SALT

(Volhard Method)

PRINCIPLE

To determine salt, an analysis is made for total chlorides and

the result is expressed as sodium chloride. The method involves
the digestion of the sample with concentrated nitric acid and
oxidation of any remaining organic matter with potassium
permanganate. The dissolved chlorides in the sample are
precipitated with excess silver nitrate as silver chloride, and
the excess silver ions backtitrated with thiocyanate using ferric
alum as the indicator. When all the excess silver ions have
reacted with thiocyanate, any slight excess of thiocycnate will
react with ferric alum to form a red-coloured complex (ferric
thiocyanate) at the end-point. n excess of thiocyanate may react
with the precipitated silver chloride, since the solubility
product of silver thiocyanate is !.!" that of silver chloride.
The addition of nitroben#ene, diethyl ether or acetone overcomes
this difficulty by coating the precipitated silver chloride and
thereby withdrawing it from reaction with the thiocyanate
solution. $itroben#ene is toxic and its use is best avoided.

 APPARATUS
". %ipettes and burettes.
&. 'aboratory glassware.

REAGENTS
". erric alum indicator saturated a*ueous solution of reagent
grade ferric ammonium sulphate (+&&).

&. ilver nitrate solution, !.&! $ - dissolve "/.!0 g of silver

nitrate, (previously dried at ""!12) in distilled water and
dilute to " litre. tandardi#e (using excess silver nitrate
solution) against !."! $ sodium chloride (3.403 g per litre).

5. %otassium thiocyanate solution (!."!!$) - dissolve 6./& g of

reagent grade potassium thiocyanate in distilled water, and
dilute to one litre.

0. 2oncentrated nitric acid.

3. $itric acid ("7").
8. $itroben#ene.
/. %otassium permanganate solution (39).

PROCEDURE
ccurately weigh appropriate amount (about &-5 g) of sample into
a 5!! ml :rlenmeyer flask. (or shrimp paste or other highly
salted foods, weigh about 3 g into &3! ml volumetric flask and
digest for about one hour in water bath to dissolve the salt.
ilter through $o. " filter paper. Take appropriate amount of
this filtrate) (e.g. for shrimp paste, take "! ml). dd &3 ml of
!."!!$ silver nitrate solution, swirl flask until sample and
solution are in intimate contact. dd "3 ml of concentrated
nitric acid. (The silver nitrate solution must be added first,
followed by the concentrated nitric acid. The order of addition
ensures complete precipitation of the chlorides. +f nitric acid
is added first, loss of chloride by volatili#ation as hydrogen
chloride could occur, since hydrogen chloride has a far greater
vapour pressure than nitric acid.)

;oil in a fume hood until dissolved and add potassium

permanganate solution (39) until colour disappears and the
solution becomes colourless. (hould too much potassium
permanganate be accidently added, colour removal can be effected
by the addition of small *uantities of sugar). dd about "3 to &3
ml of distilled water, boil for 3 mins. 2ool and dilute to about
"3! ml with distilled water. dd about " ml nitroben#ene, & ml of
ferric alum indicator and shake vigorously to coagulate the
precipitated silver chloride. Titrate the excess silver nitrate
with !."!! $ potassium thiocyanate solution to a permanent light
brown end-point. 2arry out a blank titration containing &3.! ml
of !."!!$ silver nitrate solution, & ml ferric alum indicator and
"3 ml of ("7") nitric acid with !."!!$ potassium thiocyanate.

or highly salted foods re*uiring dilution, multiply the above

calculation by &3!<ml ali*uot taken for analysis.

REFERENCE
fficial =ethods of nalysis of the 2, "640, 5&.!55, and other
references under other commodity headings.