Chapter 7
Chapter 7
Chapter 7
Indicators
b.) Eosin Y TS
dissolve 50mg of Eosin Y in 10ml of water
STANDARD SOLUTIONS
the reaction of the sample with the zinc dust in formic acid is such
as to reduce the mercuric ion to free elemental mercury which then
amalgamates with the excess zinc metal
the amalgam is dissolved in the nitric acid as it is being oxidized
to the bivalent state as Hg2+
the urea and potassium permanganate ensure that all the mercury is
in the form of mercuric ion
the excess potassium permanganate is then reduced by the hydrogen
peroxide, and the mercury is ready to be determined with the ammonium
thiocyanate
the assay for the phenylmercuric compound is performed by a direct
titration reaction of the available mercuric ion with thiocyanate
In the mercury content assay any and all mercury is converted to
elemental mercury and then oxidized before reacting with thiocyanate
Mercuric ion does not yield a copious precipitate upon titration
with ammonium thiocyanate as does silver ion
This is explained by the fact that mercuric thiocyanate Hg(SCN)2,
complexes with the yet unreacted Hg2+
The presence of halide ions (Cl, Br and I) will interfere with the
determination of mercuric mercury because they too form slightly
dissociated compounds, as does thiocyanate with Hg2+
CALCULATIONS:
1.) a 0.2182-g sample of sodium chloride was assayed by the Volhard
method using 50.00ml of 0.0985 N silver nitrate and 11.75ml of 0.1340N
ammonium thiocyanate. Calculate the percent NaCl in the sample.
Given:
Sample: 0.2182g
AgNO3: 50.0 ml & 0.0985 N
AgSCN: 11.75 ml & 0.1340 N
NaCl: mEq.wt: 0.05844
Formula:
% = 89.73
Theophylline
AKA: 8-chlorotheophylline
the determination of this substance in official preparations
such as aminophylline, aminophylline injection and tablets,
dimenhydrinate, theophylline tablets, theophylline olamine solution
and theophylline sodium glycinate and tablets is accomplished by the
reaction of theophylline with silver nitrate in a mole-for-mole ratio
Sodium tetraphenylboron
Na(C6H5)4B
will quantitatively precipitate such organic nitrogen
compounds as alkaloids, amines, and quartenary salts, as well as
ammonium, potassium and silver ions
Quaternary compounds
it will react with certain dyes such as bromophenol blue, an
anionic dye, to form a blue, chloroform-soluble complex and this
colored complex will react with sodium tetraphenylboron to form an
insoluble compound
COMPLEXATION METHODS
INTRODUCTION
the quantitative analysis of inorganic pharmaceutical products
containing metal ions such as Al, Bi, Ca, Mg and Zn was performed
using gravimetric methods
these procedures were very time-consuming, since they involved
precipitation, filtration, washing, and drying or ignition to constant
weight
official calcium preparations were later analyzed volumetrically
using an oxalate-permanganate procedure which involved a precipitation
technique and titration of a carefully heated solution of oxalate ions
Disodium ethylenediaminetetraacetate
C10H14N2Na2O8.2H2O
commonly reffered as EDTA
an analytical reagent used in a new volumetric procedure
evolved for metal determination employing metal-ion indicators in the
same manner that pH indicators are used in acid-base titrations
has a molecular weight of 372.24
consequently, a 1/20 M solution would contain 372.24/20 or
18.612g dissolved in 1 liter of solution
the water should be metal-free; therefore, glass-distilled
water is preferred
Solutions are best stored in polyethylene containers or in
glass containers previously prepared by boiling the container in an
alkaline 2% solution of EDTA to remove any metal ions
COMPLEXATION REACTION
COMPLEX when a metal ion combines with a molecule which can donate
electrons
NOTE!!
*** the higher the stability constant, the more acid the pH at which
the complexation titration can be run
*** Organic Solvents also increase the stability of the complex
*** Neutral Salts such as NaCl decrease the stability
* Eriochrome black T
the colored form are RED, BLUE and YELLOW-ORANGE
this dye is sensitive to changes in metal concentration as
well as to changes in Ph
RED COMPLEXES are formed with Mg2+, Zn2+ and many other metals,
such as Al, Ca, Pb, and Hg