Subject:

Quality Management

Submitted By:
Tasneem Rasheed
Roll # DPRF15E094

Submitted To:
DETERMINATION OF Sir Dr. Zubair

SELENIUM

College of Pharmacy University of Sargodha, Sargodha.

 Selenium Determination

Introduction:
Selenium is a chemical element with the symbol Se and the atomic number 34 and atomic mass
number is 78.96. It is metalloid in 1817 Johns Jacob Berzelius isolated and identified selenium.

Chemical properties:
 Essential trace element
 Component of glutathione peroxidase.
 4 oxidative states:
1. Elemental se (0)
2. Selenide (-2)
3. Selenite(+4)
4. Selenate (+6)

Inorganic forms: Selenate, selenite (found in water)

Organic forms: selenomethionine, selenocysteine (found in veggies and cereals)

Physical properties:
 Selenium is found in various forms ranging from a grey metallic to a reddish glassy
appearance.
 It is found in various rocks, minerals, coal and oil.
 Melting point is 221 ̊C.
 Boiling point is 685 ̊C.
 Heavey metal selenides(-2) and elemental selemiun are insoluble in water.
 Inorganic alkali selenites (+4) and selenates (+6) are soluble in water.

Method of Determination:
1. STOCK solution:
Dissolve 40mg of selenium in 100mL dilute nitric acid in a 1000mL volumetric flask, warm
it on steam bath for effective solution, add water to make up the volume and mix it. Pipet
5mL of this solution into a 200ml volumetric flask, add water to volume and mix.
 2. Diaminonaphthalene solution:
Dissolve 100mg of 2, 3 diaminonaphthalene and 500mg of hydroxylamine hydrochloride
in 0.1N hydrochloric acid to make 100 mL. Prepare this solution on the day of use.

3. Standard solution:
Pipet 6 mL of stock solution into a 150 mL beaker and add 25 mL of dilute nitric acid and
25 mL of water.

4. Test Solution:
Clean combustion of the test material is important for conducting the test for this addition
of magnesium oxide results in thorough combustion and reduce soot formation using a
1000 mL combustion flask and using 25 mL of dilute nitric acid as absorbing liquid, using
a test specimen weighing 100mg to 200mg, unless directed in individual monograph. Upon
completion of combustion, place a few mL of water in the cup, loosen the stopper and rinse
the stopper, the specimen holder and the sides of the flask with about 10mL of water.
Transfer the solution with aid of 20mL of water to a 150mL beaker and heat gently to
boiling temperature for 10 minutes and allow the solution to cool at room temperature.

Procedure:
 Treat the standard solution, the test solution and the reagent blank consisting of 25mL of
dilute nitric acid and 25ml of water.
 Add ammonium hydroxide solution to adjust to a pH of 2.0±0.2.Dilute with water to 60mL
and transfer to low actinic separator with aid of 10mL of water, adding the 10mL of risings
to the separator.
 Add 200mg of hydroxylamine hydrochloride, swirl to dissolve, immediately add 5mL of
diaminonphthalene solution, insert the stopper and swirl to mix.
 Allow the solution to stand at room temperature for 100 minutes.
 Add 5mL of cyclohexane, shake vigorously for 2 minutes, and allow the layers to separate.
 Discard the aqueous layer and centrifuge the cyclohexane extract to remove any dispersed
water.
 Determine the absorbance of cyclohexane extract of the test solution and the standard
solution in a 1cm cell at the wavelength of maximum absorbance at about 380nm, with a
suitable spectrophotometer, using the cyclohexane extract of reagent blank as blank and
compare the absorbance.
 The absorbance of the test solution is not greater than the that of standard solution where a
200mg specimen has been taken, or is not greater than one half of the standard solution
where a 100mg test specimen has been taken.
Significance of selenium:
Medical use:
 Dietary supplement.

Application:
 Manufacturing of ceramics, glass, pigments, semiconductors and steel.
 Use in photography and pharmaceutical production.