Acidimetry

ACIDIMETRIC ANALYSIS

 DIRECT TITRATION
 conducted by introducing a STANDARD ACID
SOLUTION gradually from a buret into a solution of the
base being assayed until chemically equivalent
amounts of each have reacted as shown by some
change in properties of the mixture.
Direct Titration

 % P = ( Vol of acid ) x (N of acid) x meq of analyte x 100

Sample weight (g)

 % P = ( Vol of acid) x (NF of acid) x titer for analyte x 100

Sample weight (mg)
ASSAY OF SODIUM BICARBONATE – DIRECT
TITRATION METHOD

 METHYL ORANGE – used as indicator because

phenolphthalein and most other indicators are affected
by the carbonic acid liberated in the reaction, which
causes a change in color before the reaction is
complete.

2NaHCO3 + H2SO4 → Na2SO4 + 2H2O + 2CO2 

Sample Problem:
% NaHCO3 = ml x N x meq. wt. of NaHCO3 x 100
sample wt. (g)

If exactly 1.5 grams of NaHCO3 required 25.5mL of

1.011 N HCl VS, what will be the % NaHCO3 in the
assay?
Sample Problem:

If a 0.2800 – g sample of sodium bicarbonate

(96.5%NaHCO3) is titrated with 0.9165N sulfuric aid,
what is volume of the acid should be required to
produce an end point?
 ACIDIMETRIC ANALYSIS
 RESIDUAL TITRATION (BACK TITRATION)

 usedwhen ever the end point of a direct titration

deviates appreciably from the stoichiometric
points for some reason
 Ex.when the basic sample is insoluble in water and rate
of its reaction with the standard acid is relatively slow.
 when the substance to be assayed does not give
a distinct, sharp end point with an indicator by
direct titration.
Residual Titration
% P = [( Vol x N of acid ) - (Vol x N of base] x meq of analyte x 100
Sample weight (g)

% P = [( Vol x NF of acid ) - (Vol x NF of base)] x titer for analyte x100

Sample weight (mg)
ASSAY OF ZINC OXIDE

 freshly ignited zinc oxide, contains nlt 99% and nmt

100.5% of ZnO
 MO – indicator
 Titrant – 1N H2SO4 and 1N NaOH

•Residual titration is carried out by dissolving the analyte in

an accurately measured quantity of VS known to be in
excess and titrating the excess of the latter with another
standard solution.

•The equivalent weight is 40.68g, therefore each mL of 1N

H2SO4. 1 mEq neutralized by ZnO is equivalent to 40.68 mg.
 (ml acid x N) -(ml base x N) x meq.wt. x 100
%ZnO = --------------------------------------------------------
Sample weight

Sample Problem:
 1. Calculate the titer value of 1N H2SO4 for ZnO.
Zn = 65.38 O = 16
 2. If 1.2 g of ZnO, were treated with 50 mL of 1.1230N
sulfuric acid, and 27.6 mL of 0.9765N NaOH were
required in the back titration. Calculate the %ZnO
in the sample
ASSAY OF MILK OF MAGNESIA – RESIDUAL
TITRATION METHOD
 Methyl red – indicator used.
 U.S.P. requires that milk of magnesia contain not
less than 7% and not more than 8.5% Mg(OH)2.
 Milk of magnesia is dissolved in accurately
measured excess of 1N sulfuric acid solution to
ensure complete neutralization of all the
magnesium hydroxide with the formation of the
soluble magnesium sulfate.
Formula:

(mL acid x N)–(mL base x N) x meq.wt. x 100

%Mg(OH)2 = ----------------------------------------------------
Sx wt in grams

Sample Problems:
1. What is the percent Mg(OH)2, if a sample of magnesia magma
weighing 5.2430g when dissolved in 25ml of 0.9915N H2SO4
required 9.85ml of 1.1402N NaOH to titrate the excess acid?

2. Calculate the MgO content of milk of magnesia, 12.32 g if which was

dissolved in 50 ml of 1.0340N sulfuric acid, producing a mixture that
required 24.60ml of 1.1255 N NaOH.
NITROGEN
DETERMINATION BY THE
KJELDAHL METHOD
NITROGEN DETERMINATION BY THE
KJELDAHL METHOD
 KJELDAHL METHOD
-applied widely in the analysis of proteins of food,
fertilizer, blood, etc.
-decomposed by adding hot conc. sulfuric acid
(converting the bound nitrogen into NH4+ ) which is
then cooled, diluted and made basic.
-liberated NH3 collected in acidic sol’n which is titrated
under neutralization titration.
NITROGEN DETERMINATION BY THE
KJELDAHL METHOD
a. Method I – a macromethod in which the ammonia is distilled into
excess boric acid solution.
- it is used if nitrates or nitrites are not present
- one gram of sample is used.
- If nitrates or nitrites are present – salicylic acid, Na2S2O3 + benzoic
acid is added to facilitate decomposition of the substance.

b. Method II – a semi micromethod in which smaller samples are

employed using a semi micro Kjeldahl apparatus.
- 2-3 milligram of sample is used.
- nitrogen is first liberated by acid digestion
- salicylic acid + nitric acid = nitrosalicylic acid
NITROGEN DETERMINATION BY THE
KJELDAHL METHOD
 Formula:

(N x ml ) acid – (N x ml) base x meq. wt. of N x 100

%N = ---------------------------------------------------------------
Sample weight

 Protein = %N x 6.25
 Meq. wt. of N = M.W. / 1000
Sample Problems:

 1. The ammonia from a 6.20g of sample of

an organic nitrogen compound was
distilled into 50ml of 0.1248N sulfuric acid,
and the mixture was titrated with 22.45 ml
of 0.0965N NaOH. Calculate the %N and
%protein.
Answer:

[(0.1248N) (50ml) – (0.0965N) (22.45ml)] 0.014 x 100

a. %N = ------------------------------------------------------------------
6.2g
%N = 0.92%

b. %protein = 0.92%N x 6.25 = 5.75%

Sample Problem:

 2. Calculate the %CN2H4O (urea) in a 0.5g sample of urea,

15.35ml of 0.4967N NaOH where required in the titration after the
ammonia from the sample had been distilled into 50ml of 0.4861N
H2SO4.

C = 12 N = 14 H=1 O = 16
Meq. wt. urea = (12) (1) + (14) (2) + (1) (4) + (16) (1) = 60 / 2000 =
0.03
Answer:

(N x ml) acid – (N x ml) base x meq. wt. of urea x 100

%CN2H4O = ---------------------------------------------------------
Weight of sample (g)

[(0.4861N x 50ml) – (0.4967N x 15.35ml)] 0.03 x 100

= -----------------------------------------------------------
0.5g
(24.305 – 7.624) (0.03) x 100
= --------------------------------- = 100.08%
0.5g