TAMIL NADU SALT CORPORATION LIMITED.

Process
Manual

SOP-09 : SPECTROPHOTOMETRIC IRON CONTENT

SPECTROPHOTOMETRIC IRON CONTENT DETERMINATION IN
SALT

Experimental
Reagent Solutions:
0.3% 1.10-phenunthroline solution
Weigh out 3 g of reagent grade 1.10-phenanthroline monohydrate into a
600 ml beaker. Add approximately 500 ml distilled (iron free) water. Heat
on a hot plate till all the crystals are dissolved. After cool down transfer
the solution to all volumetric flask with distilled water and fill up to the
mark.
Buffer Solution (0.2 M potassium biphthalate solution)
Potassium biphthalate is also known as potassium hydrogen phthalate
(KHP).
Dissolve 40.85g of KHP in approximately 500 ml distilled water with
heating. After cool down, transfer the solution to all volumetric flask with
distilled water. Dilute to the mark with distilled water.
Standard Iron Solutions:
Standard solution:
Dissolve

7.0213 g

of

reagent grade

ferrous ammonium sulphate

hexahydrate.
(NH 4)2 Fe(SO 4)2 6 H 2 O) is freshly distilled water containing 3 ml of
concentrated sulpuric acid and dilute the solution to 1 L in a volumetric
flask. This is the sock solution.
Pipetic 10 ml of the above solution into a 100 ml volumetric flask and
dilute to the mark with distilled water. This is the working solution.
The above solution will result in a solution with an iron content of 0.100
mg per ml (100 ppm).
Doc. Ref: SOP / 09

Version : 1.0

Issue Date:05/02/07

Page 1 of 4

TAMIL NADU SALT CORPORATION LIMITED.

Process
Manual

SOP-09 : SPECTROPHOTOMETRIC IRON CONTENT

Standard Concentration Cruves:

Prepare solution by pipetting aliquots of the working solution (according to
the table below) into a 25 ml volumetric flask.
Add 10 ml of 0.3% phenathroline solution and 5 ml of buffer solution to
the flask and dilute to the mark with distilled water.
The solutions should range in concentration from 0 ppm Fe to 19 ppm Fe.
Concentration of Std.

Volume

of

Fe

stock

solution

to

be

used

(ml)
-0.5
1.0
1.5
2.0
2.5

Blank
2 ppm
4 ppm
6 ppm
8 ppm
10 ppm

Measure the absorbance of each of the solutions at 396 mm. Use

blank for calibration.

Plot the cone.

Vs absorbance curves for

absorbance at 396 mm.

Inclusive of unknown samples:
Sample about 50 g of iron-Fortified salt and mill the sample in a
coffee grinder.

Weigh out about 10 g of the milled sample

(recording the weight) into 50 ml digestion tube. Add about 40 ml

of distilled water.
Acidity the solution with 1 ml of sulphuric acid and boil the solution
for 10 minutes.
Handle acid carefully and always add acid to the water.

Monitor

digestion tubes carefully.

How the sample to cool thoroughly and transfer the solution to a
100 ml volumetric flask. Dilute to the mark with distilled water. You
may see some cloudy insoluble material.
Doc. Ref: SOP / 09

Version : 1.0

Issue Date:05/02/07

Page 2 of 4

TAMIL NADU SALT CORPORATION LIMITED.

Process
Manual

SOP-09 : SPECTROPHOTOMETRIC IRON CONTENT

Either the solution through filter paper and pipette 1 ml of the

litratic into a 25 ml volumetric flask.
Add 10 ml of 0.3% phenathroline solution and 5 ml of buffer
solution to the flask and dilute to the mark with distilled water.
Read absorbance of the sample at 396 mm for total iron.
Calculations:
Determine iron content of sample from absorbance at 396 mm from
calibration curve prepared.
Read absobance of complexed sample at 396 mm.
Determine

the

concentration

of

total

iron

from

standard

concentration curve at 396 mm.

Iron content in Salt:
Fe content in salt (ppm Fe) = Conc. of iron in complexed sample (ug/ml)*
2500
----------------------------------------------------------------------mass of salt sample (g)
Laboratory Hardware Required (Apart from UV Spectrophotometer)

Analytical balance

IL Vol Flask X 3

100 ml Vol. flasks X 3

25 ml Vol. flasks X 6

Stoppers for the flasks

10 ml pipette

5 ml graduated pipette

2 ml graduated pipette

600 ml beaker X 1

Doc. Ref: SOP / 09

Version : 1.0

Issue Date:05/02/07

Page 3 of 4

TAMIL NADU SALT CORPORATION LIMITED.

Process
Manual

SOP-09 : SPECTROPHOTOMETRIC IRON CONTENT

100 ml beakers X 4

500 ml beakers X 4

Coffee grinder or small mill for milling 50 g of salt sample

50/75 ml digestion tubes (Thickened glass)

Aluminum blocks for digestion tubes (can be made by drillin

g holes of appropriate size into an aluminum blocks 2
thick)

Hot plate base should be sufficient to hold 3-6 tubes

Bottles to store solutions.

Spatula

Safety goggles

Tongs or eve mitts for handling hot glass tubes

Graduated cylinder 50 mo X 1

Doc. Ref: SOP / 09

Version : 1.0

Issue Date:05/02/07

Page 4 of 4