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Harsh K.

Dixit

Envirotech Centre for Research & Development New Delhi

Dissolve 10.86 gm Mercuric chloride + 0.066 gm EDTA + 6.0 gm Potassium chloride


And make upto 1000ml with distilled water

Sulphamic acid Solution (0.6%)


Dissolve 0.6 gm Sulphamic acid in 100 ml distill water.

formaldehyde Solution (0.2%)


Take 1.25 ml formaldehyde Solution (36-38%) and make upto 250 ml with distill water.

Pararosaniline Solution (PRA)


Stock PRA solution:
Dissolve 0.5 gm of Parasoaniline in 100 ml distill water & keep it upto 48 hour.

Working PRA solution:


Take 10 ml Stock PRA solution + 15 ml Concentrated HCl and make upto 250 ml with distill water.

Stock Iodine solution (0.1N)


Dissolve 1.27 gm of Iodine + 4.0 gm potassium iodide + 25 ml distill water, stir untill whole matter is dissolved And make upto 100ml with distilled water

Working Iodine solution (0.01N)


Take 50ml of stock iodine solution and make upto 500ml with distill water (This solution is stored in amber color glass bottle.)

Starch Indicator
Dissolve 0.4 gm of Soluble starch + 0.002 gm Mercuric iodide in small amount of water & make a paste Add 200ml distilled water & boil until clear solution

Primary Standard Potassium Iodate Solution


Dissolve 1.5 gm of Potassium Iodate (oven dried at 180C) And make upto 500ml with distilled water

(Prepare freshly)

Stock Sodium Thiosulphate Solution (0.1N)


Dissolve 6.25 gm of Sodium Thiosulphate + 0.025 gm Sodium carbonate In 250 ml boiled & cooled distill water Stand for one day before standardization

Stock Sulphite Solution


Dissolve 0.15 gm of Sodium metabisulphite

In 250 ml boiled & cooled distill water


1ml = 320 400ug SO2, Find actual concentration after Standardization

Standardization of Soduim thiosulphate solution


Take 50 ml of Sodium Iodate Solution in 250 ml Iodine Flask. Add 2.0 gm Potassium Iodide & 10ml of (1 : 10) HCl. Put Stopper on the flask and allow to react for 5.0 min. Titrate with stock sodium thiosulphate solutio to a pale yellow color. Add 2 5 ml starch indicator, it shall give blue color. Continue Titration up to disappearance of color.

Standardization of Soduim thiosulphate solution


Calculate the normality as follows:N = w 103 0.1 OR N= 2.8 W V 35.67 V Where:W = Weight of Potassium Iodate, gm (Primary Standard) V = Volume of Sodium Thiosulphate Solution consumed (ml). 35.67 = Equivalent wt. of Potassium Iodate. N = Normality of Sodium Thiosulphate.

Working Soduim thiosulphate solution


Calculate the required volume of Stock Sodium Thiosulphate solution to prepare a required volume of working sodium

thiosulphate solution
N1V1=N2V2 N1 = Normality stock Sodium Thiosulphate Solution (0.1N) V1 = volume of Stock Sodium Thiosulphate solution N2 = Normality of warking Sodium Thiosulphate (0.01N) V2 = Required volume of working Sodium thiosulphate solution Take..ml of stock sodium thiosulphate solution and make up to.ml with freshly boiled & cooled distilled water.

Iodine Flask 250ml (for Blank) Pipette 50ml of 0.01N Iodine Solution Add 25ml distill water

Iodine Flask 250ml (for Sample) Pipette 50ml of 0.01N Iodine Solution Add 25ml Stock Sulphite solution

Stopper the flask & allow to react for 5.0 minutes Titrate each flask in turn to a pale yellow with working Sodium thiosulphate solution (0.01N) Add 5.0ml starch solution to each flask (it gives blue color to solution)

Note the volume of 0.01N Sodium thiosulphate solution consumed for Blank & Sample
For blank consumed Sodium thiosulphate For sample consumed Sodium is V1ml thiosulphate is V2ml

Calculation for Strength of Stock Sulphite solution


C = (V1-V2) x N x K V Where C = Concentration of SO2 (g/ml) V1 = Volume of sodium thiosulphate solution (0.01N) consumed for Blank (ml) V2 = Volume of sodium thiosulphate solution (0.01N) consumed for Sample (ml) N = Normality of sodium thiosulphate solution K = 32000 Miliequivlent wt. of SO2/g V = Volume of sulphite Solution (25ml)

Working Sulphite solution


Take 2.0ml of Stock Sulphite solution And make upto 100ml with absorbing media (TCM 0.04M)

Strength of Working Sulphite solution


= Cx2 100 Where C = Concentration of Stock Sulphite Solution (gSO2/ml)

Volumetric Flask Working Sulphite Sol Absorbing Media

25ml Blank 0.0ml 10ml

25ml Sample1 0.5ml 9.5ml

25ml Sample2 1.0ml 9.0ml

25ml Sample3 1.5ml 8.5ml

25ml Sample4 2.0ml 8.0ml

25ml Sample5 3.0ml 7.0ml

Sulphamic acid

1.0ml

1.0ml

1.0ml

1.0ml

1.0ml

1.0ml

Keep all volumetric flask for 10 minutes to destroy the nitrite resulting from oxide of Nitrogen Formaldeh yde Sol. Working PRA 2.0ml 2.0ml 2.0ml 2.0ml 2.0ml 2.0ml 2.0ml 2.0ml 2.0ml 2.0ml 2.0ml 2.0ml

Make upto 25ml with distill water, Mix thoroughly , After 30 minutes measure absorbance of each flask at 560nm wavelength

Plot calibration curve with absorbance versus concentration of SO2

Volumetric Flask Exposed absorbing Media Absorbing Media Sulphamic acid

25ml For Blank 0 ml 10ml 1.0ml

25ml For sample 10ml 0ml 1.0ml

Keep all volumetric flask for 10 minutes to destroy the nitrite resulting from oxide of Nitrogen Formaldehyde Sol. Working PRA 2.0ml 2.0ml 2.0ml 2.0ml

Make upto 25ml with distill water, Mix thoroughly , After 30 minutes measure absorbance of each flask at 560nm wavelength

Total volume of air passed through Nox impinger (V, in liter) Avg. Flow Rate (lpm) X Time (minute)

Concentration (ug SO2/m3) = C x A x 1000 x D VxB


Where: C= SO2 Curve value A= Absorbing reagent taken for sampling, ml V= Volume of sampled air B= Volume taken for sample analysis, ml D= Dilution factor 1000 for conversion from liter to m3

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