Fluoridisation using impregnated Activated Charcoal with Al/Zr

© Ramaiah University of Applied Sciences
1
Faculty of Management and Commerce
Fluoridisation using impregnated Activated
Charcoal with Al/Zr
Guides: Dr. J.R. Mudakavi
Dr. Harshad Parate
• Gowthami M • Prajwal S Gowda
• Karthik H.M • Prathna P. Bhandary
• Magdum Hussain • Vishikha Keshava
• Manjunath P G
Team

2
1. Introduction, scope and literature survey
2. Materials and Methods
3. Prototype development
4. Results, discussion and conclusion
5. Future scope
6. References
CONTENTS

3
Introduction
• With increase in population in recent years there is a constant
demand for natural recourses, especially in case of drinking water.
• Due to increased demand, quality of the water is being
compromised, which in turn is creating serious health problems.
• This is very common in the rural areas of our country.
• When drinking water has excess amount of elements like fluoride or
arsenic removal of such elements is a must for healthy life.

4
Introduction contd..
• Consuming larger concentration of fluoride in drinking water causes
Decaying of teeth, osteoporosis, affects bones, kidney respiratory
organs muscle and nerves.

5
STAGES OF FLUOROSIS

6
Permissible limit as per WHO guidelines
About 0.5mg/l Beneficial in preventing dental
caries during tooth development
1.5 - 2mg/l Fluorosis or other health problem
2- 4 mg/l Deformation of body shape
More than 4mg/l Serious health issues and death

7
Current scenario in India
• Fluoride is the 13th most common substance in the world. Over 230
districts of over 20 states were reported with high level of fluoride
content.
• Around 11.7 million people were reported on 1.4.2014 were
reported to have risk associated with high level of fluoride content.

8

9
Current scenario in India contd..
The aims and objectives of (NPPCF) are as follows:
(National programme for prevention and control of fluorosis)
• To collect data, asses the present situation and use the surveyed data
as base line to start the project.
• To maintain the level of flourosis in the selected area, to find the
source of the element if it is caused because of naturally found
fluoride or it is because of external factor.
• Constructing a building in the specific area for maintaining fluorosis
cases, finding a way to diagnose them for further prevention and
managing the present fluoride cases.

10
• For these problems studies are conducted on the use of activated
carbons for removal of the fluoride element from the water body.
• Activated carbon doesn't have the property to absorb fluoride
from the water. However impregnation of GAC with aluminium or
zirconium is known to adsorb fluoride.
• Our investigations are aimed at developing impregnated GAC
process and examine its effectiveness for the removal of fluoride
from drinking water.
Solution

11
1. Defluoridation of water using impregnated GAC impregnated
with zirconium(Zr-GAC) and aluminum(Al-GAC) and
combinations there of.
2. To optimize the defluoridation process.
3. To design and develop defluoridation portable water filter and
water bottles for the average Indian families and students.
Objectives

12
Literature Review
Sl. no Author Year Title Overview
1 M. Rajan & G
Alagumuthu
2013 Study of fluoride
affinity by zirconium
impregnated walnut
shell carbon in
aqueous phase:
kinectic and isotherm
•The paper examines the kinetics
of Fluoride removal from water by
absorbent zirconium impregnated
walnut Shell.
•The kinetic profile has been
modified using pseudo first order
model and intra-particle diffusion
model.
•As per the result the fluoride
removed was 94%.
• It was measured by Orion ion
selective electrode equipment.

13
Literature Review contd…
2 C Janardhan
etal.,
2007 Study on
defluoridation of
drinking water using
zirconium ion
impregnated
activated charcoal.
•This paper reviews that the
absorption capacity of the fluoride
can be increased 3 to 5 times
more than that of plain activated
charcoal.
•The study was conducted by
impregnating ZrOCl2 in 3 columns
containing Groundnut shell,
coconut shell and coconut fiber.
•Results concluded that coconut
fiber was more efficient in
removing fluoride. This method
was best in removing fluoride
concentration from 2-10mg/l

14
3 Litz HAlla
Vela Zquez
2007 Zirconium-Carbon
Hybrid sorbent for
removal of fluoride
from water: oxalic
acid mediated Zr(IV)
assembly and
adsorption
mechanism.
• A activated carbon was modified
with Zr(IV) together with italic acid
which is used to maximize the
zirconium depression and enhance
fluoride absorption.
•Data Analysis by Langmuir and
Freundich isotherm models were
done

15
4 R Leyva
Ramos ab
etal.,
1999 Adsorption of
fluoride from
aqueous solution on
aluminium-
impregnated carbon
•The impregnated carbon is prepared
by impregnation of aluminium nitrate
solution at a fixed pH, followed by
calcination under nitrogen at
tempreratures above 300°C.
•The adsorption of fluoride on
impregnated carbon is dependent on
both pH of the impregnating solution
and temperature of calcination
•Impregnated carbon has fluoride
adsorption capacity of 3 to 5 times
that of plain activated carbon

16
5 M.
Mohapatra
etal.,
2009 Review of fluoride
removal from drinking
water
•Fluoride removal is broadly of
two types; one with membrane
and other with adsorption
techniques.
•Membrane techniques are
reverse osmosis, nanofiltration,
dialysis and electro dialysis
•Adsorption is one of the
conventional technique with
reoval of fluoride by aqueous
solutions using reversed zeolites,
modified zeolites, and ion
exchange resins based on cross
limked polystyrene

17
Research Gap
.
• No treatment methods adopted was 100% efficient
• Used activated carbon was made from coconut fiber, coconut shell,
cashew nut shell and groundnut shell, these are not available in
plenty, which makes the process slower
• There was no research paper which gives entire process of effective
deflouridation

18
Materials used
.
• Zirconium oxychloride
• Aluminium Nitrate
• Activated carbon
• SPADNS
• Hydrochloric Acid
• Sodium Fluoride
• Glass wares
Chemicals used are of Analar grade
Glasswares used are of A grade

19
Technical specifications GAC(Granular Activate Carbon)
.
Properties Specifications
Appearance Black granular
Moisture 2.5-3%
Hardness 88%
pH 7-8
Iodine Value 600-700 mg/g
Bulk density 0.50 g/l
Ash Max 3%
Surface area 800 sqm
CTC adsorption Min 45%
Activation steam

20
Method Merits Disadvantages
Nalgonda Low technology
adaptable at
point of use and
point of source
level
• Large quantity of sludge.
• High chemical dose.
• Dose depend on F- level.
• Daily addition of chemicals and stirring in point of
source units.
Bone Char Local available
media
• May impart taste and odour and result in organic
leaching if not prepared properly.
• Requires regeneration periodically.
• Effected by high alkalinity.
• May not be acceptable in some countries.
Activated
alumina
Effective, much
experience
• Periodic regeneration.
• Skilled personnel for plant operation.
• Properly trained staff for regeneration of point of use
units.
• Suitable grades may not be indigenously available in
less developed countries.
Existing Techniques

21
Method Merits Disadvantages
Contact precipitation Not much experience • Algal growth can occur in phosphate
solution.
• Bone char used as a catalyst may not
be acceptable in many countries.
Reverse osmosis Can remove other ions • Skilled operation.
• Interference by turbidity
• High cost
Existing Techniques contd…

22
Fluoride analysis
SPADNS (method)
.
Preparation of the reagent
• Stock fluoride solution (100 ppm): Dissolve 22.1 mg of anhydrous
sodium fluoride in deionised water and make up to 100 ml.
• Standard Fluoride solution ( 5 ppm): Dilute 5 ml of the stock fluoride
solution to 100 ml with deionised water.
• SPADNS solution: Dissolve 191.6 mg of SPADNS in deionised water
and dilute to 100 ml with deionised water.
• Zirconyl- Acid reagent: Dissolve 26.6 mg of zirconylchloride
octahydrate (ZrOCl2.8H2O) in about 5ml of deionised water and add
70 ml of concentrated HCl and dilute up to 100 ml using deionised
water.

23
Fluoride analysis
SPADNS (method) contd..
.
Preparation of the reagent contd..
• Acid- Zirconyl- SPADNS reagent: Mix equal volume of SPADNS
solution and acid- zircolyl reagent to obtain 50 ml of the acid-
zirconyl- SPADNS reagent.
Procedure
• Transfer 0, 1, 2, 3, 4 ml of 5 ppm standard fluoride solutions into six
different 10 ml volumetric flasks.
• Add 2 ml of acid- zirconyl- SPADNS reagent to each.
• Dilute to 10 ml with deionised water.

24
Fluoride analysis
SPADNS (method) contd…
.
Procedure contd..
• After 10 -15 minutes, measure the absorbance of each solution in a
spectrometer with 1 cm path length at a wavelength of 570 nm
against the blank.
• Subtract the absorbance values from that of the blank.
• Prepare a calibration curve of the difference absorbance versus
concentration of the fluoride
• Determine the concentration of the samples by referring to the
calibration curve.

25
Fluoride analysis
SPADNS (method) contd…
.
Recommended sample volume for 2ml:
• Cookbook value : 10 micro grams of fluoride in 10ml (1.0 ppm) gives
an absorbance of 0.198

26
UV Spectrophotometer
.
•Spectroscopy deals with production, measurement and
interpretation of spectra arising from the interaction of
electromagnetic radiation with matter.
•Spectrophotometer is an instrument used to measure the
absorbance of light by a sample and works on the principle of Beer-
Lambert Law.

27
Procedure
.
Preparation of Impregnated Activated Carbon
• 1%, 2% & 5% Al(NO3)3 in 100 ml of water + 10 g Granulated activated
carbon impregnated and stirred for 1 hour
• Then it is filtered and dried in muffle furnace for 200°C /250°C/
300°C/400 °C for 1 hour.

28
Procedure contd…
.
Preparation of solution
•1 g, 2 g, 5g of Zr-GAC/Al-GAC is added to 100 ml of 5 ppm fluoride
solution.
•It is stirred for 1, 2, 3, 24 hours and sample was taken for testing.

29
Bottles, Cartridges and Portable water filter
.
Membrane infuser water Bottle with top candle
• Water bottle is USFDA approved PET (polyethylene terrphtalate).
• This bottle is made of 100% food grade material & is BPA free which
ensures a safe drink.
Specification
Type- fridge water bottle
Design- transparent and plain
Capacity- 750 ml

30
.
Membrane infuser water bottle with bottom candle
• Smooth bottle mouth
• Detachable stainless steel strainer
• Multifunction practical bottle
• Anti – slip silicone belt
• Convenient membrane storage

31
.
• The membrane infuser bottles are the best way to store water.
• Just washing and re-using ,for pouring a hot and cold water.
• Bottles will never smell or carry any residue taste while keeping the
membrane in contact
• The bottles are transparent plastic body, a stainless steel strainer
and lids which makes it absolutely perfect material for drinking pure
water free from fluoride.
• Keep the bottle aside for 45 minutes to an hour allowing to slowly
extract the fluoride from the water.

32
Compact, Light and Durable
.
• This membrane infuser bottles are of moderate size bottles which is
light in weight and easy to use
• Made with high quality plastic material body with the heat resistant
silicone band which makes the bottle durable and long time
companion
• Leak-proof and Drop-Resistant
• We can keep cool or warm water for much longer without sweating
or leaking
• Can use it freely without worrying about any damage

33
Cartridge filter
.
• A cartridge filter is a filter that uses a barrier/sift method in order to
clean sediments and harmful solids out of water.
• Some of these filters are made to stop it microscopic items and
others are made simply to stop the major solids from entering a
system.
• One of the most economic and versatile of cleaning methods, these
filters are used for drinking water purification systems and also in
fish aquariums and swimming pools
• The cartridge filter is usually a cylindrical object, though in some
cases it can look flat, much like an Air Filter.
• The shape of the filter is most dependent on its location.

34
Cartridge filter contd..
.
• If located in a pipe or filter housing, it will, by necessity, be
cylindrical.
• Many prefer to use a cartridge filter when drinking water from a
home tap due to the number of additives often found in
municipal water system or also in ground water.
• Chlorine and other additives, used to make the water safe, can also
leave an undesirable taste. A filter can be used to take some of these
chemicals out of the water, leading to an improved taste.

35
Sediment filters
.
• In the mechanical type of filter we will always see a rating which will
tell, what size particles it will and won’t remove.
• Filters are rated in microns.
• A micron is one millionth of a metre. A human hair is 70 microns in
diameter, a cryptosporidium oocyst 4-6 microns and a Giardia cyst 8
– 12 microns.

36
Housing
.
• These cartridges are inserted into filter housings that are installed as
part of the plumbing of the home or cottage.
• They can be installed in a basement or utility room or smaller
systems can even be installed under the kitchen sink.
• (See RO systems) The housings and cartridges are interchangeable
in most cases, so we can buy the best value brand cartridge and do
not have to stay with the brand originally installed.

37
Housing Attached
.
Storage tank
Cartridge With ZrGAC
pH booster
Discharge unit
Storage tank
Cartridge With ZrGAC
pH booster
Discharge unit

38
Cost Estimation of portable model
Laboratory condition.
GAC cost = Rs 400/- per kg2.
ZrOCl2 =Rs 500/- per 100 g3.
Processing charges – water filteration, oven, muffle furnace = Rs 100/- per kg
Total cost of ZrGAC = 400+ 500 +100= 1000 per kg
For 100 ml of water to be defluoridised, 5 g of ZrGAC is required.
For 20 litres of water under pH 3 to be defluoridised 200g of ZrGAC is required ie; Rs
200/- Therefore for 1 litre of defluoridation it costs Rs 10/-.

39
Cost Estimation of portable model
material Price (Rs)
Bottom candle (750ml) 500
Zr-GAC (37.5g) 37.5
Materials Price (Rs)
Top candle bottle (500ml) 150
Zr-GAC (25g) 25
Total cost= Rs 154
Total cost = Rs 540

40
• Cartridge 1 piece = RS200/-
• Housing 1 piece = Rs 200/-
• pH booster = Rs 249/-
• 5” inch pipe = Rs50/-
• Wooden sheet = 8’X4’ = Rs 1,650/-
• Total nuts and bolts = Rs 300/-
• Total cost = Rs 2,649/-
Cost Estimation of Housing model

41
Determination of fluoride content using 1 % ZrGAC with stirring.
Blank Standard Difference
0.677 0.454 0.223
1% Zr.
Activated
carbon
Absorbance at
570 nm
Difference % Removal
1 g 0.468 0.209 6.28
2 g 0.509 0.168 24.66
5 g 0.534 0.143 35.87
Results

42
Determination of fluoride content using 1 % AlGAC with stirring.
0.677 0.454 0.223
1 % Al.
Activated
carbon
Absorbance at
570 nm
1 g 0.521 0.156 30.04
2 g 0.497 0.180 19.28
5 g 0.645 0.032 85.65
Results contd…

43
Determination of fluoride content using 2 % ZrGAC with stirring
0.948 0.758 0.190
2 % Zr.
Activated
carbon
Absorbance at
570 nm
1 g 0.756 0.192 0
2 g 0.859 0.089 53.16
5 g 1.118 -0.17 100
Results contd…

44
Determination of fluoride content using 2 % AlGAC with stirring.
0.948 0.758 0.190
2 % Al.
Activated
carbon
Absorbance at
570 nm
1 g 0.791 0.157 17.36
2 g 0.840 0.108 43.16
5 g 1.113 -0.165 186.84
Results contd…

45
Determination of fluoride content using 5 % ZrGAC with stirring
0.948 0.758 0.190
5 % Zr.
Activated
carbon
Absorbance at
570 nm
1 g 0.791 0.157 17.37
2 g 0.931 0.017 91.05
5 g 0.992 -0.044 100
Results contd…

46
Determination of fluoride content using 5 % AlGAC with stirring
0.948 0.758 0.190
5 % Al.
Activated
carbon
Absorbance at
570 nm
1 g 0.840 0.108 43.16
2 g 0.847 0.101 46.84
5 g 0.918 0.03 84.21
Results contd…

47
5 % Zr.
Activated
carbon
Absorbance at
570 nm
5 g 0.992 -0.044 100
5 % Al.
Activated
carbon
Absorbance at
570 nm
5 g 0.918 0.03 84.21
5% of 5gm ZrGAC at shows better results compared to rest of the
combinations.
0.948 0.758 0.190
Results contd…

48
Results shows 250 0C is the best temperature for impregnation of
zirconium into activated carbon.
Temperature of
5 % Al.
Activated
carbon
Absorbance at
570 nm
200 0.625 0.06 72.60
250 0.683 0.002 99.00
300 0.618 0.067 69.41
400 0.523 0.162 26.02
0.685 0.466 0.219
Results contd…

49
5 % of 0.5g Zr.
Activated carbon
with different pH
Absorbance at
570 nm
pH 1 0.656 0.011 94.44
pH 2 0.647 0.013 93.43
pH 3 0.666 0.001 99.49
pH 4 0.596 0.071 64.14
pH 5 0.567 0.100 49.49
pH 6 0.577 0.090 54.54
0.667 0.469 0.198
At pH 3 the removal of fluoride from water is maximum
Results contd…

50
Results shows 250 0C is the best temperature for impregnation of
zirconium into activated carbon.
Temperature of
5 % Al.
Activated
carbon(in 0C)
Absorbance at
570 nm
200 0.625 0.06 72.60
250 0.683 0.002 99.00
300 0.618 0.067 69.41
400 0.523 0.162 26.02
0.685 0.466 0.219
Results contd…

51
5 % of 0.5 Zr.
Activated carbon
with different pH
Absorbance at
570 nm
pH 1 0.656 0.011 94.44
pH 2 0.647 0.013 93.43
pH 3 0.666 0.001 99.49
pH 4 0.596 0.071 64.14
pH 5 0.567 0.100 49.49
pH 6 0.577 0.090 54.54
0.667 0.469 0.198
At pH 3 the removal of fluoride from water is maximum
Results contd…

52
0.678 0.480 0.198
Results of bottle with bottom candle
Time Absorbance Difference % Removal
10 mins 0.557 0.121 38.89
20 mins 0.527 0.151 23.73
30 mins 0.542 0.136 31.31
40 mins 0.565 0.113 42.92
50 mins 0.606 0.072 63.63
1 hour 0.668 0.010 94.95
37.5g of ZrGAC is used for 750 ml water bottle with bottom candle

53
0.688 0.490 0.198
Results of bottle with top candle
Time Absorbance Difference % Removal
10 mins 0.577 0.111 43.94
20 mins 0.587 0.101 48.99
30 mins 0.592 0.096 51.51
40 mins 0.599 0.089 55.05
50 mins 0.609 0.079 60.10
1 hour 0.682 0.006 96.96
25g of ZrGAC is used for 500 ml water bottle with top candle

54
For 20 lit water tank, 100g of ZrGAC is taken and pH 3 is optimized.
Results of Cartridge
5 % of 0.5 Zr.
Activated carbon
with pH 3
Absorbance at
570 nm
15 mins 0.567 0.100 49.49
30 mins 0.577 0.090 54.54
45 mins 0.596 0.071 64.14
1 hour 0.666 0.001 99.49
Blank absorbance Standard absorbance Difference
0.667 0.469 0.198

55
Conclusion
.
• Comparative studied was done Zirconium chloride produces better
result compared to aluminium nitrite for the same condition.
• The efficiency of both zirconium and aluminium is maximum when the
pH 3 is maintained in the water sample.
• 5% of 5g zirconium in 100 ml water removes 100 % fluoride from water
within one hour stirring.
• 5% of 0.5g of zirconium in 100ml water of pH 3 removes 100 % fluoride
from water.
• To make the model cost effective 5% 0.5 gm zirconium at pH 3 should
be considered.

56
• To conduct the experiments with normal borewell water.
• To optimize the continuous process conditions.
• To determine the effect of hardness, chloride, sulphate, nitrates,
carbonates and alkalinity.
• To evaluate cost effectiveness.
Future Scope

57
References
.
1. Halla, L. et al., 2014. Zirconium-carbon hybrid sorbent for removal of
fluoride from water: Oxalic acid mediated Zr(IV) assembly and
adsorption mechanism. Environmental science and technology, I(48),
pp. 1166-1174.
2. Mohapatra, M. et al., 2009. Review of fluoride removal from drinking
water. Journal of Environmental Management, II(3), pp. 67-77.
3. Rajan, M. & Alsgumuthu, G., 2013. Study of Fluoride affinity by
zirconium impregnated walnut shell carbon in aqueous phase: Kinetic
and istherm evaluation. Journal of chemical , II(23), pp. 15-23.
4. Ramos, R. L., Turrubiartes, O. & Castillo, S., 1999. Adsorption of
fluoride from aqueous solution on aluminium- impregnated carbon.
III(24), pp. 78-84.
5. Rao, N. G. et al., 2007. Study of defluoridisaton of drinking water
using zirconium ion impregnated activated charcoal. Indian Journal of
Chemical Technology, 14(I), pp. 350-354.

58
Thank you

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