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Sodium Hydrogen Sulphide Determination

Author: Axis House Pty Ltd

Doc. No: AHSOP017

2017
1 Contents
2 Purpose: .......................................................................................................................................... 2
3 Scope: .............................................................................................................................................. 2
4 Prerequisites: .................................................................................................................................. 2
5 Abbreviations: ................................................................................................................................. 2
6 Responsibilities: .............................................................................................................................. 2
7 Safety: ............................................................................................................................................. 2
8 Determination of Total Sulphide Content in the sample using Iodometric Titration: .................... 3
9 Sample Preparation: ....................................................................................................................... 3
10 Reagents and Apparatus: ................................................................................................................ 3
11 Iodometric Titration Procedure: ..................................................................................................... 4
12 Total Sulphide Calculation: ............................................................................................................. 4
13 Determination of Sodium Sulphide Content in the sample by Acid- Base Titration Method......... 4
14 Reagents and Apparatus: ................................................................................................................ 5
15 Acid-Base Titration Procedure: ....................................................................................................... 5
16 Total Sodium Sulphide Calculation: ................................................................................................ 5
17 Total Sodium Hydrogen Sulphide Calculation:................................................................................ 5

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2 Purpose:
The Commercial flake products of Sodium Hydrogen Sulphide is made up of Sulphide components
and Sodium Sulphide. These Sodium Hydrogen Sulphide (NaHS) flakes are used in mineral processes
and affects the Sulphidisation outcome of Controlled Potential Sulphidisation.

Axis House has developed two titration methods to quantify each of these sulphide species.

3 Scope:
This procedure applies to the purpose of determining the total Sulphide content, Sodium Sulphide
content and determining the percentage of Sodium Hydrogen Sulphide in the NaHS flakes.

4 Prerequisites:
N/A

5 Abbreviations:
NaHS – Sodium Hydrogen Sulphide

Na2S – Sodium Sulphide

6 Responsibilities:
The Lab Analyst/Operator should:

 Be trained the on the following procedure before proceeding the test.


 Work with the relevant acid in a fume cupboard.

7 Safety:
Analyst must ensure that he/she adheres to the following safety instructions while doing the
following procedure:

 To always wear a lab coat.


 Ensure that safety goggles are worn at all times.
 Correct safety shoes are worn.

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8 Determination of Total Sulphide Content in the sample using
Iodometric Titration:
The purpose of the Iodometric Titration is to determine the Total Sulphide content in the NaHS
flakes.

The total Sulphide in the sample is defined here as a combination of Sodium Hydrogen Sulphide and
Sodium Sulphide.

Both sulphide chemicals react with Iodine (I2) quantitatively as per Equation 1 and Equation 2 that
gives a basis for titration measurements:

Equ. 1 - NaHS + I2 = S + NaI + HI

Equ. 2 - Na2S + I2 = S + 2NaI

The Iodine consumption by the sample is then determined by the process of back titration using the
Thiosulphate titration procedure shown in Equation 3.

Equ. 3 - 2Na2S2O3 + I2 = Na2S4O6 + 2NaI

9 Sample Preparation:
The flake samples should be dissolved in distilled water at a strength of 20% with respect to
percentage prior to titration.

10 Reagents and Apparatus:


 0.1M Sodium thiosulphate Solution
 0.05M Iodine (I2) solution
 5M HCl Solution
 Starch Indicator
 50ml Burette
 50ml Pipette
 200ml conical flask
 100ml measuring cylinder

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11 Iodometric Titration Procedure:
1. Fill the burette with 0.1M Sodium Thiosulphate solution
2. Accurately weigh 0.4 – 0.5g weight of the prepared NaHS solution into a 200ml conical
flask.
3. Pipette out 50ml of the 0.05M Iodine solution and add it into the NaHS solution.
4. Close the flask with the stopper and thoroughly mix the contents for 30 seconds.
5. Add 30ml of 5M HCL to the flask and immediately close it to prevent loss of hydrogen
sulphide
6. Mix up contents in the flask for 30 – 60 seconds
7. Add a small amount 0.1 -0.2g of starch indicator into the solution.
8. Start the titration by adding the thiosulphate solution from the burette.
9. Continue the titration until the dark colour mixture turns colourless.
10. To determine the blank for this titration repeat the above procedure but do not add the
sample (NaHS).

12 Total Sulphide Calculation:


Use the following expression to calculate the percentage Sulphide in the sample.

%Total sulphide (S2-) = [(V0-Vs) * (0.1/1000) * 0.5 * (Mm sulphur) * 100] / sample mass

= [(V0-Vs) * 0.1603] / sample mass

The above total sulphide expression is measured in a 20% solution. Therefore, in the actual flake the
expression would be % total Sulphide * 5.

13 Determination of Sodium Sulphide Content in the sample by Acid-


Base Titration Method.
The Na2s content is measured by titration using standard HCl acid with phenolphthalein indicator.
The end point is reached when the solution changes from pink to colourless.

The chemical reaction occurs as follows:

Eq.5 - Na2S + HCl = NaHS + NaCl (aq)

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14 Reagents and Apparatus:
 50ml Burette
 50ml Pipette
 200ml conical flask
 100ml measuring cylinder
 0.1M HCl
 Phenolphthalein indicator
 Deionised Water.

15 Acid-Base Titration Procedure:


1. Fill up the 50mL burette with 0.1M HCl solution.
2. Accurately weigh 0.2 – 0.5g sulphide sample in a conical flask and dissolve it in 30mL of
distilled water.
3. Add a few drops of indicator.
4. Start titrating by adding HCl solution from the burette.
5. Stop titrating when the solution changes from red to colourless (initial colour).

16 Total Sodium Sulphide Calculation:


Use the following expression to calculate % Na2S in the sample:

%Na2S = [(Vol. of HCl) * (0.1/1000) * (Mm Na2S) * 100] / sample mass

= [(Vol. of HCl) * (0.1/1000) * (78.06) * 100] / sample mass

= [(Vol. of HCl) * 0.7806] / sample mass

17 Total Sodium Hydrogen Sulphide Calculation:


From the value of total sulphide and Na2S the %NaHS can be calculated as follows:

%NaHS = [Total sulphide mole – Na2S] * (Mm of NaHS)

Determination of % Sodium Hydrogen Sulphide


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