$t'""#() t*#"+$'-'t!%!**'t!+III MOHAMA1 LFIRI IN MAT 6SOH
ST1ENT NMER
20480247
PARTNER9S NAME
AMIRL IMRAN IN I1OPI
GROP
AS2022M
LECTRER9S NAME
1R. LIM YING CHI N
LA. INSTRCTOR
MISS SARAH
1ATE OF EXPERIMENT
5t &22n. OCT. 205
1ATE OF SMITION
30t OCT. 205
OBJECTIVE:
1. To synthesis synthesis potassium potassium tris(oxalate)ch tris(oxalate)chromium romium(III) (III) trihydrat trihydrate. e. 2. To prepa prepare re a copper copper(II) (II) oxal oxalate ate compl complex. ex. 3. To synthesis synthesis potassiu potassium m tris(oxa tris(oxalate)fer late)ferrate(III) rate(III) trihydrate. trihydrate.
INTRODUCTION:
One of import important ant aspects aspects of any chemical chemical researc research h was the prepar preparatio ation n of new compound. This process called as synthesis. In this experiment we will synthesised a special kind of compound called as a coordination compound. A coordination compound consisted of a central metal ion chemically onded to one or more atoms or !roups of atoms known as li!ands y coordinate co"alent ond. Transition metal readily formed these coordination compound# often resultin! in ri!ht colour. In this experiment we performed three experiment was aout preparation of crystals. The crystal that we prepared were potassium tris(oxalate)chromium(III) trihydrate# copper(II) oxalate complex and potassium tris(oxalate)ferrate(III) trihydrate. The amount of coordination compound expected from !i"en mass of reactants can e calculated and it was called theoretical yield. The actual mass of the coordination compound synthesised was called actual yield and it was usually less than the theoretical yield.
PROCEDURE: Experiment 3
1. $.%% ! of oxalate oxalate acid was was dissol"ed dissol"ed in 1% 1% ml distilled distilled water water in a conical conical flask. flask. 1.& ! of potassium dichromate was added into the mixture in small portions and the funnel was placed on the mouth of conical flask. 2. After the the reaction reaction had susided# susided# 2.1% 2.1% ! of of potassium potassium oxalate oxalate monohy monohydrate drate was was added into the hot !reen'lack liuid and it was heated until oilin! for $ minutes. 3. The flask flask was cooled cooled down at at room temperature temperature and and 1% ml ml $* ethanol ethanol was added into the flask and it was cooled in ice ath with freuent stirrin!. +. After coolin! coolin! in ice ice for 1$ minutes minutes or or when the the precipitate precipitate completely completely formed# formed# the precipitate was collected y suction filtration. $. The crystals crystals were were washed with $ ml portion portion 1,1 1,1 ethanol-d ethanol-distille istilled d water and and followed y 13 ml of $* ethanol. . The crystals crystals were placed placed on the the watch watch !lass and it was allowed allowed to dry dry in the o"en. o"en. /. The mass mass of the the synthesis synthesis crystals crystals and percenta!e percenta!e yield yield were were determined. determined. &. The crystals crystals were transferre transferred d into a plastic plastic packet. packet. It was kept kept for next next experiment. experiment. Experiment 4
1. 2.%% ! copper(II) copper(II) sulphate sulphate was was wei!hed wei!hed and it was was placed in conical conical flask. flask. 3% ml of distilled water was added in the flask. The flask was heated slowly on a hot plate until the solid dissol"es. 2. .2% ! of potassium potassium oxalate oxalate monohy monohydrate drate was dissol" dissol"ed ed in 3% ml ml of distilled distilled water water in another flask. 3. The heat heated ed 0u 0uO+ solution was added into the flask contained potassium oxalate monohydrate slowly. The flask was swirled swirle d slowly to mix. +. The mixture mixture was cooled cooled in ice ath for for 3% minutes. minutes. lue lue crystals crystals were formed. formed. $. The crystals crystals were placed placed on the the watch watch !lass and it was allowed allowed to dry dry in the o"en. o"en. . The mass mass of the the synthesis synthesis crystals crystals and percenta!e percenta!e yield yield were were determined. determined. /. The crystals crystals were transferre transferred d into a plastic plastic packet. packet. It was kept kept for next next experiment. experiment.
Experiment 5 Procedure A
1. $.%% ! of ferrous ferrous ammonium ammonium sulphate sulphate was was dissol"ed dissol"ed in 2$ 2$ ml distilled distilled water water containin! 1 ml of diluted sulphuric acid in the eaker. 2. 2.$% ! of oxalate oxalate acid dihyd dihydrate rate was dissol"ed dissol"ed in 2$ ml of of distilled distilled water water in another eaker. Then it was added into the eaker containin! ferrous ammonium sulphate. 3. The mixture mixture was heated heated slowly slowly until until oilin! oilin! and then then it was was allowed allowed the yellow yellow precipitate to settle. The supernatant was discarded. 1$ ml hot water was added into the yellow precipitate. It was stirred and a nd the supernatant was discarded. +. 1$ ml of hot hot water was was added to to precipitate. precipitate. 3.$ 3.$ ! of solid solid potassium potassium oxalate oxalate o
monohydrate. It was heated to approximately +% 0. Then immediately 1% ml of * 2O2 was added drop wisely and it was stirred continuously. continuously. $. It was heated heated to oilin! oilin! and and the dissol" dissol"ed ed solution solution of 2.% 2.% ! of oxalic oxalic acid in in 3% ml of of distilled water was added into the mixture until the rown precipitate was dissol"ed. . It was oiled oiled until the the solution solution was clear. clear. The The solution solution was filtered filtered throu!h throu!h uchner uchner funnel. 3% ml of $* ethanol e thanol was added slowly to the solution. Any crystals were formed was redissol"ed. Then# it was lea"ed in not direct li!ht to crystallise for a week. Procedure B
1. The crystals crystals were collected collected y suction suction filtration filtration process. process. The eaker eaker was was rinsed with with 1% ml of 1,1 ethanol-distillation water for two times. The crystals were washed with cold acetone. 2. The crystals crystals were were placed on the the watch !lass and and it was was allowed allowed to dry dry on air. air. 3. The mass mass of the the synthesis synthesis crystals crystals and percenta!e percenta!e yield yield were were determined. determined. +. The crystals crystals were transferre transferred d into a plastic plastic packet. packet. It was kept kept for next next experiment. experiment.
tris(ox tris(oxalat alate)fe e)ferrat rrate(II e(III) I) trihyd trihydrate rate.. The The proces processs to synthe synthesis sis the crystal crystalss were were known known as crystallisatio crystallisation. n. The results of the experiment experiment that we otained otained were +.&/1 +.&/1 ! emerald !reen solid 7 380r(02O+)3. 32O# 2.1% ! lue solid 7 280u(02O+)2(2O)29 and +.+%/& ! !reen solid 7 38
7 380r(02O+)3.
32O#
1.11
*
of
7 2 80u(02O+)2(2O)29
and
/%.13
*
of
7 38
CONC!UION:
The
conclusion
in
tris tris(o (oxa xala late te)c )chr hrom omiu ium( m(II III) I)
the
experiment
trih trihy ydrat drate# e#
was
copp copper er(I (II) I)
the
oxal oxalat atee
crystals comp comple lex x
of
potassium
and and
pota potass ssiu ium m
tris(oxalate)ferrate(III) trihydrate were synthesised y crystallisation process. The percent yield ield of the the cry crystal stalss ota otain ined ed were ere &/.3 &/.3 * of 7 380r(02O+)3. 32O# 1.11 * of 7 280u(02O+)2(2O)29 and /%.13 * of 7 38
RE-ERENCE:
