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PENETAPAN KADAR NIKEL

DALAM NIKEL SULFAT


(NISO4)
Nama Kelompok :

Ahmad Pandu (4)

Nova Indah Nurmala (19)

Zsa Zsa Khafifah Octaviana (31)

ENGLISH

INDONESIAN

DASAR
Garam nikel dapat diendapkan dengan pereaksi
organik dimetilglioksima (dalam alkohol) dalam
suasana basa lemah, membentuk endapan nikel
dimetilglioksima yang berwarna merah.

REAKSI
NiSO4 + 2C4H8N2O2 + 2NH4OH

Ni(C4H7N2O2)2 + (NH4)2SO4 + 2H2O

PERALATAN DAN BAHAN


Peralatan

Bahan

Piala gelas 400 ml

Sampel Nikel sulfat (NiSO4)

Kaca arloji

Dimetilglioksima (C4H8N2O2) 1%
(dalam alkohol)

Tutup kaca

Ammonium hidroksida (NH4OH)


10%

Pengaduk

Barium khlorida (BaCl2) 0,5N

Cawan kaca masir

Asam khlorida (HCl) 4N

Vakum

Air suling

Desikator

Air suling panas

Kassa
Labu semprot
Kakitiga

CARA KERJA
1.

Timbang 0,1 gram NiSO4.7H2O.

2.

Larutkan dengan 100 ml air suling dalam


piala 400 ml.
Panaskan larutan sampai 80C
(thermometer).
Bubuhi 15 ml C4H8N2O2 1 % (dalam alkohol).

3.
4.
5.

Basakan dengan NH4OH 10 % sampai


terbentuk endapan dan tercium sedikit bau
NH3

6.
7.
8.
9.
10.

11.

Simpan piala dan isinya di atas penangas air


mendidih selama - 1 jam
Uji pengendapan sempurna
Saring dengan cawan kaca masir G2/G3 atau
cawan Gooch
Cuci endapan dengan air panas sampai bebas
sulfat
Keringkan endapan dalam cawan kaca masir
pada oven dengan suhu 140 C, didinginkan
dan ditimbang
Lakukan sampai bobot tetap Ni(C4H7N2O2)2

PENGHITUNGAN KADAR

Kadar
Ni = x 100%
fk = Faktor kimia

PEMBAHASAN
Garam Nikel dapat diendapkan dengan pereaksi
organik C4H8N2O2 (Dimetilglioksima) sebagai
endapan Ni(C4H7N2O2)2 (Nikel Dimetilglioksima)
yang berwarna merah. Dimetilglioksima
merupakan pengendap organik non polar yang
spesifik, hanya dapat digunakan untuk
mengendapkan Nikel dan Paladium.

Karena merupakan senyawa non polar,


Dimetilglioksima tidak dapat melarut dalam
pelarut polar seperti air. Oleh karena itu, pelarut
untuk senyawa ini harus juga bersifat non polar
seperti alkohol. Inilah alasan mengapa
Dimetilglioksima selalu dilarutkan dalam
alkohol.
Nikel Dimetilglioksima optimal pembentukannya dalam
suasana basa lemah (NH4OH), sedangkan Paladium
harus dalam keadaan asam (HCl). Selain
Dimetilglioksima, terdapat pula beberapa pereaksi
organik yang digunakan sebagai pengendap spesifik,
antara lain 8-Hidroksi Kuinolina dengan Alumunium
dan Magnesium, lalu Nitroso 2-Naftol dengan Kobalt.

Endapan yang dihasilkan (Nikel Dimetilglioksima)


merupakan endapan merah dengan kerapatan yang
rendah dikarenakan volumenya yang besar. Hal ini
mengakibatkan endapannya mudah merayap
(creeping). Endapan tidak perlu dipijarkan, cukup
dengan pemanasan dengan oven bersuhu 1400C.
Oleh karena itu digunakan cawan kaca masir sebagai
penyaring. Endapan ini kecil kelarutannya dalam air
suling panas, oleh karena itu pencuci digunakan air
suling panas untuk mempermudah pencucian. Untuk
mempercepat pengeringan, pada tahap terakhir
endapan dibilas dengan alkohol 1 : 1.

PERTANYAAN & JAWABAN


1. Mengapa Dimetil Glioksima dilarutkan dalam
alkohol?
Jawab : Karena merupakan senyawa non polar,
Dimetilglioksima tidak dapat melarut dalam
pelarut polar seperti air. Oleh karena itu, pelarut
untuk senyawa ini harus juga bersifat non polar
seperti alkohol.

2. Mengapa larutan harus dipanaskan sampai


80C?
Jawab : Karena suhu pemanasan mempengaruhi
larutan. Pemanasan hinggga suhu 80 C
dilakukan agar terbentuk endapan yang
sempurna karena jika suhu kurang dari 80 C
endapan tidak akan mengendap sempurna dan
apabila suhu lebih dari 80 C pereaksi organik
akan rusak.

3. Mengapa endapan harus dikeringkan pada suhu


140 C?
Jawab : Karena 140 C merupakan suhu yang
pas untuk mengeringkan endapan nikel.
Endapan nikel juga bersifat labil pada suhu di
atas 200 C.

4. Mengapa endapan Ni+ terbentuk dalam basa


lemah?
Jawab : Karena jika diendapkan dalam suasana
netral tidak akan terbentuk endapan, dan jika
diendapkan dalam suasana basa kuat akan
terjadi kopresipitasi.

5. Apakah Ni dapat diendapkan dengan pereaksi


non-organik?
Jawab : Tidak, karena dikhawatirkan apabila
diendapkan dengan garam (anorganik) dalam
suasana netral tidak akan terbentuk endapan
dan jika diendapkan dengan basa kuat
(anorganik) akan terjadi kopresipitasi.

BASIC THEORY
Nickel salt can be precipitated with
Dimethylglyoxime, an organic reagent in a weak
base condition, forms nickel dimethylglyoxime
precipitate that is red colored.

CHEMICAL REACTION
NiSO4 + 2C4H8N2O2 + 2NH4OH

Ni(C4H7N2O2)2 + (NH4)2SO4 + 2H2O

REQUIRED TOOLS & MATERIALS


Tools

Bahan

400 ml beaker glass

Nickel sulfate (NiSO4) sample

Watch glass

Dimethylglyoxime (C4H8N2O2) 1% (in


alcohol solution)

Glass

Ammonium hydroxide (NH4OH) 10%

Stirrer

Barium chloride (BaCl2) 0,5N

Sintered glass crucible

Hydrochloric acid (HCl) 4N

Vacuum

Distilled water

Desiccator

Hot distilled water

Wire gauze
Wash bottle
Tripod
Test tubes

PROCEDURES
1.

Measure 0,1 gram of NiSO4.7H2O.

2.

Dilute with 100 ml distilled water in 400 ml


beaker glass.
Heat the solution until 80C (using
thermometer).
Add 15 ml C4H8N2O2 1 % (in alcohol
solution).
Add NH4OH 10 % until it forms precipitate
and smells of ammonia (NH3).

3.
4.
5.

6.

Put the beaker along with the solution on


boiled-water bath for - 1 hour.

7. Do the test of perfect precipitation.


8. Filter the precipitate using a sintered glass
crucible (G2/G3).
9. Rinse the precipitate using hot distilled water
until the sulfate excess is cleared from the
precipitate.
10. Dry the precipitate in the oven in 140 C.
11. Cool the precipitate inside the desiccator.
12. Do the 10th-11st steps until the precipitates
(Ni(C4H7N2O2)2 ) constant weight is reached.

RATE CALCULATION

THEORY
Nickel salts can be precipitated with an organic
reagent, Dimethylglyoxime (C4H8N2O2,), resulting
the red-colored Nickel dimethylglyoxime
(Ni(C4H7N2O2)2) precipitate. Dimethylgyoxime is a
spesific non-polar organic reagent, and it is only
used to precipitate Nickel and Palladium.

Because Dimethylglyoxime is a non-polar


compound, it cannot be dissolved in polar
solvents, like water. Thus, the suitable solvent for
this compound is, the solvent must also have a
non-polar character, like alcohol. This is the
reason why Dimethylglyokximes are always
dissolved in alcohol.
Nickel Dimethylglyoximes are formed optimally in
weak base condition (using (NH4OH), while
Palladium precipitates should be formed in acid
condition (using HCl). Aside from Dimethylglyoxime,
there are other organic reagents that can be used to
precipitate Nickel salts or metals, e.g. 8Hydroxyquinoline with Alumunium and
Magnesium, and Nitroso 2-naphthol with Cobalt.

The precipitate which is formed (Nickel


dimethylglyoxime) is a red-colored precipitate with a
low density. Its low density is caused by its high
volume. This characteristic causes the precipitate to
creep in the filter. It is not required to burn the
precipitate, it is good enough to heat the precipitate in
the oven in 1400C.
That is why, it is advised to use a sintered glass
crucible as the filter. The precipitate has small
solubility in hot distilled water, thus hot distilled
water is used to rinse the precipitate and it eases the
rinsing. To hasten the drying time in the oven, at the
last step of rinsing the precipitate, the precipitate is
rinsed with 1:1 alcohol once.

QUESTIONS &
ANSWERS
1.

Why Dimethylglyoxime is dissolved in alcohol?


Answer : Because Dimethylglyoxime is a nonpolar compound, it cannot be dissolved in polar
solvents, like water. Thus, the suitable solvent for
this compound is, the solvent must also have a
non-polar character, like alcohol.

2. Why is the solution heated until 80C?


Answer : Because the temperature of the heating
affects the solution. Heating until 80C is done so
the solution can form a perfect precipitate. If the
temperature is less than 80C, the perfet
precipitate cannot be formed and if the
temperature is more than 80C, the organic
reagent can be damaged.

3. Why is the precipitate dried in 140 C ?


Answer : Because 140 C is the suitable
temperature to dry the nickel precipitate. The
nickel precipitate also exhibits volatility above
200 C.

4. Why is Ni+ precipitate formed in weak base


Answer : Because if Ni+ is precipitated in neutral
condition, no precipitate can be formed. And if
Ni+ is precipitated in strong base condition,
coprecipitation can occur.

5. Can Ni+ be precipitated with inorganic reagents?


Answer : No, because it is concerned if Ni+ is
precipitated with salts (inorganic), no precipitate
will be formed, and if Ni+ is precipitated with
base (inorganic), coprecipitation will occur.

6. What will happen if the solution is heated until


more than 80C ?
Answer : If the solution is heated until more than
80C , the organic reagent will be damaged.

7. Why is hot distilled water used to rinse the


precipitate?
Answer : The precipitate has small solubility in
hot distilled water, thus hot distilled water is
used to rinse the precipitate and it eases the
rinsing.

8. What are organic reagents?


Answer : Organic reagents are reagents which
are comprised of organic compounds.
An organic compound is any member of a large
class of gaseous, liquid or solid chemical
compounds whose molecules contain carbon. A
few types of carbon-containing compounds such
as carbides, carbonates, simple oxides of carbon
and cyanides are considered inorganic.