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CHAPTER 1

INTRODUCTION
Presence of fluoride above the prescribed limit in groundwater used for drinking
has caused many health problems, mainly dental fluorosis and skeletal fluorosis.
Fluoride is one of the main constituents occurring in groundwater of India, thus
creating a major problem in safe drinking water. Several methods of defluoridation
of drinking water have been developed. In India, precipitation and adsorption are
mostly preferred. Precipitation methods involve addition of chemicals and
removing insoluble compounds as precipitates. In adsorption method, different
adsorbents like chemically activated carbon, activated alumina are used.
The problem with above mentioned methods are high operating and
maintenance cost, low fluoride removal capacity, undesirable after effects on
water quality. Nalgonda technique is the most common precipitation technique
used in India. Its major limitations are daily addition of chemicals, large amount of
sludge production, least effective in water having large amount of total solids and
hardness. Large portion of ionic fluoride is converted into soluble aluminum
complex thus removing only a small portion of fluoride in the form of precipitate.

1.1 Effects of Fluoride


Following are the effects of fluoride on human health
• Skeletal fluorosis
• Dental fluorosis
• Risk of fractures in bones
• Immune deficiency
It is estimated that more than 11 million people in India in 160 districts spread
over 16 states, are affected with fluorosis, caused by continuous intake of water
with excess fluoride content ranging from 1.5 mg/l to 16 mg/l. Its effects are
mainly due to the depositing of fluoride in bones and cartilage including

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metabolic disorders, mottled teeth, bent skeletal structure and some cases even
paralysis.

Effects of concentration of Fluoride


Concentration of fluoride Effect

<1.0 Reduces dental caries

1.0-1.5 Marginal risk of fluorosis

1.5-3.0 High risk of dental fluorosis

3.0-10.0 Leads to skeletal fluorosis with adverse


change in bones

>1 0.0 Crippling and skeletal fluorosis

Table 1.1 showing effects of concentration of fluoride

1.2 Distribution of fluoride in India


In India states of Andhra Pradesh, Orissa, Punjab, Rajasthan, Tamilnadu, Uttar
Pradesh and West Bengal are affected by fluoride contamination in water. This
involves about 9000 villages affecting 11 million people. The fluoride content of
the water in some states is given in the table 1.2.

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Distribution of fluoride in India
Place Fluoride in PPM

Jammu & Kashmir 0.2to18

Himachal Pradesh 0.2to 6.5

Rajasthan >1.5

Haryana 0.2 to .6

West Bengal 12.0

Chhattisgarh 15to 22

Orissa 8.2to13.2

Table 1.2 showing distribution of fluoride

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Chapter 2
Defluoridation using brick powder as an adsorbent
2.1 Materials and methods
Bricks utilized were washed with distilled water, dried and grounded to obtain fine
powder. The brick powder was washed several times with distilled water till clear
water was obtained and was dried in oven at 105 °C for 12 h. The dried material
was sieved to separate less than 300 μm size of particles. The comparison of the
brick powder (BP) was made with the commercially available activated charcoal
(CAC) LR grade. The characteristics of brick powder and activated charcoal used in
the present study are given in Table 2.1. The brick powder does not require any
activation in preparation of adsorbent as well as its easy accessibility in rural area
reduce it cost as compare to activated charcoal.

Characteristics of adsorbents

Characteristics Brick powder Activated carbon

Bulk density (g/cc) 1.02 0.46

Matter soluble in 1.12 1.5


water (%)

Matter soluble in acid 2.23 2.5


(%)

pH 6.14 7.16

Particle size (μm) <300 <300

Table 2.1 showing characteristics of adsorbents

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Keeping in view that the maximum concentration of fluoride reported in
groundwater of most of the fluoride-affected area is around 5 mg /l, the tests were
conducted on solution with fluoride concentration of 5mg/l. All the experiments
were carried out in 250 ml conical flasks with 100 ml test solution at room
temperature (25 ± 3 °C). At the end of desired contact time, the conical flasks were
allowed to stand for 2 min for settling the adsorbent. Then, samples were filtered
using Whatman filter paper of grade no 42 and filtrate was analyzed for residual
fluoride concentration by SPADNS method. Batch study was conducted to
determine the optimum conditions and to study the effect of pH, adsorbent dose
and contact time on test solution. The effect of pH on fluoride was studied by
adjusting the pH of test solution using 0.1N HCl or 0.1N NaOH on fixed quantity of
adsorbent, while effect of adsorbent dose and contact time were studied by varying
dose and contact time, respectively.

2.2 Results and discussion


2.2.1 Effect of pH
The effect of pH on removal of fluoride was studied in the pH range of 4.0–9.0
and results are shown in Fig. 2.1 pH played a major role in fluoride adsorption on
brick powder. The studies were conducted with contact time and initial fluoride
concentration as 60 min, 5.0 mg/l for both brick powder and activated carbon.
Adsorbent doses are 1.0 g/100 ml for brick powder and 0.6 g/100 ml for activated
carbon.
• Maximum adsorption of fluoride was found to be 51.0–56.8% in pH range
between 6.0 and 8.0.
• Percentage removal fell sharply as pH decreased below 6.0 and above 8.0.
• The lower adsorption efficiency of fluoride in acidic medium might be due to
the formation of weakly ionized hydrofluoric acid, which reduces availability
of free fluoride for adsorption.

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• In alkaline conditions, lower adsorption may be due to the competition of
OH− ions with F− ions for adsorption because of similarity in F− and OH− in
charge and ionic radius.
• Optimum pH was found to be 8 for brick powder and 4 for activated carbon.

Fig 2.1 showing effect of pH on fluoride removal for contact time of 60 min.

2.2.2 Effect of contact time


• The effect of contact time on adsorption of fluoride is studied and the results
were presented as percentage removal of fluoride by BP and CAC after
different contact times in fig 2.2
• As contact time was increased, initially, percentage removal also increased,
but after some time, it gradually approached an almost constant value,
denoting attainment of equilibrium.
• It was assumed that the equilibrium time is that at which curves appear
nearly asymptotic to the time axis.
• In the present case, the equilibrium time was obtained at 60 min for BP and
CAC.
• The changes in the rate of removal might be due to the fact that initially all
adsorbent sites were vacant and the solute concentration gradient was high.

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Later, the fluoride uptake rate by adsorbent had decreased significantly, due
to the decrease in number of adsorption sites.
• Decreased removal rate, particularly, towards the end of experiment,
indicates the possible monolayer of fluoride ions on the outer surface, pores
of both the adsorbents and pore diffusion onto inner surface of adsorbent
particles through the film due to continuous shaking maintained during the
experiment.

Fig 2.2 showing effect of contact time on fluoride removal

2.2.3 Effect of dose


The effect of adsorbent dosage on adsorption of fluoride at pH 8.0 for BP and 4.0
for activated carbon and contact time 60 min for both adsorbents was studied and
the results were presented as percentage removal of fluoride versus adsorbent
dosage in fig 2.3.
• The removal of fluoride increased from 43.2 to 56.8% for 0.2–2.0 g/100 ml
dosage of brick powder and 49.4–84.2% for 0.2–2.0 g/100 ml dosage of
activated carbon.

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• It can be seen from fig 2.3 that after dosage of 0.6 g/100 ml in case of brick
powder and 1 g/100 ml in case of activated carbon, there was no significant
change in percentage removal of fluoride. It was due to the overlapping of
active sites at higher dosage, thus, reducing the net surface area.

Fig 2.3 showing effect of adsorbent dosage on fluoride removal.

Discussion
• The optimum pH was found to be in the range of 6.0-8.0 for maximum
adsorption of fluoride, which makes it very suitable for use in drinking water
treatment especially in rural areas.
• Presence of others ions in groundwater did not significantly affect the
defluoridation process thereby indicating that brick powder is selective
adsorbent for fluoride.
• Comparisons of brick powder and activated carbon revealed that brick
powder is economical adsorbent for removal of fluoride due to greater and
easy abundance as compare to activated carbon and it can work on natural
pH while CAC work on acidic pH.

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CHAPTER 3
Defluoridation using Basil leaves
As basil is available at every household and as it is easy to identified due to is proven
medicinal values this was selected for the study.
3.1Method
Sample collection and preparation
• Fresh basil leaves were selected by cutting them into small portions
and by taking different doses of 25, 50, 75, 100 and 125 mg.
• A synthetic fluoride solution was prepared having initial concentration of 5
ppm and experimental work was conducted by varying doses and pH levels
shaking on a shaker for 20 min. The combination of doses and pH levels were
selected at which maximum fluoride removal was observe
3.2 Dose selection

• Different doses of fresh basil leaves as 25, 50, 75, 100 and 125 mg were taken
in different beakers and reagent bottles each containing 100 ml synthetic
fluoride solution having concentration of 5 ppm.
• Beakers containing different doses were kept for shaking on shaker for 20
min
• After shaking, experimental solutions were filtered through Whatman filter
paper and 50 ml of filtrate was analyzed for residual fluoride concentration
by SPADNS method.
• Optimum dose was found to be 75 mg

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Effect of dosage on fluoride removal
Dose of basil Fluoride sample, Initial fluoride Fluoride
leaves ml concentration concentration
,ppm after treatment
,ppm
25 100 5 0.42

50 100 5 0.52

75 100 5 0.32

100 100 5 BDL

125 100 5 BDL

Table 3.1 showing effect of dosage on fluoride removal

120

100
PERCENTAGE REMOVAL OF FLUORIDE

80

60

40

20

0
0 10 20 30 40 50 60 70 80
DOSAGE OF BASIL LEAVES (mg)

Fig 3.1 showing effect of dosage on fluoride removal

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3.3 pH selection
• The pH of the synthetic fluoride samples was maintained at different pH
levels as 6, 7, 8, and 9.
• The optimum dose of basil leaves was selected at which maximum fluoride
removal was obtained.
• By adding the constant dose of leaves at different pH levels 6, 7, 8 and 9
procedure was carried out for 20 min.
• After treatments, solution was filtered through Whatman filter paper and
filtrate was analyzed for residual fluoride concentration by SPADNS method.
• Optimum pH was found to be 9.

Effect of pH on fluoride removal


Dose of basil leaves, Initial fluoride pH of fluoride Fluoride
(mg) concentration ,ppm solution concentration after
treatment ,ppm
75 5 6 0.20

75 5 7 BDL

75 5 8 BDL

75 5 9 0.12

Table 3.2showing effect of pH on fluoride removal


(NOTE: BDL –Below detectable level)

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99.5

PERCENTAGE REMOVAL
99

98.5

98

97.5

97

96.5

96

95.5
0 2 4 PH 6 8 10

Fig 3.2 showing effect of pH on fluoride removal

3.4 RESULT AND DISCUSSION


• After treatment of fresh basil leaves at a dose of 25, 50 and 75 mg with initial
fluoride concentration of 5 ppm; it was reduced to < 0.6 ppm by both boiling
and shaking methods. The resulting solution became slightly greenish in
colour due to increase in doses of material with a pleasant odour.
• However, at higher doses of fresh basil leaves of 100 and 125 mg/100 ml, the
resulting fluoride concentration was below detectable limit.
• At selected dose of 75 mg of fresh basil leaves with variable pH levels of 6, 7,
8 and 9 maximum fluoride removal was observed at pH 9 and fluoride
concentration remaining was 0.12 ppm.

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CHAPTER 4
COMPARISION OF DEFLUORIDATION USING BRICK POWDER AND BASIL LEAVES
and CONCLUSION

CHARACTERISTICS BRICK POWDER BASIL LEAVES

OPTIMUM DOSAGE 0.6g/100ml 0.75g/100ml

pH RANGE 6-8 6-8

OPTIMUM CONTACT TIME 60 minutes 20 minutes

% REMOVAL About 50% About 80%

Table 4.1 showing comparison of defluoridation using brick powder and basil
leaves

Conclusion
From the results obtained it can be concluded that both brick powder and basil
plant can be used as defluoridating agents. The resulting concentrations of
fluoride after treatments were under within the permissible limit of Indian
Standard for drinking water (IS 10500:1991, Fluoride 1.0-1.5 ppm) and thereby
fluorosis and other adverse health effects on human being can be minimized. The
techniques adopted are easy to understand and less expensive, hence has
potential to be adopted throughout India as adsorbents to remove excess fluoride
in water.

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REFERENCES
1. World Health Organization: Industrial Pollution Control Handbook, H.F. Lund,
1971, McGraw Hill Book Co., New York, p. 4/23-4/39 (1994).
2. Shiv Pratap Raghuvanshi, Renu Singh and Chandra Prakash Kaushik, Asian Journal
of Chemistry (2008)
3. Rahul K Kambul Indian, Journal of Environmental Protection 32(1):37-44 (2012)

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