APPROVAL SHEET

Complate report of Analytical Chemistry experiment with tittle

“Gravimetry” arranged by:
name : Radiatul Awalia Amir
ID : 1713441007
class : Icp of Chemistry Education
group : V (Five)
after checked by assistant and assistant coordinator, so this report accept

Makassar, October 2018

Assistant Coordinator, Assistant,

Desi Renika Khairul Ashar Chairan, S.Pd

Known by
Lecture of Responsibility

Sitti Faika, S.Si., Apt., M.Sc. Ph.D

NIP. 19780319 200501 2 003
A. THE TITLE OF EXPERIMENT
Gravimetry

B. OBJECTIVE OF EXPERIMENT
At the end of the experiment students can find out about:
1. Basic principle of gravimetry
2. Determine the contents of terusi crystalline water (CuSO4.xH2O) AND iron
content as iron (III) oxide

C. LITERATURE REVIEW
The science that deals with the identification and quantification of the
components of material systems such as these is called analytical science. It is called
that because the process of determining the level of any or all components in a
material system is called analysis. It can involve both physical and chemical
processes. If it involves chemical processes, it is called chemical analysis or, more
broadly analytical chemistry. The sodium in the peanut butter, the nitrate in the
water, and the ozone in the air in the above scenarios are the substances that are the
objects of analysis. The word for such a contained because substance is analyte, and
the word for the material in which the analyte is found is called the matrix of the
analyte (Kenkel, 2003: 1).
Several analytical methods are based on mass measurements. In
precipitation gravimetry, the analyte is separated from a solution of the sample as a
precipitate and is converted to a compound of known composition that can be
weighed. In volatilization gravimetry, the analyte is separated from other
constituents of a sample by conversion to a gas of known chemical composition.
The weight of this gas then serves as a measure of the analyte concentration. These
two types of gravimetry are considered in this chapter.' In electrogravimetry, the
analyte is separated by deposition on an electrode by an electrical current. Two
other types of analytical methods are based on mass. In gravimetric titrimetry, the
mass of a reagent, of known concentration, required to react completeLy with the
analyte provides the information needed to determine the analyte concentration.
Atomic mass spectrometry uses a mass spectrometer to separate the gaseous ions
formed from the elements making up a sample of matter (Skoog, 2004: 314).
Modified analytical strategy flow chart at the beginning of each discussion,
with the parts designated “carry out the analytical method” and “work the data”
highlighted. The first of the two wet chemical methods we will consider is the
gravimetric method of analysis. Gravimetric analysis is characterized by the fact
that the measurement of weight is the primary measurement, usually the only
measurement made on the sample, its components, or its reaction products. Thus,
weight measurements are used in the calculation of the results and are often the only
measurements used in this calculation. The analytical strategy flow chart specific
to gravimetric analysis (Kenkel, 2003: 37).
Solution reaction between analytes and reagents to give sparingly soluble
products; filtration, drying or ignition of precipitates; electrolytic deposition of
metals; weighing. Extensive numbers of inorganic ions are determined with
excellent precision and accuracy, widely used in routine assays of metallurgical and
mineralogical samples. Relative precision 0.1–1%. Requires careful and time-
consuming procedures with scrupulously clean apparatus and very accurate
weighings. Coprecipitation cannot always be avoided. Gravimetry includes any
analytical method in which the ultimate measurement is by weight. The simplest
form may merely be the drying or heating of a sample in order to determine its
volatile and non-volatile components, or possibly the sample might be distilled and
the residue and fractions of distillate weighed. Metals may be deposited
electrolytically and weighed. Subsequent attention will be restricted to these
precipitation methods (Fifield and Kealey, 2000: 216-217).
Ideally, a gravimetric precipitating agent should react specifically or at least
selectively with the analyte. Specific reagents, which are rare, react only with a
single chemical species. Selective reagents, which are more common, react with a
limited number of species. In addition to specificity and selectivity, the ideal
precipitating reagent would react with the analyte to give a product that is:
1. easily filtered and washed free of contaminants;
2. of sufficiently low solubility that no significant loss of the analyte occurs
during filtration and washing;
3. unreactive with constituents of the atmosphere;
4. of known chemical composition after it is dried or, if necessary, ignited.
Few, if any, reagents produce because precipitates that possess all these desirable
properties (Skoog, 2004: 315).
Precipitation is probably the most frequently used method in the practice of
qualitative analysis. The occurrence of a precipitate as the result of the addition of
a certain reagent may be used as a test for a given ion. In such cases we simply
observe whether the precipitate formed has the proper colour and general
appearance and sometimes carry out tests with further reagents, observing their
effectson the precipitate. The ease with which a precipitate can be filtered and
washed depends largely upon the morphological structure of the precipitate, that is
the shape and size of its crystals. Crystals with more complex structures, containing
dents and cavities, will retain some of the mother liquid, even after thorough
washing. With precipitates made up of such crystals quantitative separations are
less likely to be achieved (Svehla G, 1979: 83-84).
To be of gravimetric value, a precipitation process must fulfil certain
conditions. The precipitate must be formed quantitatively and within a reasonable
time. Its solubility should be low enough for a quantitative separation to be made.
It must be readily filterable and, if possible, have a known and stable stoichiometric
composition when dried so that its weight can be related to the amount of analyte
present. Failing this, it must be possible to convert the precipitate to a stoichiometric
weighable form (usually by ignition). In both cases the weighed form should be
non-hygroscopic (Fifield and Kealey, 2000: 217).
The laboratory instrument built for measuring weight is called the balance.
The name is derived from mechanical devices that utilize known weights to balance
the object to be weighed across a fulcrum, like a teeter-totter. Most balances in use
today are electronic, rather than mechanical, balances. An electronic balance is one
that uses an electromagnet to balance the object to be weighed on a single pan. The
older mechanical balances also utilize a single-pan concept, but these also use the
teeter-totter design, so they are mechanical and not electronic. Different examples
of laboratory work require different degrees of precision, i.e., different numbers of
significant figures to the right of the decimal point. Some balances are read to the
nearest gram; some are read to the nearest tenth or hundredth of a gram; some are
read to the nearest milligram; and still others are read to the nearest tenth or
hundredth of a milligram. Balances with few such significant figures to the right of
the decimal point (zero to three) are often referred to as ordinary balances or top-
loading balances precision is ± 100 to ±1 mg (Kenkel, 2003: 38).
The particle size of crystalline solids can often be improved significantly by
minimizing Q or maximizing S, or both,Minimization of Q is generally
accomplished by using dilute solutions and adding the precipitating reagent slowly
and with good mixing. Often, S is increased by precipitating from hot solution or
by adjusting the pH of the precipitation medium. Digestion of crystal1ine
precipitates (without stirring) for some time after for mation frequently yields a
purer, more filterable product. The improvement in filterability undoubtedly results
from the dissolution and recrystallization that occur continuously and at an
enhanced rate at elevated temperatures. Recrystallization apparently results in
bridging between adjacent particles, a process that yields larger and more easily
filtered crystalline aggregates. This view is supported by the observation that little
improvement in filtering characteristics occurs if the mixture
is stirred during digestion (Skoog, 2004: 320-321).
The rate of crystal growth is the other factor which influences the size of
crystals formed during the course of precipitation. If this rate is high, large crystals
are formed. The rate of crystal growth depends also on the degree of
supersaturation. It is advisable however, to create circumstances under which
supersaturation is moderate, allowing only a relatively small number of nucleid to
be formed, which in turn can grow into large crystals. Two important processes may
be distinguished which cause coprecipitation. The first is the adsorption of foreign
particles on the surface ofa growing crystal, while the second is the occlusionof
foreign particles during the process of crystal growth. Adsorption, in general, is
greatest because the precipitation with gelatinous precipitates and least for those of
pronounced macrocrystalline character (Svehla G, 1979: 84-85).
Precipitation from homogeneous solution is a technique in which a
precipitating agent is generated in a solution of the analyte by a slow chemical
reaction. This hydrolysis proceeds slowly at temperatures just below 100°C. Urea
is often used for the homogeneous generation of hydroxide ion. The reaction can be
expressed by the equation:
(H2N) 2CO + 3H2O CO2 + 2NH4- + 2OH-
Urea is particularly valuable for the precipitation of hydrous oxides or basic salts.
For example, hydrous oxides of iron(III) and aluminum, formed by direct addition
of base, are bulky and gelatinous masses that are heavily contaminated and difficult
to filter dehydration of aluminum oxide is not complete until a temperature greater
than IOOO°C is achieved. Below about 135°C, unbound water is eliminated to give
the monohydrate CaC204 • H20. This compound is then converted to the anhydrous
oxalate CaC204 at 225°C. The decomposition of calcium oxalate to calcium
carbonate and carbon monoxide. The final step in the curve depicts the conversion
of the carbonate to calcium oxide and carbon dioxide (Skoog, 2004: 324-326).
Since the successive surveys in 2013 of the Soultz network can be dismissed
because of an instrument defect, we basically only rely on the 6 surveys performed
in summer 2014 using a new instrument. The time changes of the weekly repetitions
of the stations are clearly small and mostly within the uncertainty level of the order
of 5 μGal. We have to repeat again these measurements in summer 2015 to check
that the changes from 1 year to the next are also small, especially in the lack of
geothermal activity. If this is true, we will then have a well-defined reference
network to detect the possible gravity changes that might occur when the
geothermal plant will be restarted in 2016. The comparison of the uncertainties in
the ties between the local reference station (GPK1) and the external reference
station (J9 Observatory) shows that the use of absolute measurements at GPK1
combined with continuous SG observations at J9 leads to better results than CG5
RG ties alone. It is also obvious that the ideal case would be to install at GPK1 a
permanent SG regularly checked with FG5 measurements as suggested in a true
hybrid gravimetric approach (Hiderer, 2015).
Another example of the use of the level of accuracy of the gravimetric
method is the low measurement results of glucomannan levels by gravimetry
presumably due to imperfect coagulation and precipitation processes. Coagulation
process and size. Coagulants are influenced by 3 factors, namely heating, stirring,
and addition electrolyte. The stirring done in this process is not uniform so the size
particles are not uniform too. This results in a large number of small size
precipitates pass the fine filter paper, so it's not weighted and not counted as
glucomannan. Various particle sizes cause the number of particles that pass through
the filter paper too varies, which results in high data variation and precision
decreases (Widjanarko, 2015).
D. APPARATUS AND CHEMICALS
1. Apparatus
a. Analytical balance (1 unit)
b. Exicator (1 unit)
c. Stove (1 unit)
d. Stir bar (1 unit)
e. Spray bottle (1 unit)
f. Drop pipette (3 units)
g. Watch glass (1 unit)
h. Beaker glass 500 mL (1 unit)
i. Beaker glass 50 mL (1 unit)
j. Graduated cylinder 10 mL (1 unit)
k. Graduated cylinder 250 mL (1 unit)
l. Clamp (1 unit)
m. Crus porcelain (2 units)
n. Funnel (1 unit)
o. Stopwatch (1 unit)
p. Smooth cloth (1 unit)
q. Rough cloth (1 unit)
2. Chemicals
a. Terusi crystal (CuSO4.xH2O)
b. Iron crystal (II) ammonium sulfate ((NH4)2 FeSO4.6H2O)
c. Aquadest (H2O)
d. Concentrated of nitric acid (HNO3)
e. Ammonia (NH3)
f. Ammonium nitric 1 % (NH4NO3)
g. Filter paper
h. Ammonium 1:1 (NH4)
i. Hydrochloric acid (HCl)
j. Aluminium foil (Al2O3)
k. Tissue
l. Label
E. WORK PROCEDURES
1. Determination of terusi crystal water (CuSO4 . X H2O)
a. Crus porceline weighed
b. Crus porceline heated for 10 minutes
c. Crus porceline cooled for 5 minutes (Repeat step a, b and c for 4 times)
d. Weighing 0.505 grams of fermented crystal (in a porcelain cup), recorded as Wo
e. Heated over a gas stove for 10 minutes, until the CuSO4 crystal is white
f. Moved into exicator for 5 minutes and after cold weigh again. Record the weight
as W1.
g. Reheat CuSO4 crystals over a gas stove for 10 minutes.
h. CuSO4 crystals cooled for 5 minutes. The last weight is recorded as Wn.
i. Calculate the water content of the crystal terusi by using the following formula:
(W0 – Wn)
BM Water
x=
Wn
BM terusi
2. Determination of Iron as iron III oxide
a. Weighing 0.803 grams of iron (II) ammonium sulfate crystals, and included in a
250 mL glass cup (weight is recorded as W0).
b. The solution is added with 250 mL of water and 10 mL of 1: 1 HCL stir and
covered with a arloji glass.
c. 3 mL of concentrated HNO3 is added to the solution and boiled for several
minutes until it has a clear yellow color.
d. Then the solution is diluted with water to 200 mL and boiled again.
e. Slowly added with 1: 1 ammonia to excess (smells of ammonia).
f. The solution is filtered with ash-free filter paper.
g. Washing precipitation with 1% ammonium nitrate + 250 mL of boiling water to
chloride ion free filtrate (test with silver nitrate solution) and incandescence at
800-900 0C.
h. The filtrate was tested with 0.1 N AgNO3
i. The precipitate on the crucible is heated over 5 minutes.
j. The results of the incendescence were weighed as Fe2O3 and the results were
recorded as W. The iron content in Fe2O3 was calculated using the formula:
2 x BM Fe x Wn (mg)
BM Fe2O3
X= x 100 %
W0 (mg)
F. OBSERVATION RESULTS
1. Determine the contents of terusi crystalline water (CuSO4.xH2O)
No Activity Result
1 - Crus porceline was weighed 30.516 gram
- heated for 10 minutes
- cooled for 5 minutes
2 - Crus porceline was weighed 30.506 gram
- heated for 10 minutes
- cooled for 5 minutes
3 - Crus porceline was weighed 30. 502 gram
 - heated for 10 minutes
- cooled for 5 minutes
4 - weight crystall Cu SO4 0.505 gram
- heated for 10 minutes
- cooled for 5 minutes
5 - CuSO4 crystals in porcelin was weighed 30,857
-heated for 10 minutes
-cooled for 5 minutes
6 - CuSO4 crystals in porcelin was weighed 30,859
-heated for 10 minutes
-cooled for 5 minutes
7 - CuSO4 crystals in porcelin was weighed 30,861
-heated for 10 minutes
-cooled for 5 minutes

2. Determine iron content as iron (III) oxide

No Activity Result
1 NH4Fe(SO4)2 Crsytal was weighed 0.803 gram
2 Dissolved with 250 mL H2O Yellow solution
3 Added 10 mL HCl 1:1 Yellow solution
4 Added 3 mL of concentrated HNO3 Yellow solution
5 The solution was heated Clear Yellow solution
6 Added 250 mL H2O Clear Yellow solution
7 Added ammonia 1:1 Precipitation formed
8 Filtered the solution
9 Put the filter paper into porcelin and heated Red brown
10 The filtrate is tested with AgNO3 0.1 n. Red brown
11 Precipitate and filter paper put in crusible Brown precipitate
12 Precipitate was heated brown
13 Precipitate was weighed Filter paper : 0.4353 g
 precipitate : 0.0367 g
Filter paper and
precipitate : 0.4353 g

G. DATA ANALYSIS
1. Determination the water content of crystal hydrate CuSO4.xH2O
Known: Mw H2O = 18 g/mole
Mw CuSO4.xH2O = 177.5 g/mole
Wcrus empty = 30. 502 grams
W0 + Crus = 30,857 grams
W0 = 0.505 grams
W1 + Crus = 30,859 grams
W2 + Crus = 30,861 grams
Asked: (x) the content of water =…?
Solution:
Wn = (W2 + Crus) grams – Wcrus empty
= 30,861 grams – 30. 502 grams
= 0.359 grams
(W0 −Wn ) (0.505−0.359)g
Mw H2 O 18 g/mole
x = Wn = 0.359 g
Mw CuSO4 .xH2 O 177.5 g/mole

0.00811 mole
= 0.002 mole

= 4.05
Based on theory
CuSO4∙xH2O → CuSO4 + x H2O
0,5 g - -
Crystal weight
Mole of CuSO4.5H2O = Mw terusi
0.500 g
= 177.5 g/mole

= 0.0028 mole
1
Mole of CuSO4 = 1 × 0.0028 mole = 0.0028 mole
 5
Mole of H2O = 1 × 0.0028 mole = 0.014 mole

Mass of CuSO4 = mole CuSO4 × Mw CuSO4

= 0.0028 mole × 159.5 g/mole
= 0.447 grams
Mass of H2O = mole H2O × Mw H2O
= 0.014 mole × 18 g/mole
= 0.252 grams
(m H2 O) 0.252 g
Mw H2 O 18 g/mole
x = m CuSO4 .xH2 O = 0.500 g
Mw CuSO4 .xH2 O 177.5 g/mole

0.014 mole
= 0.0028 mole

= 5
So, x (theory) = 5
x (experiment)
% rendement = × 100%
x (theory)
4.05
= × 100%
5

= 81 %
2. Determination of Fe as Fe2O3
Known: Mw Fe2O3 = 160 mg/mmol
Mw Fe = 56 mg/mmol
W0 = 0.803 g = 803 mg
W1 = 0.036 g = 36 mg
Asked: % Fe = ....?
Solution:
2 x Mw Fe
x W1 (mg)
Mw Fe 2 O 3
% Fe = x 100%
W0
(2 𝑥 56)𝑚𝑔/𝑚𝑜𝑙𝑒
𝑥 36 𝑚𝑔
160 𝑚𝑔/𝑚𝑜𝑙𝑒
= 803 𝑚𝑔
25.5
= 𝑥 100%
803
= 3.14%
Based on theory:
Menurut Teori
 Ar Fe
% Fe = x 100 %
Mr Fe 2 O 3

56 g/mol
= x 100 %
160 g/mol
= 35 %
H. DISCUSSION
Gravimetri merupakan suatu metode analisis kuantitatif suatu zat atau
komponen yang telah diketahui dengan cara pengukuran berat komponen dalam
keadaan murni setelah melalui proses pemisahan. Analisis gravimetri adalah cara
analisis kuantitatif berdasarkan berat tetap (berat konstannya). Dalam analisis ini
unsur atau senyawa yang dianalisis dipisahkan dari sejumlah bahan yang dianalisis.
Bagian terbesar analisis gravimetri menyangkut perubahan unsur atau gugus dari
senyawa yang dianalisis menjadi senyawa lain yang murni dan stabil sehingga dapat
diketahui berat tetapnya. Berat unsur atau gugus yang dianalisis selanjutnya
dihitung dari rumus senyawa serta berat atom penyusunnya dalam membentuk
suatu senyawa (Gandjar, 2007: 91).
Metode gravimetri untuk analisis kuantitatif didasarkan pada stoikiometri
reaksi pengendapan. Gravimetri merupakan penetapan kuantitas atau jumlah
sampel melalui perhitungan berat zat. Sehingga dalam gravimetri produk harus
selalu dalam bentuk padatan (solid). Prinsip dasar dari percobaan gravimetri
didasarkan pada stoikiometri pengendapan. Adapun prinsip kerja dari percobaan ini
adalah penimbangan, pemanasan, pendinginan, pencampuran, pengenceran,
pengendapan, dan pemijaran. Percobaan ini dilakukan dua tahap yaitu penentuan
kandungan air kristal terusi dan penentuan kadar besi dalam besi (III) oksida.
Adapun tujuan dari percobaan ini adalah untuk mengetahui kadar air yang
terkandung air dalam kristal terusi dan untuk menentukan kadar besi dalam besi
(III) oksida.
1. Penentuan Kandungan Air Kristal Terusi (CuSO4 anhidrat)
Tujuan dari percobaan ini yaitu untuk menentukan kandungan air yang ada
di dalam kristal terusi. Kristal terusi yang mengikat air berwarna biru sedangkan
yang tanpa air kristal berwarna putih. Kristal terusi yang digunakan dalam
percobaan ini adalah CuSO4 yang berwarna biru, ini menandakan bahwa pada
kristal tersebut mengikat air. Percobaan ini dilakukan berdasarkan prinsip dasar
gravimetri yaitu penguapan dan penimbangan dan hasil yang didapatkan dihitung
secara stoikiometri. Penguapan dilakukan untuk menetapkan komponen-komponen
dari suatu senyawa yang mudah menguap.
Metode penguapan ini dapat dilakukan dengan pemanasan untuk
memisahkan senyawa dari zat lain dan dilakukan penimbangan pada senyawa awal
dan senyawa akhir yang lebih murni sehingga dapat diketahui perbandingan berat
senyawa dengan komponen-komponennya yang ingin diketahui.
Langkah pertama yang dilakukan pada percobaan ini yaitu menimbang
kristal terusi menggunakan neraca analitik sebanyak 0,505 gram. Neraca analitik
digunakan karena memiliki keakuratan yang tinggi dibandingkan lainnya.
Selanjutnya kristal yang telah ditimbang dipanaskan dengan menggunakan oven.
Fungsi dari pemanasan yaitu untuk menghilangkan atau menguapkan air yang
terkandung pada kristal terusi CuSO4. Hilangnya kandungan air ditandai dengan
berubahnya warna kristal dari berwarna biru menjadi putih dan berkurangnya berat
kristal. Pemanasan pada suhu tinggi perlu dilakukan untuk menghilangkan air
secara sempurna. Senyawa CuSO4 dan kristal air berikatan secara kovalen sehingga
diperlukan energi yang besar untuk memisahkan ikatannya. Oleh karena itu,
diperlukan suhu yang tinggi untuk membebaskan molekul air agar dapat menguap
dan bereaksi dengan oksigen membentuk karbon dioksida sehingga pada akhirnya
kandungan air akan habis menguap dan yang tersisa adalah endapan murni CuSO4.
Pemanasan dilakukan di kompor gas karena oven yang berada di
laboratorium rusak. Hal pertama yang dilakukan adalah dengan memanaskan krus
porselin kosong, kemudian didinginkan dan ditimbang. Proses tersebut dilakukan
selama tiga kali pengulangan. Fungsi pemanasan adalah untuk menghilangkan
kandungan air yang berada pada krus porselin. Selanjutnya dilakukan penimbangan
kristal terusi sebanyak 0.505 gram. Kristal terusi dalam krus porselin dipanaskan
yang berfungsi untuk menghilangkan kandungan air yang berada di kristal
kemudian kristal dimasukkan ke dalam eksikator yang fungsinya untuk
mempercepat proses pendinginan karena di dalam eksikator terdapat silika yang
dapat menyerap panas. Hasil yang diperoleh setelah pemanasan dan pendinginan
kistal tersebut berubah dari warna biru muda menjadi warna putih. hal ini
menandakan bahwa Kristal yang sebelum dipanaskan mengikat air. Selanjutnya,
dilakukan pemanasan sebanyak 3 kali, diperoleh bobot kristal yaitu W 1 = 30.857
gram, W2 = 30.859 gram, W3 = 30.861 gram. Nilai yang diperoleh dari W2 dan W3
memiliki selisih 0,002 sama sehingga berat inilah yang dianggap berat konstan.
Dari hasil perhitungan diperoleh kandungan air sebanyak 4,05. Namun selisih yang
diperoleh pada percobaan ini tidak konstan, ini disebabkan karena kurang telitinya
praktikan serta keterbatasan waktu yang dimiliki sehingga percobaan tidak dapat
dilanjutkan dan mempengaruhi hasil.
Berdasarkan analisis data, diperoleh kandungan air hanya 4,05 artinya
koefisien H2O dalam kristal terusi adalah 4,05. Jadi, rumus kristal terusi yang
digunakan adalah CuSO4. 4,05 H2O. Sedangkan seacara teori kandungan air dalam
kristal terusi dalah 5 dengan rumus CuSO4. 5 H2O. Hal ini disebabkan karena
pemanasan yang dilakukan tidak maksimal dimana hanya dilakukan sebanyak 3x
dalam penentuan berat konstan dari kristal tersebut, yang seharusnya pemanasan
dihentikan hingga diperoleh selisih antara dua penimbangan hanya berbeda
beberapa mg saja. Selain itu pada proses pendinginan tidak digunakan eksikator
yang berfungsi untuk mempercepat proses pendinginan dan mencegah kristal terusi
mengikat kembali uap air. Sehingga kristal terusi yang sudah dipanaskan hanya
dipanaskan dalam udara bebas oleh karena itu kristal terusi mudah untuk menyerap
uap air an memiliki kandungan air yang masih banyak. Selama pemanasan
berlangsung, air menguap sesuai persamaan reaksi:
CuSO4∙xH2O → CuSO4(s) + xH2O(g)
∆

(Putih) (Biru)
2. Penentuan kadar besi sebagai besi (III) oksida
Tujuan dari percobaan ini adalah untuk mengetahui cara Penentuan kadar besi
sebagai besi (III) oksida. Percobaan ini dimulai dengan menimbang kristal
(NH4)2Fe(SO4) kemudian dilarutkan dengan H2O hal ini dilakukan karena Fe akan
teroksidasi dari Fe menjadi Fe2+.
Reaksi yang terjadi adalah:
 (NH)2 SO4. FeSO4 + H2O Fe + NH4+ + 2SO42-
Besi (II) Air Besi Ammonium Sulfat
ammonium
sulfat

Selanjutnya, larutan tersebut ditambahkan HCl 1:1. Tujuan penambahan HCl 1 : 1

adalah sebagai pemberi suasana asam yang mendukung terjadinya proses oksidasi
Fe2+ menjadi Fe3+. Setelah itu campuran tersebut ditambahkan dengan HNO3 yang
fungsinya untuk menyumbangkan NO3 yang nantinya berikatan dengan Fe3+.
Hasilnya larutan berwarna kuning jernih. Reaksi yang terjadi:

Fe + 2 HCl FeCl2 + H+
Besi Asam Besi (II) Ion
klorida klorida H
+

FeCl2 + 3HNO3 Fe(NO3)3 + HCl

Besi Asam Besi (III) Asam klorida
(II) Nitrat Nitrat
klorida

Larutan tersebut kemudian diencerkan dengan aquades dengan tujuan untuk

melarutkan semua zat terlarut dalam larutan kemudian dididihkan kembali untuk
mempercepat terjadinya reaksi. Setelah dididihkan, maka larutan ditambahkan
dengan amonia 1:1 sampai terbentuk endapan. Fungsi penambahan amonia 1:1
yaitu untuk mengendapkan Fe dalam bentuk Fe(OH)3. Selain itu sebagai hasil dari
reaksi antara larutan dengan amonia sehingga mempermudah proses pemisahan.
Adapun reaksinya :

Fe(NO)3 + NH3 + H2O Fe(OH)3NH4 + 3NO3-

Besi (III) Amonia Air Ammonium Nitrat
Nitrat Besi (III)
hidroksida

Fe(NO3)3 + NH4OH Fe(OH)3NH4 + 3NO3-

Besi (III) Nitrat Amonium Amonium Nitrat
Hidroksida Besi (III)
hidroksida
 Selanjutnya, larutan didiamkan sampai endapan turun ke permukaan gelas
kimia. Endapan yang diperoleh selanjutnya disaring menggunakan kertas saring
bebas abu dan menghasilkan endapan yang berwarna coklat. Penggunaan kertas
saring bebas abu ini karena memiliki pori-pori yang lebih kecil sehingga lebih
optimal memisahkan antara filtrat dengan endapan dibandingkan dengan kertas
saring biasa dan juga ketika dipijarkan bersama endapan tidak meninggalkan abu
sehingga hasilnya dapat dibedakan setelah dipijarkan.
Endapan yang telah disaring, dicuci dengan air mendidih yang telah
ditambahkan dengan NH4NO3 1% tujuannya yaitu untuk menyempurnakan
pembersihan dan menetralkan kembali endapan yang diperoleh. Pencucian dengan
air mendidih dilakukan sampai filtrat bebas ion klorida yang ditandai dengan
hilangnya warna putih pada filtrat ketika diuji dengan larutan perak nitrat.Tujuan
penambahan NH4NO3 1% ini untuk menghindari terikutnya ion-ion lain atau ion
pengganggu sehingga pada akhir percobaan akan diperoleh Fe dalam keadaan
murni. Adapun filtrat yang diperoleh diuji dengan AgNO3 yang berfungsi untuk
mengetahui apakah endapan sudah terbebas dari ion klorida atau belum, dimana hal
ini ditandai dengan tidak terbentuknya endapan putih pada saat filtrat ditetesi
AgNO3. Reaksi yang terjadi:

Fe(OH)3(S) + NH4 + 3NO3 Fe2O3. xH2O

Besi (III) Ammonium Nitrat Besi(III) Oksida
Hidroksida Hidroksida

Fungsi AgNO3 yaitu untuk menguji adanya ion klorida dalam filtrat.
Dengan cara menambahkan beberapa tetes AgNO3 ke dalam filtrat. Apabila filtat
bebas dari ion klorida maka larutan akan berwarna bening. Reaksi antara kedua
senyawa ini dapat menghasilka perak klorida dan ion nitrat.
Adapun reaksinya sebagai berikut:

AgNO3 + Cl- AgCl- + NO-3

Perak ion Perak Nitrat
Nitrat Klorin klorida
 Endapan yang telah dicuci, dipijarkan diatas kompor yang berfungsi untuk
menghilangkan air yang masih terkandung di dalam endapan. Adapun hasil pijaran
dari endapan coklat. Reaksi yang terjadi:

Fe(OH)3 Fe2O3 + 3H2O

Besi(III) Besi Air
Hidroksida (III)
oksida

Hasil pemijaran kemudian didinginkan setelah dipijarkan diatas kompor.

Hasil pemijaran kemudian ditimbang dan hasilnya penimbangan yaitu 1,656 gram
Fe2O3 dengan kadar besi sebesar 3.14%, artinya kadar Fe dalam 0,803 gram Fe2O3
sebesar 3,14%. Hasil tersebut sangat berbeda dengan teori yaitu 35 %. Hal ini
disebabkan karena reaksi tidak berlangsung secara sempurna pada saat penambahan
ammonia serta kurang bagusnya alat dan bahan yang digunakan dalam percobaan
ini.

I. CONCLUSION AND SUGGESTION

1. Conclusion
a. Gravimetry is a quantitative analysis that has the basic principles of purification
and weighing.
b. Determine the contents of terusi crystalline water (CuSO4.xH2O) and iron
content as iron (III) oxide. The contents of terusi crystal water (CuSO4.XH2O)
is 4.05 with a yield of 81% on the determination of iron precipitate is 3.14%.
2. Suggestion
In conducting the experiment it is expected to be careful in examining the
weighing and addition of chemical because it will affect the final results obtained.
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