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0 Scope
This test method covers the determination of the relative activation level of unused
carbon by adsorption of iodine from aqueous solution. The amount of iodine adsorbed
(in mg) by 1 g of carbon is called the iodine number.
2.0 Apparatus
2.1
2.2
2.3
2.4
2.5
2.6
2.7
2.8
2.9
2.10
2.11
3.0 Reagent
3.1
3.2
3.3
3.4
3.5
3.6
3.7
3.8
Purify water.
Hydrochloric Acid, Concentrated.
Sodium Thiosulfate, (Na2S2O3. H2O).
Iodine.
Potassium Iodide.
Potassium iodide primary standard.
Starch solution.
Sodium carbonate.
4.4
Potassium Iodate Solution (0.100N)
Dry 4g of primary standard grade potassium iodate (KIO3) at 1100c for 2 hour and
cool into desiccators.
Dissolve 3.5667 mg of the dry potassium iodate in about 100ml distilled water
Quantitatively transfer to a 1L volumetric flask mark up to volume with distilled
water and use the flask stopper.
4.5
Starch Solution
Mix 1.0 0.5g of starch with 50-10ml of cold water to make paste.
Add an additional 25 5ml of water while stirring to the starch paste
Pure the mixture while stirring into boiling water and boil for 4-5 minutes. This
solution should be made fresh daily.
5.0 Standardization of Solution
5.1
Standardization of 0.100N Sodium Thiosulfate
Pipet 25.0ml of potassium iodate (KIO3) solution prepared above into a 250ml
wide mouth Erlenmeyer flask.
Add 2.0g potassium iodide (KI) to the flask and shake the flask to dissolve the
potassium iodide crystal.
Pipet 5.0ml of concentrated hydrochloric acid into the flask. Titrate the free iodine
with the sodium thiolsulfate solution until the a light yellow color is observed in
the flask
Add new a few drop of starch indicator and continue titration drop wise until one
drop produce a colorless solution. Determine the sodium thiosulfate normality as
followed
N1 = (P. R) / S
Where:
N1= sodium Thiosulfate, N
P = Potassium Iodate, ml
R = Potassium Iodate. N
S = Sodium thiosulfate, ml
5.2
6.0 Procedure
6.1
6.2
Dry the ground carbon from (6.1), and cool the dry carbon to room
temperature in desiccators
6.3
6.4
6.5
Pipet 10.0ml of 5 wt% hydrochloric acid solution into each flask content
carbon. Stopper each flask and swirl gently until the carbon is completely
wetted. After that loosen the stopper to vent the flask, place on the hot
plate in a fume hood and boil the content for 30s to remove the sulfur
content then cool it at room temperature.
6.6
Pipet 100.0ml of 0.100N iodine solution into each flask. Stopper the flask
and shake the content for 30s.
Quickly filter each mixture by gravity thought one sheet of folded filter
paper into a beaker.
6.7
For each filtrated use the first 20 to 30ml to rinse a pipet. Discard the
rinse portion. Use clean beaker to collect the remaining filtrates
6.8
Swirl the beaker and then pipet 50.0mL of each filtrated into a clean
Erlenmeyer flask.
6.9
Titrate each filtrate with standardize sodium thiosulfate solution until the
solution is a yellow pale. Then add 2mL of starch solution and continue
the titration until one drop produces colorless solution, and record the
volume of sodium thiosulfate used,
7.0 Calculation
7.1
7.2
7.3
7.4
7.5
Using log paper, plot X/M (as ordinary) versus C (abscissa) for each of
the three carbon dosage.
Calculate the least squares fit for the three points and plot.
The iodine number is the X/M value at a residual iodine concentration (C)
of 0.02N.
7.6
Carbon Dosage
M= [A (DF) (C) (126.93) (50)] / E
Where:
M
= Carbon, g
A
= (N2) (12693.0)
DF
= Dilution factor
C
= Residual Iodine
F
= Estimate iodine number of the carbon.
(Three carbon dosages are calculated using three values of C, usually is
0.01, 0.02, and 0.03).
8.0