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Holding Company for Drinking water and Waste water CWC/MR/Test P/25
Cairo Water Company Issue No.: 01
Laboratories & Research Sector
Quality Control Administration Issue Date: 1/ 4/2018
Test Procedure
Page No. : 1 / 8
Determination of Sulfate
TITLE: Determination of Sulfate
Name Signature
Prepared by Mai Abdullah Mai Abdullah
Saeed Ibrahim Saeed Ibrahim
Reviewed by
Warda Adel Warda Adel
Final reviewed by Mai Sadek Mai Sadek
Approved by Atef Dokhan Atef Dokhan
Holding Company for Drinking water and Waste water CWC/MR/Test P/25
Cairo Water Company Issue No.: 01
Laboratories & Research Sector
Quality Control Administration Issue Date: 1/ 4/2018
Test Procedure
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Determination of Sulfate
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Holding Company for Drinking water and Waste water CWC/MR/Test P/25
Cairo Water Company Issue No.: 01
Laboratories & Research Sector
Quality Control Administration Issue Date: 1/ 4/2018
Test Procedure
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Determination of Sulfate
CONTENTS
1. Purpose.
2. Scope and Application.
3. Principle.
4. Responsibility.
5. Environment conditions.
6. Equipment.
7. Reagents.
8. Precautions.
9. Sample handling and Storage.
10. Interference.
11. Procedure.
12. Calculation
13. Assuring the test results.
14. Criteria.
15. Test report.
16. References.
Edited by Foxit Reader
Copyright(C) by Foxit Software Company,2005-2008
For Evaluation
Holding Company for Drinking Only.
water and Waste water CWC/MR/Test P/25
Cairo Water Company Issue No.: 01
Laboratories & Research Sector
Quality Control Administration Issue Date: 1/ 4/2018
Test Procedure
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Determination of Sulfate
1. PURPOSE
This procedure applied for determination of Sulfate (SO42-) using Turbidimeter according to
SMWW Standard Methods for the Examination of Water and Wastewater 23rd Edition, Method
No. 4500- SO42- E. (Turbidimetric Method).
2. SCOPE AND APPLICATION
2.1 This procedure is applicable to all types of water sample such as raw water, water during
intermediate stages of the treatment, drinking water and ground water samples as well as
external or internal samples.
2.2 This procedure is applicable in the range of 1 to 40 mg SO42-/L
2.3 The minimum detectable limit is approximately 1mg SO42- /L.
3. PRINCIPLE
Sulfate ion (SO42-) is precipitated in an acetic acid medium with barium chloride (BaCl2) so as
to form barium sulfate (BaSO4) crystals of uniform size. Light scattering of the BaSO4
suspension is measured by a Turbidimeter and the SO42- concentration is determined by
comparison of the reading with a standard curve.
4. RESPONSIBILITY
All Chemists are responsible for carrying out and understanding the contents of this Test
Procedure.
5. ENVIRONMENT CONDITIONS
Make determination at room temperature; variation over a range of 10°C will not cause
appreciable error.
Name and Model
6. EQUIPMENT
6.1 Magnetic stirrer with variable speed so that it can be held constant just below splashing.
Use identical shape and size magnetic stirring bars.
6.2 Turbidimeter. HACH MODEL 2100N
6.3 Stopwatch.
6.4 Measuring spoon, capacity 0.2 to 0.3 ml.
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water and Waste water CWC/MR/Test P/25
Cairo Water Company Issue No.: 01
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Quality Control Administration Issue Date: 1/ 4/2018
Test Procedure
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Determination of Sulfate
7. REAGENTS
7.1 Buffer solution A (required when the sample SO42- concentration is between 10 - 40mg/L):
Dissolve 30g magnesium chloride MgCl2 • 6H2O, 5g sodium acetate CH3COONa .3H2O, 1g
potassium nitrate KNO3, and 20ml acetic acid, CH3COOH (99%), in 500ml distilled water
and make up to 1L.
7.2 Buffer solution B (required when the sample SO42- concentration is less than 10mg/L):
Dissolve 30g magnesium chloride MgCl2 • 6H2O, 5g sodium acetate CH3COONa .3H2O, 1g
potassium nitrate KNO3, 0.111 g sodium sulfate, Na2SO4,and 20ml acetic acid, CH3COOH
(99%), in 500ml distilled water and make up to 1L. Remove
7.3 Barium chloride (BaCl2), crystals, 20 to 30 mesh: In standardization, uniform turbidity is
produced with this mesh range and the appropriate buffer.
7.4 Standard sulfate solution: Prepare a standard sulfate solution as described :
7.4.1 Dilute 10.4ml standard 0.02 N H2SO4 titrant specified in Alkalinity, to 100 ml with
distilled water. (1 ml = 100 µg SO42-)
7.4.2 Or by dissolve 0.1479 g anhydrous Na2SO4 in distilled water and dilute to 1L.
(1 ml = 100 µg SO42-)
8. PRECAUTIONS
8.1 Every precaution should be taken to ensure the cleanliness of sample containers, as well as
other materials and apparatus that come in contact with the sample.
8.2 Use reagents low in SO42-, and SO42- -free distilled water.
8.3 Volumetric measurement of sample and reagent is extremely important to analytical
accuracy.
8.4 Above 40mg/L accuracy decreases and BaSO4 suspensions lose stability.
8.5 Keep speed of stirring constant and use the same magnet shape for each run of samples and
standards and adjust it to prevent splashing.
8.6 Draw the fresh calibration curve with change of reagents or chemicals.
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water and Waste water CWC/MR/Test P/25
Cairo Water Company Issue No.: 01
Laboratories & Research Sector
Quality Control Administration Issue Date: 1/ 4/2018
Test Procedure
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Determination of Sulfate
9. SAMPLE HANDLING AND STORAGE
9.1 Collect samples use glass or plastic containers and examine them as soon as possible after
collection.
9.2 Minimum sample size for Sulfate test is 100ml, in grab or composite sample.
9.3 In the presence of organic matter certain bacteria may reduce SO 42- to S2- to avoid this,
store samples at 4°C.
9.4 Store samples at ≤ 6°C for 28 day (Maximum storage recommended).
10. INTERFERENCE
10.1 Color or suspended matter in large amounts will interfere. Some suspended matter may be
removed by filtration.
10.2 Silica in excess of 500 mg/L will interfere.
10.3 waters containing large quantities of organic material it may not be possible to precipitate
BaSO4 satisfactorily.
11. PROCEDURE
11.1 Preparation of calibration curve:
11.1.1 Prepare a series of Sulfate standards by accurately measuring the calculated
volumes of standard Sulfate solution into 100ml distilled water.
St. No. Volume of standard Volume of [Link] Conc. of standard
1 5 ml 95ml 5 mg/l
2 10ml 90ml 10 mg/l
3 15ml 85ml 15 mg/l
4 20ml 80ml 20 mg/l
5 25ml 75ml 25 mg/l
6 30ml 70ml 30 mg/l
7 35ml 65ml 35 mg/l
8 40ml 60ml 40 mg/l
11.1.2 Space standards at 5mg/L increments in the 0 - 40 mg/L sulfate range.
11.1.3 Transfer preparing standards into a 250ml Erlenmeyer flask. Add 20ml buffer
solution and mix in stirring apparatus.
Holding Company for Drinking water and Waste water CWC/MR/Test P/25
Cairo Water Company Issue No.: 01
Laboratories & Research Sector
Quality Control Administration Issue Date: 1/ 4/2018
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Determination of Sulfate
11.1.4 While stirring, add a spoonful of BaCl2 crystals and begin timing immediately.
Stir for 60 ± 2 s at constant speed.
11.1.5 After stirring period has ended, pour solution into cell of turbidimeter and
measure turbidity at 5 ± 0.5 min.
11.1.6 Prepare a standard curve by plotting turbidity of standards against SO42-
Concentration.
11.2 Sample analysis:
11.2.1 Measure 100ml sample, or a suitable portion made up to 100ml, into a 250ml
Erlenmeyer flask.
11.2.2 Add 20ml buffer solution and mix in stirring apparatus.
11.2.3 While stirring, add a spoonful of BaCl2 crystals and begin timing immediately.
Stir for 60 ± 2 s at constant speed.
11.2.4 After stirring period has ended, pour solution into cell of turbidimeter and
measure turbidity at 5 ± 0.5 min.
11.3 Correction for sample color and turbidity:
11.3.1 Correct for sample color and turbidity by running blanks to which BaCl2 is not
added.
11.3.1 Determine SO42- concentration directly from the calibration curve after
subtracting sample turbidity before adding BaCl2.
12. CALCULATION
Read mg SO42- directly from the calibration curve.
13. ASSURING THE TEST RESULTS
13.1 The laboratory apply internal quality control program that specifies the
Measures required producing data with known precision and accuracy.
13.2 This program consists of control charts (X & R Charts)
13.3 The laboratory will construct the charts according to the work instruction
CWC/MR/ Work. I /01
Holding Company for Drinking water and Waste water CWC/MR/Test P/25
Cairo Water Company Issue No.: 01
Laboratories & Research Sector
Quality Control Administration Issue Date: 1/ 4/2018
Test Procedure
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Determination of Sulfate
14. CRITERIA
The acceptance and rejection criteria of the samples according to the Egyptian Standards
& Regulations (No. 458) for the year 2007, the maximum value of Sulfate ≤ 250 mg/l.
15. TEST REPORT
The laboratory has different test reports according to required tests, for Sulfate test using form
N4/LAB.
16. REFERENCES
SMWW Standard Methods for the Examination of Water and Wastewater 23rdEdition, 2017,
Method No. 4500- SO42- E.
