperature.
 Weigh the precipitate.
 Repeat the procedure 3 times (15 minutes
for second and third measurement) until the
deviation between measurement is 0.0002
g.
 Result: (Watch Glass + Precipitate)
1. 34.9794 g
2. 34.9789 g
3. 34.9787 g
 2. Experiment: Determination of Ca using Oxalate solution

No. Observation Treatment Description/Reaction

1. Take 10 mL CaCO3  CaCO3 is easy to precipate. So,
using Volumetric we should always mix the
Flask solution before put in Bekker
Glass
 Rinse the Cylinder Glass using
aquadest 2-3 times

2. Put 2 mL HCl (1:1)  Add 2 mL HCl (1:1) by pippete

slowly.
 The precipitate will lose and
the solution will be clear
3. Heat the solution in  Put the Bekker Glass in Heater
heater  Wait until the solution is boil
 Until CO2 lose from the
solution
 Put aquadest until 100 mL
 Stir with Spatula (perfect
dissolved)

4. Add 3 drops of  Add 3 drops of methyl red

methyl red using Pippete
 Stir the solution until the color
change into pink

Add Ammonium  Put 10 mL Ammonium Oxalate

Oxalate 10 mL with Volumetric Pippete
 Stir the solution with Spatula
when Amonium oxalate added.

Add a few drops of  Put the Ammonium using

diluted Ammonium Volumetric Pippete slowly
until the color of solution
change into yellow
 Check the pH value using
Litmus paper. If netral or a bit
of base, the solution is ready to
use
 Wait for 1 hour until
precipitate is formed
 Throw away the surface partly
(to analyze the precipitate
easily).
Filter using filter  Measure the filter paper and
paper porcelain, to know the first
mass
Result: 40.1787 g
 Put the filter paper in the top of
Erlenmeyer Flask
 Put the solution into
Erlenmeyer Flask slowly until
all solution filtrate perfectly
 Rinse the Bekker Glass using
aquadest
 Wait until all solution drop to
Erlenmeyer Flask

Dry the filter paper  Take the filter paper and put
into the porcelain
 Dried in the oven at 105°C for
15 minutes
 Cool down for 2 minutes, then
put into desiccator for 15
minutes until it reach room
temperature
 Measure the mass of filter
paper
Result:
1. 40.2721 g
 Put in Furnace  Heat in furnace for 1 hour
 Dried in the oven at 105°C for
15 minutes
 Cool down for 2 minutes, then
put into desiccator for 15
minutes until it reach room
temperature
 Dried in oven at 105o C for 15
minutes
 Measure the mass of filter
paper
Result:
1. 49,9860 g (another sample)

3.2. Discussion

The third practicum of Enviromental Chemistry I subject which is held on 12

October 2017 at 8.30 am – 14.30 am in Aquadest Treatment Laboratory discusses
Gravimetric Analysis. Gravimetric is the oldest and the simplest analytical technique to
quantitavely measure the amount of substance than any other chemical analysis.
Materials and apparatus for this experiment are:

1. Apparatus include:
 Beaker glass 100 mL
 Spatulas
 Vacuum Pump
 Buchner Funnel
 Erlenmeyer Flask
 Evaporating dish
 Wash bottle
 Volumetric Pippete
 Pippete
 Cylinder Glass 10 mL
 Oven
 Furnace
 Analytical balance
 Desiccator
 Porcelain

2. Materials include:
 CaCO3
 HCl (1:1)
 Filter Paper
 Litmus Paper
  Methyl Red
 Ammonium Oxalate
 Ammonium
 Aquadest

There are 2 experiments for this practicum. First, determination Total Suspended
Solid. We should find the Ca value from CaCO 3 solution. We need to prepare all
materials and apparatus. Take the Filter Paper and measure the mass using Analytical
balance. The mass of Filter Paper and Petri Dish is 34.9029 g. We need to know the
first mass. So, we can find the Recovery Factor. After that, put the filter paper under
Buchner Funnel. Prepare 10 mL CaCO 3 solution. We need to shake the solution to get
best precipitate and move it to 10 mL Cylinder Glass. Move the solution from Cylinder
Glass to Bekker Glass and rinse that for 2-3 times. Turn on the Vacuum Pump and spill
the 10 mL CaCO3 solution into Buchner Funnel. We get precipitate in filter paper now.

Take the filter paper from Buchner Funnel and put that in Petri Dish. Dried in
the oven at 105°C for 1 hour. It used to release H2O from the precipitate and to know
the pure mass of the precipitate. After that, take the Filter Paper and cool down for 2
minutes, then put into desiccator for 15 minutes until it reach room temperature. Weigh
the precipitate in Analytical Balance. After that, we repeat the procedure from dry the
precipitate in oven until measure the precipitate. The mass of precipitate are; 34.9794 g,
34.9789 g, and 34.9787 g. Average of precipitate mass is 34.979 g.

1. Recovery Factor:

Precpitate−(Filter Paper+ Petri Dish)

RF = x 100 %
mass of CaCO 3
34.979−(0.1652+34.7377)
RF ¿ x 100 %
0.1
RF = 76.1 %

2. Total Suspended Solution

Precpitate weight x 1000

TSS =
V
0.0761 x 1000
TSS =
10
TSS = 7.61 mg/L

Second experiment is determination of Ca using Oxalate solution. In this

experiment, we use 10 mL CaCO3 solution. After prepare all materials and apparatus,
move the 10 mL CaCO3 from Cylinder Glass to Bekker Glass. Rinse the Cylinder Glass
using aquadest to get all solution. Take 2 mL HCl (1:1) using Volumetric Pippete. Add
to CaCO3 solution slowly. HCl used for clear the solution. Put the solution in Heater and
heat until the solution is boil. Wait until the solution lose the CO 2. The solution will be
change into CaO.
 Wait for the minutes, and drop 3 methyl red to the solution using pippete. It
used to change the color of the solution and as an indicator. After that, add 10 mL
Ammonium Oxalate to the solution to accelerate precipitation process of the solution.
We should stir the solution when add the Ammonium Oxalate. Add Ammonium to the
solution until the color change into yellow and measure the pH value using Litmus
Paper. The solution should be neutral or little bit base. The pH value of the solution is
8.9.

Cool down the solution for 1 hour until the precipitate is formed. Throw away
the surface of the solution. Prepare the Filter Paper and Porcelain. The first mass of the
Filter Paper and Porcelain are 40.1787 g. Put the Filter Paper in upper part of
Erlenmeyer Flask and drop the solution slowly. It used to take the filtrate for the next
step. After all solution drop into Erlenmeyer Flask, take the Filter Paper and put in the
Porcelain again. Dried in the oven at 105°C for 15 minutes. It used to release H2O from
the precipitate and to know the pure mass of the precipitate. After that, take the Filter
Paper and cool down for 2 minutes, then put into desiccator for 15 minutes until it reach
room temperature. Weigh the precipitate in Analytical Balance. The mass of precipitate
is 40.2721 g. Another sample, that have weight 49.9134 g, heat the precipitate in
furnace at 550o C for 1 hour. We would get CaO from the drying process. Then, put
into oven at 105o C for 15 minutes. Take the precipitate and cool down for 2 minutes.
After that put into desiccator for 15 minutes until it reach room temperature. Weigh the
precipitate in Analytical Balance. The mass of precipitate after furnace is 49.9860 g.

1. Sample 1 (Oven):
Precipitate mass = mass after being dried (evaporating dish + filter paper
+ mass of precipitate) – mass before being dried
(evaporating dish + filter paper only)
= 40,2721 – 40,1787
= 0,0934 g

Ar Ca
Ca mass in the precipitate = x mass of precipitate
Mr CaCO 3
40.078
= x 0.0934
100.086
= 0,0374 g

The Recovery Factor :

Camass∈the precipitate
x 100 %
% RF = Ar Ca
x gr
Mr CaCO 3
0,0374
x 100 %
= 40,078
x 0.1
100,086
0,0374
= x 100 %
0,04004
 = 0,9339 x 100%
= 93,39 %

2. Sample 2 (Furnace):

Precipitate mass = mass after being dried (evaporating dish + filter paper
+ mass of precipitate) – mass before being dried
(evaporating dish + filter paper (ash) only)
= 49,9860 – 49,9134
= 0,0726 g

Ar Ca
Ca mass in the precipitate = x mass of precipitate
Mr CaCO 3
40.078
= x 0.0726
100.086
= 0,0518 g
The Recovery Factor :

Camass∈the precipitate
x 100 %
% RF = Ar Ca
x gr
Mr CaO
0,0518
x 100 %
= 40,078
x 0.1
56,077
0,0518
= x 100 %
0,07146
= 0,7248 x 100%
= 72,48%
 CHAPTER IV
CONCLUSION

4.1. Conclusion

Gravimetric Analysis is used to weigh the material accurately. So, we can find
the pure mass from the solution. There are many step to get the precipitate of the
solution, and one of them is filtration. We must do the filtration process correctly by
filter paper. The precipitate that used for practicum, we can find it in filter paper.
Another step is dry the solution using oven or furnace. We should ensure there is no
H2O in the precipitate. So, we can know the pure mass of the precipitate.

Able to perform the precipitation technique and fully understand the concept of
simple gravimetic analysis procedure is important. To get the precipitate, there are
several steps, like precipitation, filtration, precipitate washing, drying, and weighing.
Do it step by step . It will help us to understand the gravimetric analysis. And for the
last, recovery factor is ratio of mass of precipitate and mass of analyte and
representated in percent. From recovery factor, we can conclude the error process of
our experiment.

4.2. References

Harley, David, 2000, Gravimetric Methods of Analysis, Modern Analytical Chemistry,

United States, McGraw-Hill Companies, Page 235

Jeffery, G.H., J. Bassett, J.Mendham, R.C. Denney, 1989, Gravimetry, Vogel’s

Textbook Of Quantitive Chemical Analysis, United States, John Wiley &
Sons, Inc., Fifth Edition, Page 417
Liang, Dong, Chris Steinert, Stefan Bammesberger, Laurent Tanguy, Andreas Ernst,
Roland Zengerle and Peter Koltay, 2012, Novel gravimetric measurement
technique for quantitative volume calibration in the sub-microliter range,
Measurement Science and Technology, United Kingdom, IOP Publishing
Ltd, Vol. 24 (2013) 025301 (10pp)
Lindahl, Mattias, Erik Sundin, Johan Östlin and Mats Björkman, 2006, Concepts and
definitions for product recovery - Analysis and clarification of the
terminology used in academia and industry, Linköping University Electronic
Press Book Chapter

Manahan, Stanley, 2001, The Chemical Analysis Process, Fundamentals of

Environmental Chemistry, Second Edition

CHAPTER V
QUESTION

5.1. Question and Answer

1. In experiment I and II, why 100% of recovery can not be obtained?

Answer:
Because, when the all process happen, human error and disruption make
the recovery factor be far from 100%. It can be H 2O from the precipitate not
fully dried, the filtration process is not correctly or another potential error.

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?

Answer:
In gravimetric analysis, we should measure the precipitate, the H 2O from
the precipitate must be unless or nothing. So, we can find recovery factor that
approach with 100%. If the RF is 100% or approached, our experiment will be
succesful.

3. What is the meaning of recovery analysis/method?

Answer:
Recovery Factor is a ratio of mass of precipitate and mass of analyte and
representated in percent.

4. Explain factors that lead to potential errors in gravimetric analysis, and how to
deal with it?

Answer:
Potensial Error:
1. The precipitate is not perfectly formed
2. Fail to obtaint the pure precipitate because H2O is still present
 Factor:
1. Precipitation and filtration process does not correclty work.
2. There are still H2O in the precipitate
3. Environment made the precipitate is not pure
4. The amount of volume of other solutions that added to sample is incorrect
We can solve this problem by increase the accuracy level from the
material and apparatus that support Gravimetric Analysis or isolate the sample
from the environment. So, we can get the pure sample that used in Gravimetric
Analysis.

OFFICIAL LABORATORY REPORT

ENVIRONMENTAL CHEMISTRY
“GRAVIMETRIC ANALYSIS METHOD"

NAME : MUHAMMAD RIFANI

NRP : 03211740000056
LECTURER : ARSETO YEKTI BAGASTYO, ST., MT., M.Phil., Ph.D.
 LABORATORY’S ASSISTANT : KIKI GUSTINASARI

ENVIRONMENTAL ENGINEERING DEPARTMENT

FACULTY OF CIVIL ENGINEERING, ENVIRONMENT AND GEOSCIENCE
SEPULUH NOPEMBER INSTITUTE OF TECHNOLOGY
2017