TCI Sanmar Chemicals LLC Description Version : 01

QC Lab. Department RM-001 Issue Date : 05/06/2008

Raw Salt Page : 1 of 8

1-Determination of Ca & Mg
1-Scope:
This method is applicable to the analysis of Ca & Mg ions in raw salt.

2-Principle:
Ca & Mg are determined volumetrically by selective complexing with standard EDTA

3- Reagents:
1- Standard EDTA solution, (0.02M).

2- Ammonia buffer solution, (6.75 %).

3- Sodium Hydroxide Solution, NaOH (8N).
4- Muroxide indicator, (1%).
5- E.B.T indicator, (1%).

4-Procedure:
1- Weight 12.5 gm from raw salt sample, then dissolve using Distilled water in 250 ml

measuring flask and complete to the mark.

2- Transfer accurately 20 ml from dilute solution into 250 ml volumetric flask, add 5 ml Amm.
Buffer solution and E.B.T indicator, then titrate with standard EDTA (0.02 M) solution (VT, ml).

3- In another conical flask transfer 20ml from the sample, add 3 ml NaOH (8N) and Muroxide

indicator and titrate with standard EDTA (0.02 M) solutions (VCa, ml).

5-Calculations :

Ca % = M x VCa x 50.1 / wt.

Mg%= M xVMg x30.38 / wt.

Factor for Ca & Mg

M x VCa x Mol.wt x 250x100
Ca % =
1000 x 20 x wt. of sample
M x V (Total - Ca) x Mol.wt x 250 x100
Mg% =
1000 x 20 x wt of sample

6-Referance:

Kolthoff,I.M.,Sandell, E.B.,Meehan,E.J.,Bruckenstein,S.,Quantitative Chemical Analysis, P. 805-

806, The Macmillan Co., London (1969 ).

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QC Lab. Department RM-001 Issue Date : 05/06/2008

Raw Salt Page : 2 of 8

2-Determination of Sodium Chloride (NaCl)

1-Scope:
This method is applicable to the analysis of Sodium chloride content in raw Salt.

2-Principle:
This method is based on the titration of excess silver nitrate after adding chloride to a known

amount of silver nitrate in the presence of free nitric acid and Iron (III) ion as indicator with
ammonium thiocyanate.
The addition of thiocyanate solution produces first a precipitate of silver thiocyanate.
Ag+ + SCN- AgSCN

When the reaction is complete, the slightest excess of thiocyanate produces a reddish-brown
coloration, due to the formation of a complex ion:
Fe3+ +n SCN- [Fe (SCN) n] 3-n

3-Reagent:
1- Standard ammonium thiocyanate NH4SCN (0.05N).

2- Standard Silver Nitrate, AgNO3 (0.05 N).

3- Ferric ammonium sulfate (ferric alum), FeNH4 (SO4)2 .12H2O(35%).
4- Nitric Acid, HNO3 (1:1).

4-Procedure:
1- Weight 12.5 gm from raw salt sample, then dissolve using Distilled water in 250 ml

measuring flask and complete to the mark.

2- Transfer 0.5 ml using micropipette from the diluted salt solution in 250 ml conical flask.
3- Transfer accurately 20 ml AgNO3 (0.05 N), add 5 ml HNO3 (1:1).
4- Add 1 ml ferric alum indicator.

5-Titrate the contents with NH4SCN (0.05N) solutions until the colour changes from white
to Buff (V1).
6- Blank is all the last steps with out adding sample (Vb).

5-Calculation:
Vs = Vb-V1

N x Vs x 2922
NaCl (%) =
Wt of sample

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Raw Salt Page : 3 of 8

Factor for Sodium Chloride:

N x Vs x 58.44 x 250 x 100

NaCl (%) =
Wt of sample x 0.5 x 1000

6-Reference:
Kolthoff,I.M.,Sandell, E.B.,Meehan,E.J.,Bruckenstein,S.,Quantitative Chemical Analysis, P. 716-
721, The Macmillan Co., London (1969 ).

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QC Lab. Department RM-001 Issue Date : 05/06/2008

Raw Salt Page : 4 of 8

3-Determination of Sulphate by complexmetric method

1-Scope:
This method is applicable for determination of Sodium Sulphate in Raw Salt.
2-Principles:
Sodium Sulphate is determined by complexmetric titration using barium Chloride to
precipitate Sulphate as Barium Sulphate as shown by the following equation;

Na2SO4 + BaCl2 BaSO4 + NaCl.

Barium Sulphate is then dissolved by Ammonia and EDTA solution then titrate the unreacted
mixture of EDTA and ammonia with MgCl2.

3-Reagents:
1- Standard EDTA solution, (0.02M).

2- Concentrated ammonia solution, (32%).

3- Barium Chloride, BaCl2 (10%).

4- Standard Magnesium Chloride Solution, MgCl2 (0.05M).
5- Concentrated Hydrochloric acid, HCl (32%).

6- Ammonia Buffer solution.

7- E.B.T indicator, (1%).

4-Procedure:
1- Weight 12.5 gm of salt to the nearest 0.1 mg and dissolve in 250ml volumetric flask.
2- In a dry and clean 250 ml beaker transfer 10 ml Solution and add 2ml concentrated HCl.

3- Heat the content of the beaker till boiling, then add 20ml BaCl2 (10%) and let it to cool.
4- Filter the precipitate then place the filter paper in a 250 ml beaker.
5- Dissolve the ppt. using 50ml of EDTA (0.02M) and 20ml concentrated ammonia solution.
6- Boil the solution until the ppt. is dissolved.

7- Titrate the solution using MgCl2 (0.05M) using ammonia buffer and E.B.T. indicator then
record the volume (VMgCl2, ml).

5-Calculations:
MMgCl2 x VMgCl2
VEDTA = 50 -
MEDTA

MEDTA x VEDTA x 240.15

SO4-- (%) =
Wt. of sample

6-Reference:
Vogel, ELBS, A text book of quantitative chemical analysis, 5th edition, 1989.

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4-Determination of Sulphate by gravimetric method

1-Scope:
This method is applicable for determination of Sulphate in brine solution.

2-Principles:
Sulphate is precipitated in a hydrochloric acid medium as barium sulfate by the addition of

barium chloride. The precipitation is carried out near the boiling temperature, and after a
period of digestion the precipitate is filtered, washed with water, ignited and dried, and
washed as barium sulphate.

As shown by the following equation;

Na2SO4 + BaCl2 BaSO4 + NaCl.

3-Reagents:
1- Concentrated hydrochloric acid, HCl (37%).
2- Barium Chloride solution, BaCl2 (10%).

4-Procedure:
1- Weight about 10 gm of raw salt (WS, gm), and transfer to 100 ml measuring flask.
2- After dissolving in distilled water, filter the solution in 250 ml beaker using filter paper

3- Add 2 ml concentrated HCl, heat the content of the beaker till boiling, then add 20 ml BaCl2
(10%) and let the contents to cool.
o
3- Dry the Gouch in an oven at 100 C for 1 hr, then cool in desiccator, weight and record to
nearest 0.1 mg as (W1, gm).

4- Filter the precipitate and wash using plenty of distilled water then place the Gouch in an
o
oven at 100 C for 1 hr.
5- Weight the Gouch and record to nearest 0.1 mg as (W2, gm).

5-Calculations:
(W2 - W1) x 41.14
2-
SO4 (%) =
WS

6-References:
Vogel, ELBS, A text book of quantitative chemical analysis, 5th edition, 1989.

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Raw Salt Page : 6 of 8

4-Determination of Moisture
1-Scope:
This method is applicable for determination of Moisture in Raw Salt.

2-Principle:
In this method we determine moisture by weight loss.

3-Procedure:
1- Take a Petri dish already washed and dried in an oven then Cool in desiccators. Weigh it
accurately. Note down as (W1, gm).
2- Put approximately 20 gm of sample in the dish and weigh it accurately. Let (W2, gm) be the
weight.

Weight of sample = (W2 - W1) gm.

3- Put the Petri dish with its contents in an oven, which has been kept at 140 - 150°C, after 4
hours remove the Petri dish, cool in the desiccators weigh accurately (W3, gm).

The loss of weight = (W2 - W3) gm.

4-Calculation:

Loss of weight
Moisture % = x 100
Weight of sample

5-Reference:
Kolthoff,I.M.,Sandell, E.B.,Meehan,E.J.,Bruckenstein,S.,Quantitative Chemical Analysis, P. 805-
806, The Macmillan Co., London (1969 ).

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Raw Salt Page : 7 of 8

5-Determination of Silica
1-Scope:
This method is applicable to the analysis of Silica in Salt.

2-Principle:
Silicate that exist in the salt react with molybdate ion in acidic medium to form molybdosilicic

acid then reduced by reducing agent to form molybdenum blue that determined by measure
the absorbance at 815 nm.

3-Reagents:
1- Ammonium Molybdate solution, (NH4)6Mo7O24.4H2O (16 %).
2- Oxalic acid, (10%).

3- Reducing agent.
4- UV Standard Solution, Si (1000 ppm).

4-Glass ware:
1- Measuring flask 100 ml.
2- Spectrophotometer measure at 815 nm.

5-Procedure:
A-Sample Procedure
1- In a clean and dry Measuring Flask 100ml, weight about 7 gm of salt and record to nearest
0.1 mg (W, gm). Dissolve the sample with 50 ml distilled water.
2- Add 1 ml of Ammonium Molybdate solution and after 5 minutes add 5 ml of oxalic acid

solution (10%).
3- Introduce 1 ml of the reducing agent and dilute to the mark with distilled water.
4- Measure the absorbance at 815 nm after 20 minute record (Sample OD, nm).

B-Standard Procedure
1-Prepare standard silica in 100 ml from the stock prepared
2- Follow the same procedure and Measure the absorbance at 815 nm after 20 minute record
(Standard OD, nm).

N.B1 Prepare the desirable concentration for standard

N.B2 the pH should be (4.5-5.0).

6-Calculation:
(Sample OD) x (Standard) x 2.139 x 100
Silicate, SiO2 (ppm) =
(Standard OD) x Wt of sample taken
7-Reference:

Kolthoff,I.M.,Sandell, E.B.,Meehan,E.J.,Bruckenstein,S.,Quantitative Chemical Analysis, P. 805-

806, The Macmillan Co., London (1969 ).

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Raw Salt Page : 8 of 8

6-Determination of Iodide
1-Scope:
This method is applicable to the analysis of Iodide in Salt.

2-Principle:
In this method we determine Iodide by UV Spectrophotometer and measure at 640 nm.

3-Reagents:
1- Hydrogen Peroxide solution, H2O2
2- Concentrated Hydrochloric acid, HCl (32%).
3- Standard iodide solution, I- (10 ppm).
4- Brilliant green solution, (0.1%).

5- Toluene, (R.G).

4-Apparatus:
1- Spectrophotometer 2- Separating funnels 250 ml
3- Common Lab equipment 4- Micro liter pipette 1 ml.

5- Procedure:
1- Weigh 12.5 gm of salt and dissolve in distilled water and make up to 50 ml. Transfer in each

of 2 separating funnels. With the micropipette add to one funnel 0.1 ml of the 10 ppm iodide
solution. This one is the standard sample. Then add 1 ml H2O2 (3%) and 0.5 ml. Hydrochloric
acid (33%) to each funnels and mix well.
2- Add 10 ml Toluene in each separating funnel and shake again. After adding of 0.5 ml

brilliant green solution to each funnel shake again vigorously leaves for phase separation.
3- Separate the two layers and measure the toluene phase at 640 nm against pure toluene as
blank.

6-Calculation:
E1 x 10 x 100
I2 (ppb)
(E2 - E1) x 50 x 1.2

Where: E1 - Extinction of the sample E2 - Extinction of the sample and standard

7-Reference:
Kolthoff,I.M.,Sandell, E.B.,Meehan,E.J.,Bruckenstein,S.,Quantitative Chemical Analysis, P. 805-

806, The Macmillan Co., London (1969 ).

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