1.

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

Analytical Balance, accuracy 0.0001g.

Buret, 10ml capacity or 5ml precision.
Flask Erlenmeyer 250ml, capacity with ground stopper.
Flask Erlenmeyer wide mouthed 250ml.
Beaker assorted sizes.
Bottle, amber for storage iodine and thiosulfate solution.
Funnels 100mm top inside diameter.
Filter paper 18.5cm prefolded paper (Whatman).
Pipets volumetric type 5.0, 10.0, 25.0, 50.0, 100.0ml.
Volumetric flask, 1L.
Graduated Cylinder, 100ml and 500ml.

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.

4.0 Preparation of reagent

4.1
Hydrochloric Acid Solution (5% by weight)
Add 70ml of concentrated hydrochloric acid to 550ml of distilled and mix well.
4.2
Sodium Thiosulfate (0.100N)
Dissolve 24.320g of sodium thiosulfate in 75 25ml of freshly distilled water.
Add 0.1g of sodium carbonate and mix well. Transfer the mixture to the 1L
volumetric flask and dilute to the mark. Allowed the solution to stand at least 4
days before standardizing. The solution should be store in the amber bottle.
4.3
Standard Iodine Solution (0.100N 0.001N)
Weight 12.700g of iodine and 19.00g of potassium iodide (KI) into the beaker.
Mix the dry iodine and potassium iodide, Add 2 to 5ml of water to the beaker and
stir well. Continue adding small increment of water (approximately 5 ml) while
stirring until the total volume is 50-60ml. Allowed the solution to stand minimum 4
hour to ensure that all crystal are thoroughly dissolved. Stir during this 4hour
period will aid in the dissolution.
Quantitatively transfer to a 1L volumetric flask and mark up with distilled water.

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

Standardization of 0.100N Iodine Solution

Pipet 25.0ml of iodine solution (4.3) above into 250ml wide mouthed Erlenmeyer
flask. Titrate with standardized sodium thiosulfate (5.1) above, until the iodine
solution is a light yellow color.
Add a few drop of starch and continue titration drop wise until one drop produces
a colorless solution.
Determine the iodine solution normality as follows.
N2 = (S. N)/ I
Where:
N2= Iodine, N
S= Sodium Thiosulfate, ml
N1= Sodium Thiosulfate, N and
I= Iodine, ml

6.0 Procedure
6.1

Sieve sample of activated carbon.

6.2

Dry the ground carbon from (6.1), and cool the dry carbon to room
temperature in desiccators

6.3

Determination of iodine number requires an estimating of three carbon

dosages, show on section (7.6). After estimating carbon dosages, weight
three appropriate amount of dry carbon to nearest milligram.

6.4

Transfer the each weighted sample of carbon to a clean, dry 250ml

Erlenmeyer flask equipped with a ground glass stopper.

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

The amount of carbon sample to be used in the determination is

governed by the activity of the carbon.
If the filtrated normality (C) is not within the range of 0.008N to 0.040N,
repeat the procedure using the different weights.
Two calculation is required for each carbon dosage as X/M and C
To calculate the value of X/M
A= (N2) (12693.0)
Where:
N2= iodine, N (from 5.2)
B= (N1) (126.93)
Where:
N1 = Sodium Thiosulfate, (N) (from 5.1)
DF= (I + H) / F
Where:
DF
= Dilution factor
I
= iodine, ml (from 5.2)
H
= 5% Hydrochloric Acid, ml
F
= Filtrate, ml
X/M= (A (DF). (B). (S) / M)
Where:
X/M
= Iodine absorbed per gram of carbon mg/g
S
= Sodium Thiosulfate, mL
M
= Carbon used, g

7.4

Calculate the value of C

C= (N1. S) / F
Where:
C
= Residual filtrate, N
N1
= Sodium Thiosulfate, (N) (from 5.1)
F
= filtrate, mL

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

Method flow chart

Sieve estimating amount of

activated carbon sample
Dry & cool the sample at room temperature.
Determine estimating of 3 carbon dosage by calculation,
showed on section 7.6
After that weight 3 appropriate amount of dry carbon to nearest milligram.
Transfer each weighted sample of carbon to 250ml Erlenmeyer flask & equipped
with stopper
Pipet 10ml 5% HCl (by weight) into each flask then stopped it with stopper and swirl
gently
Loosen the stopper and place on hot place & boil content for 30 then cool it
at room temperature
Pipet 100.0ml of 0.100N iodine solution into each flask then stopped
the flask and shake content for 30s
Quickly filter each mixture thought one filter paper into beaker.
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
Swirl the beaker and then pipet 50.0ml of each
filtrated into clean Erlenmeyer flask.
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,