Gravimetric method

DETERMINATION OF NICKEL AS THE DIMETHYLGLYOXIMATE:

Discussion: Nice! i" #reci#itated $% the additio& o' a& etha&o!ic "o!(tio& o'
dimeth%!)!%o*ime+ i,e,H- DMG to a hot+ 'ai&t!% acidic "o!(tio& o' &ice! "a!t a&d the&
addi&) a "!i)ht e*ce"" o' a.(eo(" ammo&ia "o!(tio& /'ree 'rom car$o&ate0,The #reci#itate
i" 1a"hed 1ith co!d 1ater a&d the& 1ei)hted a" &ice!2 dimeth%!)%o*imate a'ter dr%i&)
at 33453-4C,
Ni
-6
6 -H-DMG Ni /HDMG0- 6 -H
6
H
OH O O
CH75C 8 N N8 C5CH7
CH7 5 C 8 N 6 -H
6
- 6 Ni
-6 Ni
CH7 5 C 8 N
CH75C8 N N8 C5CH7
OH
O O
H
The #reci#itate i" "o!($!e i& 'ree mi&era! acid"+ i& "o!(tio&" co&tai&i&) more tha& 94
#erce&t o' etha&o! $% vo!(me+ i& hot 1ater /4,:m) #er 344m!0 a&d i& co&ce&trated
ammo&ica! "o!(tio&" o' co$a!t "a!t"+ $(t i" i&"o!($!e i& di!(te ammo&ia "o!(tio&,+ i&
"o!(tio&" o' ammo&i(m "a!t" a&d i& di!(te acetic/ etha&oic 0 acid5"odi(m acetate
"o!(tio&",
Procedure: ;ei)h o(t acc(rate!% 4,7 to 4,< ) o' &ice! "a!t i&to a 944 m! $eaer 1ith a
"tirri&) rod, Di""o!ve it i& 1ater+ add 9 m! o' di!(te HC! /3:30 a&d di!(te to -44 m!, Heat
to =45>4C+ add a "!i)ht e*ce"" o' dimeth%!)!%o*ime rea)e&t+ a&d immediate!% add di!(te
ammo&ia "o!(tio& dro#1i"e+ 1ith co&"ta&t "tirri&) (&ti! #reci#itatio& tae" #!ace+ a&d
the& i& "!i)ht e*ce"" ,A!!o1 to "ta&d o& the "team $ath 'or -4574 mi&(te"+ a&d te"t the
"o!(tio& 'or com#!ete #reci#itatio& 1he& the red ##t ha" "ett!ed o(t, A!!o1 the #reci#itate
to "ta&d 'or 3 ho(r+ coo!i&) at the "ame time ,Fi!ter the co!d "o!(tio& thro()h a "i&tered
5)!a"" or #orce!ai& 'i!teri&) cr(ci$!e+ #revio("!% heated to 334 53-4C a&d 1ei)hed a'ter
coo!i&) i& a de"iccator, ;a"h the #reci#itate 1ith co!d 1ater (&ti! 'ree 'rom ch!oride /$%
te"ti&) 1ith A)NO7 to the 'i!trate0 a&d dr% it at 33453-4C 'or <9594 mi&(te", A!!o1 to
coo! i& a de"iccator a&d 1ei)h, Re#eat the dr%i&) (&ti! co&"ta&t 1ei)ht i" attai&ed a"
Ni /C<H=O- N-0-,
Yie!d:
Teacher?" Si)&at(re:
Ro!!, No:
Date:
EX@ERIMENT: TO DETERMINE THE @ERSENTAGE @ARITY OF @OTASSIAM
BROMIDE
THEORY:
Thi" e*#erime&t i" the #reci#itatio& titratio& i&vo!vi&) the #reci#itatio& reactio& $et1ee&
"i!ver &itrate a&d "odi(m ch!oride,
A)NO7 6 NaC! A) C! 6 NaNO7
-A)NO7 6 K- CrO< A)-CrO< 6 -KNO7
A "!i)ht e*ce"" o' A)NO7 "o!(tio& react" 1ith i&dicator K-CrO< a&d 'orm" a reddi"h
$ro1& co!or o' A)CrO<, ;he& @ota""i(m Bromide i" titrated a)ai&"t A)NO7 "o!(tio& the
Br
5
io& i" #reci#itated a" "i!ver $romide,
KBr 6 A)NO7 A)Br 6 K
6
6

NO7
5
Fir"t!% #rimar% ad"or$ed !a%er i" 'ormed a&d it 1i!! ho!d the "eco&dar% ad"or$ed
o##o"ite!% char)ed io& #re"e&ti&) the "o!(tio& ,A" "oo& a" the e.(iva!e&ce #oi&t i"
reached+A)
6
io&" are #re"e&t i& the e*ce"" 1hich are #rimari!% ad"or$ed a&d &itrate io&"
are "eco&dari!% ad"or$ed , D(ri&) titratio& the eo"i& i" ("ed a" i&dicator d(e to #re"e&ce
o' 1hich the co!or o' ##t, 1i!! cha&)e to the $ri)ht #i&i"h co!or at the e.(iva!e&ce #oi&t,
The 5ve io&" o' eo"i& 1hich are m(ch more "tro&)!% ad"or$ed+ tha& the &itrate io&" are
immediate!% ad"or$ed a&d 1i!! revea! it" #re"e&ce o' ##t, $% 'ormatio& o' #i&i"h
com#!e* o' "i!ver a&d a modi'ied eo"i& io&"+ are o& the "(r'ace 1ith the 'ir"t trace o' A)
6
io&",
PROCEDURE:
1. Preparation of 0.05 M NaCl solution:
4,=<99 )m o' "odi(m ch!oride 1a" tae& $%C 1ei)ht $% di''ere&ceC method, It
1a" the& tra&"'erred .(a&titative!% to a -94 m! vo!(metric '!a" a&d 1a" di""o!ved
i& deio&o"ed 1ater+ "hai&) co&ti&(o("!% 1hi!e addi&) to mae the "o!(tio&
homo)e&eo(",
Mo!arit% o' the "o!(tio&
2. Preparation of approx 0.05 M il!er nitrate solution:
-,3-- )m o' )ive& Si!ver &itrate "o!(tio& 1a" made -94m! $% addi&) deio&o"ed
1ater,
". tandardi#ation of t$e il!er nitrate solution %it$ odiu& C$loride:
34 m! o' Sodi(m Ch!oride "o!(tio& 1a" #i#etted o(t i& a co&ica! '!a", 3m! o' 9 D
@ota""i(m Chromate "o!(tio& 1a" added ,The& it 1a" titrated $% "!o1!% addi&)
"i!ver &itrate "o!(tio& 'rom $(rette, The additio& 1a" co&ti&(ed 1ith "hai&) ti!!
the co!or $ecome" 'ai&t reddi"h $ro1&, The titratio& 1a" carried o(t a&d three
co&c(rre&t readi&)" 1ere &oted,
'. Deter&ination of percenta(e purit) of *+r:
4,>79)m o' #ota""i(m $romide "o!(tio& 1a" tae& i& 344m! o' vo!(metric '!a"
a&d it 1a" di!(ted $% ("i&) deio&o"ed 1ater,
34m! o' KBr "o!(tio& 1a" #i#etted o(t i& co&ica! '!a", The& 7> m! o' deio&o"ed
1ater+ 3,9m! o' :M CH7COOH a&d 3m! o' eo"i& /i&dicator0 1a" added i&to
co&ica! '!a", It 1a" the& titrated 1ith "ta&dard "i!ver &itrate "o!(tio& 'rom $(rette,
The additio& 1a" co&ti&(ed 1ith "hai&) ti!! the co!or o' ##t 1a" #i&,
O+EER,-./ON:
.a0le1: tandardi#ation of il!er nitrate solution:
No, o' o$", Eo!,o' NaC!
/m!0
B(rette readi&)" 'or A)NO7/m!0 Co&c(rre&t readi&)
/m!0
I&itia! Fi&a! Di''ere&ce
.a0le 2: Deter&ination of %ei($t of *+r in t$e (i!en solution:
No, o' o$", Eo!,o' KBr
/m!0
B(rette readi&)" 'or A)NO7/m!0 Co&c(rre&t readi&)
/m!0
I&itia! Fi&a! Di''ere&ce
Result:
Calculation: