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USP Limit Test For Lead

This document describes a procedure for determining the amount of lead in a substance using liquid-liquid extraction with a metal chelator. The procedure involves digesting the sample with sulfuric acid and hydrogen peroxide to destroy organic substances. The acidified sample is then mixed with ammoniacal citrate-cyanide solution and extracted with dithizone in chloroform to form a cherry-red lead dithizone complex. The concentration of lead is determined by comparing the color of the extract to that of a standard lead solution treated the same way.

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1K views2 pages

USP Limit Test For Lead

This document describes a procedure for determining the amount of lead in a substance using liquid-liquid extraction with a metal chelator. The procedure involves digesting the sample with sulfuric acid and hydrogen peroxide to destroy organic substances. The acidified sample is then mixed with ammoniacal citrate-cyanide solution and extracted with dithizone in chloroform to form a cherry-red lead dithizone complex. The concentration of lead is determined by comparing the color of the extract to that of a standard lead solution treated the same way.

Uploaded by

Abby Mata
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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LIMIT TEST FOR LEAD

Liquid-liquid extraction using Metal Chelator


Transfer 1.0 g of the substance under test to a suitable flask, add 5 mL of sulfuric acid and a few glass beads,
and digest on a hot plate in a hood until charring begins. Other suitable means of heating may be substituted.
(add additional sulfuric acid, if necessary, to wet the substance completely, but do not add more than a total of
10 mL.) add, dropwise and with caution, 30 percent hydrogen peroxide, allowing the reaction to subside and
again heating between drops. Add the first few drops very slowly, mix carefully to prevent a rapid reaction, and
discontinue heating if foaming becomes excessive. Swirl the solution in the flask to prevent unreacted substance
from caking in the walls of the flask. [Note- Add peroxide whenever the mixture turns brown or darkens.]
Continue the digestion until the substance is completely destroyed, copious fumes of sulfur trioxide again is
evolved, and cool. Repeat this procedure with another 10 mL of water to remove any traces of hydrogen
peroxide. Cautiously dilute with 10 mL of water, and cool.
Procedure:
Transfer the Test Preparation, rinsing with 10 mL of water, or the volume of the prepared sample specified in the
monograph to a separator, and unless otherwise directed in the monograph, add 6 mL of Ammonium Citrate
Solution and 2 mL of Hydroxylamine Hydrochloride Solution. (For the determination of lead in iron salts use 10
mL of Ammonium Citrate Solution.) Add 2 drops of phenol red TS, and make the solution just alkaline (red in
color) by the addition of ammonium hydroxide. Cool the solution if necessary, and add 2 mL of Potassium
Cyanide Solution. Immediately extract the solution with 5-mL portions of Dithizone Extraction Solution, draining
off each extract into another separator, until the dithizone solution retains its green color. Shake the combined
dithizone solutions for 30 seconds with 20 mL of dilute nitric acid (1 in 100), and discard the chloroform layer.
Add to the acid solution 5.0 mL of Standard Dithizone Solution and 4 mL of Ammonia-Cyanide Solution, and
shake for 30 seconds: the color of the chloroform layer is of no deeper shade of violet than that of a control
made with a volume of Dilute Standard Lead Solution equivalent to the amount of lead permitted in the sample
under examination, and the same quantities of the same reagents and in the same manner as in the test with
the sample.
Principle Involved
-Complexometry
-acidified sample containing lead is mixed with ammoniacal citratecyanide reducing solution
-solution is extracted with dithizone in chloroform (CHCl3) to form a
cherry-red lead dithizone
-pH ~ 9.5 will favor complexation of dithizone with Pb+2
Dithizone (diphenylthiocarbazone)
-green compound that is soluble in nonpolar organic solvents
-forms red, hydrophobic complexes with most di- and trivalent metal
ions
-as long as the organic phase turns red, metal ions are being
extracted from the buffer
-when the extracts are green, the last traces of metal ions have been
removed
-only certain metal ions can be extracted at a given pH
-preliminary digestion with sulfuric acid and hydrogen
peroxide oxidizes interfering metal ions and organic substances (digestion is complete when solution
becomes clear)
-addition of citrate exerts solvent action on calcium phosphate and separates it from lead phosphate (e.g.
analysis of bones)
used to keep lead in solution and avoid precipitation of lead phosphate in the alkaline condition
-hydroxylamine hydrochloride prevents oxidation of dithizone by ferric ions in the presence of cyanide (e.g.
analysis of blood)
-phenol red= indicates alkaline solution; yellow (pH 6.8), red (pH=8.4)
-weakly ammoniacal potassium cyanide solution (pH 8.5 to 9.5) complexes metals (Cd, Zn, Cu, Co, Ni)
except Bi+, Pb+2, Sn+2 and Tl+1
-acidifying with HNO3 Bi+ and Sn+2 complexes with dithizone; Pb+2 separated in aqueous solution
Tl+- extracted only partially and is rarely present in samples
-washing with chloroform to remove dithizone from aqueous solution
MAROHOMSALIC | MATA | PH CH 135 SECTION A

-standard dithizone solution vs. dithizone extraction solution the concentration of the latter is not known/not
standardized because it is only used for extracting the lead dithizone complex. In measuring for absorbance, std.
dithizone solution is used because the concentration is known

MAROHOMSALIC | MATA | PH CH 135 SECTION A

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