LEAD

Method - Dithizone

Principle

An acidified sample containing microgram quantities of lead is mixed with ammonical
citrate-cyanide reducing solution and extracted with dithizone in chloroform to form a
cherry-red lead dithizonate.

Reagents

(1) Stock lead solution: - Dissolve 0.1599 g. lead nitrate in appoximately 200 ml dissolve
0.10 g. pure lead metal in 20 ml 1+1 HNO3 and dilute t 1000 ml with water.
1ml = 100 g Pb.
(2) Working lead solution :- Dilute 2.0 ml stock solution to 100 ml with water
1ml = 2 g Pb.
(3) Nitric Acid, 1+4:- Dilute 2.0 ml concentrate HNO3 to 1 l with water
(4) Ammonium hydroxide: - NH4OH- 1+9: - Dilute 10 ml concentrate NH4OH to 100 ml
with water.
(5) Citrate-Cyanide reducing Solution: - Dissolve 400 g. dibasic ammonium citrate 20 g.
anhydrous Sodium Sulfite, Na2SO3, 10 g. Hydroxylamine hydrochloride, NH2OH.
HCl and 40 g. Potassium cyanide, KCN, in water and dilute to 1 litter. Mix this
solution with 2 litter concentrate NH4OH.
(6) Stock Dithizone Solution (I)
(7) Dithizone working solution :- Dilute 100 ml stock dithizone solution to 250 ml with
CHCl3: 1 ml = 40 g dithizone
(8) Special dithizone solution:- Dissolve 250 mg. Dithizone in 250 ml CHCl3

(9) Sodium sulphite solution: - Dissolve 5 g. anyhydrous Na2SO3 in 100-ml water.
(10) Iodine solution: - Dissolve 40 g. Kl in 25-ml water, add 12.7 g. resublimed Iodine
and dilute to 1000 ml.

Procedure

(a)With Sample digestion: - To a digested Sample Containing not more than 1 ml conc.
Acid add 20 ml 1 + 4 HNO3 and filter through lead free filter paper and filter funnel
directly into a 250 ml separatory funnel.


Rinse digestion beaker with 50-ml water and add to filter. Add 50-ml ammonical
citrate-cyanide solution, mix and cool to room temperature. Add 10-ml dithizone
working solution, shake stopped funnel vigorously for 30 seconds and let layers
separate. Insert lead-free cotton in stem of separatory funnel and draw off beaker
layer. Discard 1 to 2 ml CHCl3 layers then fill absorption cell. Measure absorbance
of extract at 510 nm. using dithizone working solution.

(b) Without Sample Digestion: - 1 to 100 ml acidified sample (pH-2) in a 250-ml
separatory funnel. 2. Add 20 ml 1 + 4 HNO3 and 50 ml of citrate cyanide reducing
solution mix. Add 10-ml dithizone working solution, then proceed as above
procedure them measure absorbance of extract at 510 nm.

Calculation
mg Pb/L = g Pb (in 10 ml from calibration curve) / ml sample