4 sop spectrophotometric iron content

7/26/2019 4 SOP Spectrophotometric Iron Content

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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 ea!er. "dd approximately #00 ml distilled $iron free &ater. 'eat

on a hot plate till all the (rystals are dissol)ed. "fter (ool do&n transfer

the solution to all )olumetri( *as! &ith distilled &ater and +ll up to the

mar!.

,uer Solution $0. / potassium iphthalate solution

otassium iphthalate is also !no&n as potassium hydrogen phthalate

$'.

2issol)e 0.4#g of ' in approximately #00 ml distilled &ater &ith

heating. "fter (ool do&n5 transfer the solution to all )olumetri( *as! &ith

distilled &ater. 2ilute to the mar! &ith distilled &ater.

Standard ron Solutions:

Standard solution:

2issol)e 7.013 g of reagent grade ferrous ammonium sulphate

hexahydrate.

$8' 9e$S 6 ' is freshly distilled &ater (ontaining 3 ml of

(on(entrated sulpuri( a(id and dilute the solution to 1 ; in a )olumetri(

*as!.


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Process

Manual


Standard @on(entration @ru)es:

repare solution y pipetting aliAuots of the &or!ing solution $a((ording to

the tale elo& into a # ml )olumetri( *as!.

"dd 10 ml of 0.3% phenathroline solution and # ml of uer solution to

the *as! and dilute to the mar! &ith distilled &ater.

ppm 9e.

@on(entration of Std. ?olume of 9e sto(!

solution to e used$ml

,lan! -- ppm 0.# ppm 1.06 ppm 1.#4 ppm .010 ppm .#

/easure the asoran(e of ea(h of the solutions at 3>6 mm. Bse

lan! for (aliration. lot the (one. ?s asoran(e (ur)es for

asoran(e at 3>6 mm.

n(lusi)e of un!no&n samples:

Sample aout #0 g of iron-9orti+ed salt and mill the sample in a

(oee grinder. Weigh out aout 10 g of the milled sample

$re(ording the &eight into #0 ml digestion tue. "dd aout 0 ml

of distilled &ater.

"(idity the solution &ith 1 ml of sulphuri( a(id and oil the solution

for 10 minutes.'andle a(id (arefully and al&ays add a(id to the &ater. /onitor

digestion tues (arefully.

'o& the sample to (ool thoroughly and transfer the solution to a

100 ml )olumetri( *as!. 2ilute to the mar! &ith distilled &ater. Cou

may see some (loudy insolule material.

2o(. Ref: S = 0> ?ersion : 1.0 ssue 2ate:0#=0=07 age of


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Process

Manual


Either the solution through +lter paper and pipette 1 ml of the

litrati( into a # ml )olumetri( *as!.

"dd 10 ml of 0.3% phenathroline solution and # ml of uer

solution to the *as! and dilute to the mar! &ith distilled &ater.

Read asoran(e of the sample at 3>6 mm for total iron.

Calculations:

2etermine iron (ontent of sample from asoran(e at 3>6 mm from

(aliration (ur)e prepared.

Read asoan(e of (omplexed sample at 3>6 mm.

2etermine the (on(entration of total iron from standard

(on(entration (ur)e at 3>6 mm.

Iron content in Salt:

9e (ontent in salt $ppm 9e D @on(. of iron in (omplexed sample $ug=ml#00

------------------------------------------------------------

------------ mass of salt sample $g

;aoratory 'ard&are ReAuired $"part from B? Spe(trophotometer

"nalyti(al alan(e

; ?ol 9las! F 3

100 ml ?ol. *as!s F 3

# ml ?ol. *as!s F 6

Stoppers for the *as!s

10 ml pipette

# ml graduated pipette

ml graduated pipette

600 ml ea!er F 1

2o(. Ref: S = 0> ?ersion : 1.0 ssue 2ate:0#=0=07 age 3 of


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Process

Manual


100 ml ea!ers F

#00 ml ea!ers F

@oee grinder or small mill for milling #0 g of salt sample

#0=7# ml digestion tues $

4 sop spectrophotometric iron content

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