HG/T 48222015

6.3.1 Potentiometric Titration(Arbitration law)

6. 3. 1.1 Method
2+ 3+
Oxidize Co to Co with potassium ferricyanide in ammonia solution. The e
2+
xcessive potassium ferricyanide is titrated with standard Co t i t r i m e t r i c s ol
ution.

Co 2 + + [Fe(CN)6] 3 - Co 3 + +[Fe(CN)6] 4 -

6. 3. 1.2 Reagent
6.3. 1.2. 1 Ammonium chloride
6. 3. 1.2. 2 Nitrite Acid Solution:1+1
6. 3. 1.2. 3 Hydrochloric Acid Solution:1+1

6.3. 1.2.4 Ammonium and Ammonium Citrate Solution

Weigh 50g Ammonium Citrate and dissolve in water, and then add 350ml ammonium so
lution, and dilute to 1000ml with water, mix well.

6. 3. 1.2. 5 Standard Cobalt titrimetric solution: Co= 3.000g/L

Weigh 3.000g Metal Co(content of Co: more than 99.99%) into 400ml beaker, add a f
ew water to wet and then slowly add 30ml Nitric Acid Solution, heat to dissolve all m
etal Co, cool to home temperature and t ransfer into 1000ml volumetric flask, dilute t
o the scale with water, mix well.

6. 3. 1. 2. 6 Standard p o t as s i u m f e r r i c y a n i d e titrimetric solution: Content of K 3 [F e(CN)

6 ]0.05mol/L
Preparation, Titration and calculation:
A).Preparation: weigh about 17g p o t a s s i u m fe r r i c y a n i d e a n d d i s s o l v e i n w a t e r ,
filtrate and dilute to 1000ml with water, mix well.
B).Titration: Transfer 20ml standard potassium ferricyanide solution in 250ml b
eaker with transfer pipette, add 5g ammonium chloride, 80ml ammonium and ammoniu
m citrate solution, place a stir bar closed with plastic, titrate with standard c
obalt titrimetric solution to titration jump(end point) on automatic potentiomet
ric titrator.
C) Calculation: c stands concentration of standard p o t a s s i u m f e r r i c y a n i d e titrim
etric solution, the unit of value is mol/L, the formula1 is following:

in which

V 1 s ta n d s t h e v a l ue of c o n su m p t i on of s ta n da r d c ob a l t t i t ri m e t r ic s o l
ution to titrate standard potassium ferricyanide solution, unit: ml;
V s t a n d s v o l um e o f s t an d a r d p o t a ss i u m f e rr i cy a n i d e s o l ut i o n , u ni t : m l ;
HG/T 48222015

s t a n d s v a l u e o f co n c e n t r a ti o n o f s t a nd ar d c o b a l t t i t ri m e t r ic s o l u t i
on, unit: g/L;
M stands the molar mass of Co, unit: g/mol(M=58.93).

6.3. 1 . 3 I n s t r u m e n t s a n d e q u i p m e n t s
Automatic potentiometric titrator: Magnetic stirring apparatus, Type 213 P
latinum electrode and Type 215 Tungsten electrode.

6.3. 1 . 4 P r o c e d u r e
Weigh 2.6g sample(accuracy: 0.0002g) into 150ml beaker. Add water and boi
l to dissolve, cool, transfer into 200ml volumetric flask, dilute to the scal
e with water, mix well.
T r a n s f e r 2 0 m l s t a n d ar d p o t a s s i u m f e r r i c ya n i d e s o l u t i o n i n t o 2 5 0 m l b e a k e r w
i t h t r a n s f e r p i p e t t e , add 5g a m m o n i u m c h lo r i d e , 8 0 m l ammonium and ammonium citra
te solution, stir on magnetic stirring apparatus, add 20ml test solution with transf
er pipette, platinum electrode as indicator electrode and tungsten electrode as refe
rence electrode, titrate with standard cobalt titrimetric solution to titration jump
(end point) on well-adjusted automatic potentiometric titrator.

6.3. 1 . 5 C a l c u l a t i o n
Mass fraction of Co is treated as content of Co, calculate acco rding to f
ormula 2

(2)

in which
V 1 s t a n d s v o l u m e o f st a n d a r d po t a s s iu m f e rri c y a n i d e s o l u t io n , u nit : m l ;
V 2 s t a n d s v ol u m e o f co n s u m p t i on o f s t a n da r d c o b a l t t i t r im e t r i c sol u t i o n , u n it : m
l;
s t a n d s co n c e n tr a ti o n o f s ta n d a r d c o b a lt t i t r i m e tr i c s ol u t i o n, u n i t : g /L ;
c s t a n d s co n c e nt r a t i o n o f s t a n da r d p ot a s s i u m f e r ri c y a n i de so l u t i o n , u n it : mo l /
L;
m stands weight of sample, unit: g;
M s t a n d s t h e m o l a r m a s s o f C o , u n i t : g / m o l (M= 5 8 . 9 3 ) ;
T r e a t t h e a r i t hm e t i c me a n v al i e o f t h e r e su l ts o f p a r al l e l d e t e rm i na t i o n a s f i n a l r
esult, the absolute difference between two parallel determiantion should be less tha
n 0.1%.