OBJECTIVE

To determine SO4-S in water sample by turbldimetric method-Tabatabai

INTRODUCTION
Sulfate (SO4) can be found in almost all natural water. The origin of most sulfate compounds
is the oxidation of sulfite ores, the presence of shales, or the industrial wastes. Sulfate is one
of the major dissolved components of rain. High concentrations of sulfate in the water we
drink can have a laxative effect when combined with calcium and magnesium, the two most
common constituents of hardness. Bacteria, which attack and reduce sulfates, form hydrogen
sulfide gas (H2S). As groundwater moves through the soils and rocks containing sulfate
minerals, some of it may get dissolved into the water. Some minerals that contain sulfate are
sodium sulfate (Glauber's salt), magnesium sulfate (Epsom salt), and calcium sulfate
(gypsum).
Sulfur-reducing bacteria, which use sulfur as an energy source, are the primary producers of
large quantities of hydrogen sulfide. These bacteria chemically change natural sulfates in
water to hydrogen sulfide. Sulfur-reducing bacteria live in oxygen-deficient environments
such as deep wells, plumbing systems, water softeners and water heaters.
Sulfate minerals can cause scale build up in water pipes similar to other minerals and may be
associated with a bitter taste in water. Elevated sulfate levels in combination with chlorine
bleach can make cleaning clothes difficult.

PRINCIPLE
In aliquot of sample of water, BaSO4 turbidity is developed in an acidic medium by adding 1
ml of 0.5% BaCl2.2H2O reagent in 0.3% gelatin solution. The BaSO4 turbidity developed is
stabilized by the gelatin and its absorbance is measured 30 minutes after developing turbidity
at 420 nm wave length on a spectrophotometer.

APPARATUS/REAGENTS

Apparatus
Volumetric flasks, graduated pipette, 500 ml capacity beaker, spectrophotometer.

Reagents
(i) Distilled water-free from sulphur.
(ii) 10.0 N Hydrochloric acid. Dilute 218.2 ml of cone HCl (AR) to 250 ml with
distilled water.
(iii) 0.5 N Hydrochloric acid. Dilute 5.0 ml of 10 N HCl to 100 ml with distilled water
(iv) 0.5% Barium chloride solution in 0.3% gelatin solution. Dissolve 0.6g of gelatine
in 200 ml of warm (60-70° C) distilled water. Thereafter, place the solution in a
refrigerator at 4°C, and allow it to stand for 16 hours. Then, remove the semi-
gelatin from the refrigerator and allow it to cool to room temperature and add 1.0
g BaCl2.2H2O crystals and shake the contents until BaC12 crystals arc dissolved.
Store the solution in a refrigerator. Remove the reagent from the refrigerator and
let it stand for 2 hours at room temperature before use.
(v) 1000 ppm SO4-S solution. Dissolve 5.4438g of K2SO4in distilled water and dilute
the solution to 1000 ml mark with distilled water.
 (vi) 0 to 20 ppm SO4-S standards. Pipette 0, 5, 10, 15 & 20 ml of 1000 ppm SO4-S
solution into separate 1000 ml volumetric flasks and dilute each SO4-S standard to
1000 ml mark with distilled water to obtain 0 to 20 ppm SO4-S solution.

PROCEDURE

1. Development of BaSO4 turbidity with an aliquot of sample water. Pipette 20.0 ml

aliquot of sample water into a 50 ml volumetric flask. Then add 2.0 ml of 0.5 N HCI.
Swirl to mix the contents, and add 1.0 ml of BaCl2 gelatin reagent. Stopper and mix
the contents. Similarly run a blank taking 20.0 ml of distilled water and following the
procedure as for sample aliquot beginning with the addition of 2 ml of 0.5 N HCI.

2. Measurement of absorbance of BaSO4turbidity developed with aliquot of sample

water. Prior to measurement of absorbance, switch on the spectrophotometer adjusting
wavelength knob to 420 nm or photoelectric colorimeter fitted with 420 nm (blue)
filter and the cuvette or test tube filled with distilled water placed in the socket
provided and allow the instrument to warm for 10 minutes.
Thereafter, measure the absorbance of BaSO4 turbidity developed in aliquot of
sample water adjusting O absorbance with the turbidity developed in blank with 20 ml
of distilled water.

3. Development of BaSO4 turbidity with SO4-S standards containing 0 to 400 μg SO4-S.

Transfer 0, 100, 200, 300 and 400 μg SO4-S by pipetting 20 ml of 0-20 ppm SO4-S
standards into separate 50 ml volumetric flasks and then proceed as described in step l
of procedure beginning with the addition of 2.0 ml of 0.5 N HCI.

4. Measurement of absorbance of BaSO4 turbidity developed with 0-400 μg SO4-S.

Adjust 0 absorbance with BaSO4 turbidity developed with 0 μg SO4-S on a
spectrophotometer or else on a photoelectric colorimeter at 420 nm wave length, and
measure the absorbance of the subsequent standards i.e. BaSO4turbidity developed
with 100 to 400 μg SO4-S.

5. Preparation of the standard calibration curve. On a linear scale graph paper, let the
ordinate be the scale for absorbance and abscissa be the scale for μg SO4-S taken for
developing turbidity. Then, plot the value of absorbance corresponding to the μg SO4-
S taken for developing BaSO4 turbidity. Connect the point of absorbance and the point
of maximum absorbance by a straight line to obtain a straight line standard calibration
curve.

6. Estimation of SO4-S in the BaSO4 turbidity developed with the aliquot of sample
water. Divide the absorbance of BaSO4 turbidity developed with aliquot of sample
water by the slope of the standard calibration curve expressed in unit of absorbance
 μg SO4-S taken for developing BaSO4 turbidity to obtain μg SO4-S present in aliquot
of sample water.

CALCULATIONS:

Absorbance value for SO4 – S Standards

Sulfate (in ppm) 0 5 10 15 20
Absorbance value 0 0.077 0.133 0.185 0.241

Absorbance value for Samples

Standard curve for Sulphates Group sample Absorbance
0.3 no no value
y = 0.012x
0.25 1 1 0.122
R² = 0.989
2 0.132
Absorbance (A)

0.2
3 0.121
0.15
2 1 0.152
0.1 2 0.123
0.05 3 0.135
3 1 0.125
0
2 0.129
0 5 10 15 20 25
Concentration (in ppm) 3 0.11
4 1 0.043
2 0.039
3 0.041
5 1 0.128
2 0.146
3 0.151