See discussions, stats, and author profiles for this publication at: https://www.researchgate.
net/publication/367221783
GRAVIMETRIC DETERMINATION OF SULPHATE
Article · January 2023
CITATIONS READS
3 11,624
6 authors, including:
Irfan Ananda Ismail
State University of Padang
36 PUBLICATIONS 81 CITATIONS
SEE PROFILE
All content following this page was uploaded by Irfan Ananda Ismail on 18 January 2023.
The user has requested enhancement of the downloaded file.
IJCC: Indonesian Journal of Chemical Connections, Vol (1) No (1) page: 30-35 (2023)
IJCC: Indonesian Journal of Chemical Connections
Journal homepage: www.ijsea.online/chemical-connections
ISSN 2964-3325
GRAVIMETRIC DETERMINATION OF SULPHATE
Irfan Ananda Ismail1, Septian Budiman2, Farid Nauval Arkhaan3, Intan Nihati3, Irvandi
Sepriyanata3, Nurul Afifah*3
1Master Candidate in Chemistry Education, FMIPA Universitas Negeri Padang,West Sumatra, Indonesia
2Chemistry Major,Departmen Mathematics and Natural Science, Universitas Negeri Padang,,West Sumatra, Indonesia
3Chemistry Major,Departmen Mathematics and Natural Science, Universitas Negeri Padang,West Sumatra, Indonesia
ARTICLE INFO ABSTRACT
Gravimetric analysis is the process of isolating and measuring the
Keywords:
weight of a particular element or compound. The major part of the
gravimetric determination of compounds involves the transformation of
• gravimetric elements or radicals into stable pure compounds which can be readily
• determination of converted into a form that can be accurately weighed. Elemental weight
can be calculated based on the formula of the compound and the atomic
sulfate weight of the element the elements or compounds contained in it are
carried out in various ways, such as: precipitation methods; evaporation
method; electroanalytical method; or various other ways
INTRODUCTION
Gravimetry is the analysis of a substance by means of weighing as well deposition. A gravimetric
method for analysis is usually based on a chemical reactions such as: aA + rR → AaRr
Where a molecule of analyte A reacts with r molecules of analyte R. The product is AaRr, usually a
very slightly soluble substance, which can be weighed under conditions thus after the drying process or
which can be heated into other compounds whose composition is known, then weighed. So the steps in
gravimetry are:
1. Dissolving the substance, the solution must be clear and homogeneous.
2. Precipitate with reagent little by little.
3. Washing of deposits.
4. Weighing of sediment results ( Tim Kimia Analitik 1, 2019 )
The gravimetry method is a quantitative analysis method based on the principle of weighing.
Gravimetric analysis is used in several fields including to determine a compounds species and the
content of certain elements /molecules of a known pure compound based on changer in weight. Analysis
of water content in uranium oxide by gravimetric method using a microprocessor oven. Water is
physically absorbed by a solid material and does not form chemical bonds in a material can be realeased
again by forming steam. This water release is highly dependent on temperature and time ( Okdayani,
2017)
Gravimetric analysis is a precise way to determine the main and auxiliary components ( usually
materials) in ore and mineral samples. Sometimes this analytical method is used to test the validity of
various instrumental methods which are now widely used as a substitue for gravimetric analysis in
various routine analyses. This methode consists of isolating the analyte in specified stoichiometric form
and can be determined by weight. A commonly used working procedure is to precipitate the analyte
from solution in the form of a slightly soluble compound, by adding a suitable reagent or reagent. The
precipitate is separated by filtration, washed to remove impurities coprecipitation, than dried, and
weighed ( using whatman 41 filter paper ) (Tim Analitik, 2014).
The several stages in the gravimetric analysis are as follows :
The solvent chosen must be in accordance with the nature of the sample to be dissolved, for example
HCL, H2SO4 and HNO3 used to dissolve samples of metals
Precipitation of the analyte is carried out by separating the analyte from the solution containing it by
making the solubility of the analyte smaller and this precipitation is carried out perfectly. For example :
Ca2+ + H2C2O4 →CaC2O4 (white preciptate )
Sediment drying. Heat drying is matched to the analyte and is carried out perfectly
Weight the precipitate. The substance being weighed must have formula clear molecule
(Mursyidi,2018 )
Generally precipitation is carried out in a dilute solution to which the reagent is added slowly with
regular stirring, the particles formed first act as the center of precipitation. To obtained a large
precipitation center a reagent is added the increase the solubility of the precipitate ( Nurhadi, 2019 )
Gravimetric analysis or qualitative analysis based on weight is isolation and weighing of an element
or a certain compound from elements it, as pure as possible. The element or compound is separated by
a portion of the substance investigated and weighed. Most of the determinations on gravimetric analysis
of changes in elements or radicals to be analyzed get it into a pure and stable compound. Which can be
easily changed
into a form suitable for weighing. Then the elemental weights or radicality can easily be weighed
from our knowledge of formulas compound and the weight Lm of its constituent elements ( Indra,
2020)
One example of the gravimetric methods is to measure the weight of a porcelain dish where as much
as 0,50 g of a sample that has been heated in an oven at temperature of 110-120 for 2 hours, is put into
a porcelain dish, then put into a desiccator in which has been saturated with ammonium vapour. The
dessicator was closed and the sample was left in contact with ammonia vapor for 24 hours, then the
desiccators was opened. The methode of gravimetric analysis is carried out quantitatively where the
weight of the object is calculated. The difference in the surface adity analysis methode produces a surface
acidity value that is not much different, but the graimetric analysis method gives a lower surface acidity
value ( Widihati,2010).
In practice the first 2 methods are the must important, the gravimetric method takes quite a long
time, the presence of imporities in the constituents can be tested and if necessary factor correction factor
can be used (Pursitasari, 2020)
Gravimetry is the determination of the quantity or number of samples by calculating the weight of
the substance. So that in gravimetry the product must always be in solid form (solid). The main tool in
gravimetry is a balance with a good level of accuracy. In the precipitate formation reaction, where the
precipitate is the sample to be analyzed, we can carefully separate the precipitate from other substances
that also precipitate. Washing the precipitate is the next stage, the washing process is generally carried
out by filtering out the precipitate, carried out by rinsing it with water. The final stage of this process is
to purify the precipitate, by evaporating the solvent or water that is still in the sample, heating or drying
in an oven is commonly done. Finally the sample weighing can be carried out and the weighing result is
the quality of the sample being analyzed (Zulfikar, 2017 )
Trends Sci. 202x; xx(xx): xxxxx 3 of 13
MATERIAL AND METHODS
Tools :
1. Krus porcelain
2. Oven
3. Scales
4. Desicator
5. Funnel
6. Cup
7. Measuring cup
Materials :
1. 6M HCL solution
2. BaCl2 1,3 %
3. Na2SO4 crystals
4. K2Cr2O7
5. Aquadest
6. Filter paper
RESULT AND DISCUSSION
Results and discussion
Result
mass BaSO4 = n x molar weight
= 0,03 mol x 233,38 g/mol
= 0,70014 grams
Mass BaSO4 theoritical = 0,70014
Mass BaSO4 practical = 0,8055
Sulphate Theoritical Rate
SO 2-
=
𝑚𝑎𝑠𝑠 𝑠𝑢𝑙𝑝ℎ𝑎𝑡𝑒 x 1000 (mg)
4
𝑉𝑜𝑙𝑢𝑚𝑒 𝑠𝑜𝑙𝑢𝑡i𝑜𝑛 (𝐿)
= 1 𝑥 𝐴𝑟𝑆042− x mass BaSO 4
𝑀𝑟 𝐵𝑎𝑆04
= 1 𝑥 96 g/𝑚𝑜𝑙 x 0,70014 g
233 g/𝑚𝑜𝑙
= 0,288 grams
Rate SO 2- = 0,288 g x 1000 mg
4
0,0125 𝑙
= 23,040 ppm
Sulphate Practical Rate
2- 96 g/𝑚𝑜𝑙
Mass SO = x 0,8055 g
4
233
= 0,3318
2- 0,3318 g𝑟𝑎𝑚𝑠 𝑥 1000(𝑚g)
Rate SO =
4
0,0125 𝑙
= 26,544 ppm
𝑟𝑎𝑡𝑒 𝑝𝑟𝑎𝑐𝑡i𝑐𝑎𝑙−𝑟𝑎𝑡𝑒 𝑡ℎ𝑒𝑜𝑟i𝑡i𝑐𝑎𝑙
% mistake = 𝑡ℎ𝑒𝑜𝑟i𝑡i𝑐𝑎𝑙
x 100%
26,544 𝑝𝑝𝑚−23,040𝑝𝑝𝑚
= 23,040 𝑝𝑝𝑚
x 100 %
= 15,2 %
Discussion
In accordance with the theory that gravimetric determination of sulfate can be carried out by weighing and
precipitation, which means in accordance with the general understanding of gravimetry, which is a way to
analyze a substance by weighing and precipitation (Svehla,1994). From the experiments conduct on the
gravimetric determination of sulfate, its hoped that it can produce meaningful results. Because in this
experiment what is needed is not a qualitative value but a quantity value. Where the quantity value is the
presence or absence of a substance and the resulting weight. Before doing the practicum, we must first make
the porcelain crucible constant because if its not constant it will result in severe calculation errors so that the
levels may not be appropriate. Constant means that the difference between on weighing and the next is only
slightly with a tolerance of 5 %.
The sample used was Na2SO4 which was dissolved in HCl and added with aquadest.
Next the sample was heated to see if there was a precipitate formed was immediately carried out by adding a
solution of BaCl2 to the hot sample solution. Precipitation is carried out in a hot solution because the solubility
increases with increasing temperature. When BaCl2 is added, the solution becomes cloudy white because a
white precipitate is formed which is a BaSO4 compound. The reaction aquation is follows :
BaCl2 + Na2SO4 BaSO4 2NaCl
Next the solution was cooled and allowed to separate the white BaSO 4 precipitation under the solution. This
cooling process is carried out so that the cellulose filtering. Filtering is done using filter paper. After filtering,
the precipitate was washed with distilled water to remove Ba 2+ ion attached to the BaSO4 precipitate, to test
the presence of Ba2+ ion attached to the BaSO4 a test was carried out using F2CrO4 solution. If the water
resulting from washing the precipitation form a yellow precipitate after dropping F 2CrO4 solution, if can be
ascertained that Ba2+ ions are still attached to the precipitate. If after the drop of the reagent no more precipitate
is formed, then the washing can be stopped in this experiment, the precipitate was washed twice. Water is used
react with BaSO4 compounds and can dissolve Ba2+ ions the reaction equation is as follows :
Ba2+ + F2CrO4 BaCrO4 + 2F+
After that, the filter paper and precipitate were dried and then put into a porcelain crucible and ignited in a
furnaces at temperature of 90 0C which served to heat until the filter paper and precipitate turned to ash. And
finally it can be determined the value of the sediment mass. Due to time constants, the filter paper and the
precipitate did not turn into ash in experiment so that the results were as they wore.
The are several error factors in this experiment, including :
- There is a precipitate that escapes from the filter paper so that the sediment obtained is not optimal
- There are deposits that fall spill during filtering
- There are still Ba2+ ions attached to the precipitate so that the SO
4
-
obtained is not pure
There is still filter paper that has not been ashed so that the sediment mass obtained is not accurate
CONCLUSIONS
- Gravimetry is the analysis of a substance by weighing and precipitation. The principle of
gravimetry is to obtained the desired material or substance along with its pure weight.
- There are 2 gravimetric methods, namely : precipitation and evaporation method. In
gravimetry we must pay attention to accuracy in work, because what is need is a quantitative
value of a substance.
- In experiment carried out when adding F2CrO4 to a solution that has been separated from the
precipitate is will turn yellow.
REFERENCES
1. Indra, M.S. 2020. Kimia Analitik I. Malang : UNM press.
2. Mursyidi, Achmad, dan Abdul Rohman. 2018. Pengantar Kimia Farmasi Analisis Voumetri dan
Gravimetri. Yogyakarta : Gadjah Mada University Press.
3. Nurhadi, Agus. 2019. Dasar Kimia Analitik. Jakarta: UI
4. Okdayani, Yoskasih. 2010. “Penentuan Kadar Air Dalam Serbuk Vo 2 Dengan Metode Gravimetri”.
Hasil-hasil Penelitian EBN. Vol. 12.no 7.
5. Pursitasari,S. M. 2020 Konsep Dasar Kimia Analitik. Jakarta :Universitas Indonesia Press
6. Tim Kimia Analitik. 2014. Penentuan Praktikum dasar-Dasar Kimia Analitik. Jambi: Universitas Jambi.
7. Tim Kimia Analitik, 2019. Penuntun Praktikum Kimia Analitik 1. Padang. UNP.
8. Widihati., I.A.G.2010. Karakterisasi Keasaman dan Luasan Permukaan Tempurung Kelapa Hijau. Jurnal
Kimia. Vol. 1. No 4
9. Zulfikar. 2017. Penunjuk Praktikum Kimia Analisis Dasar. Palembang : Politeknik Negeri Sriwijaya
View publication stats
