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CE311 Lab 7 Chlorine, Chloride and Fluride

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102 views67 pages

CE311 Lab 7 Chlorine, Chloride and Fluride

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CE311

Environmental Quality and Pollution


Course Instructor : Prof. Abhishek Chaudhary

Department Of Civil Engineering


Indian Institute of Technology (IIT) Kanpur,
India
CONTENT
• Chlorine
a) Definition & Significance
b) Measurements

• Chloride
a) Significance
b) Determination

• Fluoride
a) Significance
b) Determination
Chlorine
➢ Why should chlorine be measured?
❑ Measuring chlorine in drinking water is important for several reasons,
especially in the context of water treatment and public health:
1. Disinfection and Safety: Chlorine is commonly used to disinfect water
by killing harmful pathogens like bacteria, viruses, and protozoa.
Measuring chlorine levels ensures that there is enough chlorine present
to effectively disinfect the water and keep it safe for consumption. Water
treatment facilities are often required to maintain specific chlorine levels
to comply with public health regulations. Regular measurement ensures
that the water meets these legal standards, avoiding potential penalties
and ensuring public safety.
Chlorine

2. Preventing Chlorine By-products: While chlorine is effective in


disinfecting water, it can also react with organic matter if present in high
amounts to form harmful by-products, such as trihalomethanes (THMs).
Measuring chlorine helps control the dosage to minimize the formation of
these by-products.
3. Ensuring Effective Treatment: Chlorine levels need to be sufficient to
maintain a residual presence throughout the water distribution system. This
residual chlorine helps protect the water from pathogens if present in pipes
carrying treated water to homes.
4. Acceptability: High levels of chlorine make the water smell and give it a
bad taste, which will discourage people from drinking it.
Chlorine
➢ What is the chlorine demand?
❑ Chlorine when added to water, reacts with organic and inorganic (e.g.,
metals) substances present in the water, and entire amount of chlorine
that is added is not available for biological disinfection (sterilization). The
total amount of chlorine consumed is referred as “Chlorine Demand of the
Water.” This includes chlorine used in reaction with organic, inorganic
substances plus disinfection. Chlorine takes time to kill organisms.
➢ What is contact time?
❑ Contact time is the amount of time that the chlorine is present in the water.
The combination of residual chlorine and contact time determines the
effectiveness of the chlorination treatment. At temperatures of 18OC and
above, the chlorine should be in contact with the water for at least 30
minutes. If the water is colder then the contact time must be increased.
Chlorine
➢ What is meant by residual chlorine?
❑ If enough chlorine is added, some will remain in the water after all
possible organisms have been destroyed. What is left is called residual
chlorine. Residual chlorine will remain in the water until it too dissipates or
is consumed in destroying new contamination (e.g., in pipes).
❑ The higher the residual chlorine levels in the supply, the better and longer
the chemical will be able to protect the water supply system from
contamination. However, too high levels of chlorine make the water smell
and give it a bad taste, which will discourage people from drinking it.
Chlorine
➢ Disinfection
❑ It is the process of removal of disease-causing microorganisms from the
water (i.e., pathogens).
❑ The process of removal of all types of microorganisms is termed as
STERILIZATION.
❑ It is the minimum essential treatment required to be given to water and is
adopted as the final stage in the chain of water purification process.
❑ Disinfection can be carried out by the following methods:
❖ Physical
▪ Boiling
▪ UV rays
Chlorine
❖ Chemical
▪ Acid and Alkalies (pH < 5, pH > 11)
▪ Metallic Ion (Ag⁺, Hg⁺⁺)
▪ Oxidizing Reagent (Cl₂, Br₂, I₂, O₃, KMnO₄)

➢ CHICK'S LAW .
When microorganisms are exposed to disinfectants, the reduction in
microorganisms follows a 1st order reaction.
Nt = N0 . e-Kt
Where:
N0 = Initial number of microorganisms. .
Nt = Number of microorganisms at any time t.
K = Disinfection constant (depends on chemical and temperature).
Chlorine
➢ Free Chlorine: Concentration of chlorine available for disinfection.
Chlorine
➢ Combined Chlorine: Concentration of chlorine combined with nitrogen
(inorganic) in the water and unavailable for disinfection. We do not consider
organic here because raw water taken from rivers and lakes for disinfection
has very less dissolved organic matter.
Chlorine
➢ Chlorine Compounds Used in Disinfection
❑ Chlorine gas - Cl2

❑ Calcium Hypochlorite or Bleaching Powder - Ca(OCl)2

❑ Sodium hypochlorite - NaOCl

❑ Chlorine dioxide - ClO2 (Cl- is not a disinfectant)

Most common compound used for chlorination is Bleaching Powder

[Ca(OCl)2]. It produces HOCl & OCl- in water.

• Note that it is also used in tertiary treatment in wastewater plants for

disinfection before dumping the water in rivers but there it produces sludge

and hence nowadays its use there is limited.


Chlorine
➢ Addition of Chlorine to Water

❑ Hypochlorous acid (HOCl) is the primary disinfectant used in drinking water


❑ Chlorine gas added to water causes a decrease in pH (increase in hydrogen ions)
❑ The chlorine gas reaction is extremely fast (rate constant = 5x1014)
❑ Sodium Hypochlorite added to water increases pH (sodium hydroxide)
Chlorine
➢ Dissociation of HOCl

This reaction is pH dependent


The ionization constant is:
𝐾𝑖 = [𝐻𝑂𝐶𝑙]/[𝑂𝐶𝑙−].[𝐻+]
The value of Ki varies with temp.
At 150C, Ki is 2.32 x 10-8
pH is critical in disinfection:
❑ The concentration of HOCl for a given measured free chlorine residual is
80% at pH 7 and decreases to only 30% at pH 8.
❑ At pH 6, 98% of the free chlorine residual is hypochlorous acid.
❑ Disinfection is far more efficient at low pH 6.5 as compared to higher pH 8.
❑ Temperature has an effect as well: but it is offsetting with disinfection
mechanism.
Chlorine
➢ Chlorine Demand
Cl2 Dosage = Cl2 Demand + Residual Chlorine
❑ Sequence of Reactions:
1. Firstly, metallic ions (Reducing Agent) in water react with chlorine to get
stable (Fe2+, Fe3+, Mn2+, Mn3+, Mn4+).
2. Next, formation of chloramines & chloro-organics along with the killing of
micro-organisms takes place.
3. Finally, destruction of chloro-organics into various gases takes place.
1 + 2 + 3 → Chlorine Demand
❑ Calculating Chlorine Dose:
Amount of Cl₂ required (kg/d) = Discharge (l/d) x Cl2 dosage (mg/l) x 10-6

Amount of Cl₂ required (kg/d)


Amount of bleaching powder (kg/d) = x 100
% of Cl₂ in bleaching powder
Chlorine
➢ Chlorine Demand
Cl2 + H2O → HOCl + HCl
HOCl H+ + OCl-
Chlorine
➢ Chlorine S-Curve:

❖ Zone 1: Initial chlorine demand is caused by reducing agents (Fe+2 , Mn+2 , H2


S, NO2 ) that consume most of the chlorine applied prior to forming combined
residuals.
Chlorine
❖ Zone 2: Additional chlorine combines with available total ammonia and
reactive organics until forming maximum monochloramine residual. At the
same time, uncombined free ammonia is being depleted until it reaches
zero.
❖ Zone 3: More chlorine dosage converts monochloramine into odorous
dichloramine and nitrogen trichloride. Total combined chloramine residual
decreases and ammonia concentration approaches zero at the breakpoint.
❖ Zone 4: After breakpoint chlorination, most of the chlorine exists as free
residual after breaking down chloramines. This typically results in effective
disinfection and minimal chlorine nuisance.
Chlorine
➢ Chlorine Residuals
❑ Minimum Levels Dependent on where you are on the Curve:

❖ Levels throughout the distribution system


❖ Minimum of 0.3 mg/L free chlorine residual if on the breakpoint side of
the curve
❖ Minimum of 1.5 mg/L total chlorine residual if chloraminating.
❖ Maximum of 4.0 mg/L total chlorine
❖ Based on Running Annual Average (RAA) = MRDL (maximum residual
disinfectant level)
Chlorine
➢ Sampling and Sample Handling and Preservation
❑ As a general guide, the World Health Organization (WHO, 2006)
recommends that one sample per 1000 persons served should
be examined each month for water supply system that serves
up to 100,000 persons.
❑ Preservation of the sample is not desirable. Because biological
activity will continue after sample has been taken, changes
may occur during handling and storage.
❑ If analysis is to be carried out within 2 hours of collection, cool
storage is not necessary.
Chlorine
❑ If analysis can not be started within 2 hours of sample collection,
keep the sample at 40C.
❑ Do not allow sample to freeze.
❑ Do not open the sample bottle before analysis.
❑ Begin analysis within 6 hours of sample collection.
Chlorine

❑ Environmental significance: Active chlorine (free and


combined) should be determined at each stage in the
treatment process of drinking water and in the water pipes in
order to guarantee pathogen-free water.
Chlorine
➢ 1). Determination of the Strength of the Stock Chlorine
Solution: NaOCl vs Na2S2O3
Theory:
Based on your understanding of oxidation-reduction titrations
(N1V1 = N2V2); write down the relevant equations for determination
of the strength of an unknown chlorine stock solution using a
Na2S2O3 (Sodium thiosulphate) solution of known strength.
Chlorine
Procedure:
❖ Prepare “Standard Chlorine Solution” by first taking 10 mL of
stock chlorine solution and diluting to 1000 mL.
❖ Prepare 1000 mL 0.1 M (= 0.1 N) Na2S2O3 solution.
❖ To 25 mL of standard chlorine solution, add 5 mL of glacial
acetic acid and 1 g of KI. Dilute to 100 mL. Titrate using 0.1 M
Na2S2O3 for iodine quantification.
❖ Determine the strength of the unknown chlorine solution in
mg/L as Cl2 .
Chlorine
➢ 2). Determination of the Strength of the Stock Chlorine
Solution: NaOCl vs FAS
Theory
Based on your understanding of oxidation-reduction titrations;
write down the relevant equations for determination of the
strength of an unknown chlorine stock solution using a FAS
(ferrous ammonium sulphate) solution of known strength.
A 1000ml Stock solution is made up of 4g of Chloramine-T. this
solution has a concentration of 1000mg/l of total chlorine.
How is color formed?
Free chlorine complexes instantly with DPD(N,N-diethyl-p-
phenylenediamine) indicator to produce red color. This red color is
discharged when chlorine in the solution is consumed by FAS, thus
signifying the end-point of the titration.
Chlorine
Procedure:
❖ Prepare 0.0028 M FAS solution with freshly boiled distilled
water. Add 0.25 mL concentrated H2SO4 to the bottle. Label,
“Standard FAS Solution”.
❖ Dissolve 24g anhydrous Na2HPO4 and 46 g KH2PO4 in distilled
water. Combine with 100 mL of distilled water to which 800 mg
of disodium EDTA has been dissolved.
❖ Dilute the mixture to 1000 mL and add 20 mg HgCl2 to the
solution. Label, “Phosphate Buffer Solution for Chlorine
Measurement”.
Chlorine
❖ Dissolve 1 g of DPD Oxalate or 1.5 g of DPD sulfate
pentahydrate or 1.1 g of DPD sulfate in 6 mL of distilled water
containing 2 mL concentrated H2SO4 and 200 mg EDTA
disodium salt. Make up to 1000 mL. Store in a brown bottle in
the dark. Label, “DPD Solution for Chlorine Determination”.
❖ Add 5 mL of buffer solution and 5 mL of DPD reagent and mix in
a conical flask. Take appropriate quantity (in mL) of the standard
chlorine solution and dilute to 100 mL (after dilution the
chlorine concentration should be in the range 1-4 mg/L). Add
this diluted solution to the conical flask. Titrate rapidly with FAS
until the red color is discharged.
Chlorine
❖ Determine the strength of the unknown chlorine solution in
mg/L as Cl2 .
• Compare the strengths obtained from two different
experiments done.
Chlorine
➢ Determination of Free and Combined Residual Chlorine in
Water:
Theory
❑ Free chlorine complexes instantly with DPD indicator to produce red
color. This red color is discharged when the chlorine in solution is
consumed by FAS, thus signifying the endpoint of the titration.
❑ Subsequent addition of about 1 g of KI causes the combined chlorine
to complex with DPD (the iodide ion acts as a catalyst in this
complexation process). Further titration with FAS to a colorless
endpoint results in quantification of combined chlorine.
Chlorine
Procedure:
❑ Take 5 BOD bottles and two conical flasks.
❑ Based on determination of the average strength of the chlorine
solution in earlier part of the experiment prepare 100 mL of a
100.0 mg/L stock chlorine (as Cl2 ) solution.
❑ Pour 100 mL of the sample water in each of the 5 BOD bottles.
❑ Add appropriate concentrations of the chlorine stock solution to
each BOD bottle such that the added chlorine (as Cl2)
concentrations in the bottles are approximately 0, 1, 4, 8, and
10 mg/L. Mix well. [Space the chlorine additions 5 minutes
apart.]
Chlorine
❑ Wait for 30 minutes (this gives time for chlorine to react), before
titrating each solution by the DPD Ferrous Titrimetric Method.
❑ Chlorine quantification is done in this case by the DPD Ferrous
Titrimetric Method, which involves the following steps:
▪ Place 5 mL each of the buffer reagent and the DPD indicator
solution in a conical flask.
▪ Add 100 mL of sample (or diluted sample) to this flask and
mix.
▪ Titrate rapidly (this is very important) with the standard FAS
solution until the red color is discharged. This reading (A) is
equivalent to the free chlorine concentration.
Chlorine
▪ Add a small amount (1 g approximately) KI to the sample and
mix to dissolve. Let stand for 2 minutes. If the red color
returns, titrate until the color is discharged again.
▪ This reading is equivalent to the combined chlorine (B)
concentration.
❑ Titrate
▪ Full 100 mL of solutions with 0 and 2 mg/L chlorine dose,
▪ 50 mL of the solution diluted to 100 mL for the solutions with
chlorine doses of 4 and 8 mg/L.
▪ 25 mL of the solution diluted to 100 mL for the dilution with
chlorine dose of 10 mg/L.
Chlorine
❑ Record the volume of titrant required in each case.
❑ For each chlorine dose, determine the concentration of Free
Chlorine (A), Combined Residual Chlorine (B)
❑ Also determine the amount of chlorine consumed by other
reactions in each case. This will be given by the difference
between the added chlorine concentrations and the sum of free
and combined chlorine concentration
Chlorine
➢ Numerical Problem.01

k → disinfection rate constant


r → growth rate constant
Chlorine

%R → %Removal
Here, Chick-Watson Law is Used
Chlorine
Chlorine
Chlorine
Chlorine
Chlorine
➢ Numerical Problem.02
Chlorine
Chlorine
Chloride
➢ Chlorides in Water
❖ Part of Total Dissolved Solids
❖ Commonly Present as Chloride Ion (Cl- )
➢ Sources:
❖ Dissolution of salt deposits
❖ Discharges of effluents
❖ Oil well operations
❖ Sewage discharges
❖ Irrigation drainage
❖ Sea water intrusion in coastal area
Chloride
➢ Why or Significance of Chlorides in Water
❑ Essential elements for various life forms and abundantly
available in nature, particularly in Ocean Waters
❑ Safety Issue for various beneficial uses
❑ Aesthetics aspects for various beneficial uses
❑ Economic Considerations from the point of view of various
beneficial uses
❑ Intake and Excretion by various life forms → Increased levels in
sewage/wastewater compared to domestic water supplies →
Indicator of Pollution due to domestic wastewater
Chloride
➢ Laboratory methods for determination of Chlorides
❑ Precipitation Titration
❖ Chemical
▪ Precipitation Type - Mohr’s method
▪ Adsorption – Fajan’s method
▪ For silver analyses – Volhard method
❖ Sensors – Potentiometric or Amperometric
Chloride
➢ Mohr Method
❑ Direct titration
❑ Basis of endpoint: formation of a colored secondary precipitate
❑ Indicator: Soluble chromate salt (Na2CrO4 , K2CrO4 )
❑ Ag2CrO4 precipitation in neutral pH solution.
❑ Product is colored.
❖ Color forms just after AgCl forms.
❖ Small error involved.
❑ Has to be performed at a neutral or weak basic solution of pH 7-
9 (or 6-10)
Chloride
❑ In a lower pH (acid solution):
CrO42- (aq) + H+ (aq) → H2CrO4
H2CrO4 2H+ (aq) + CrO42- (aq)
❑ In a higher pH (basic solution):
Ag+ (aq) + OH- (aq) → AgOH(s)
Chloride
➢ Volhard Method: Used as a procedure for titrating Ag+ ;
determination of Cl- requires a back-titration:
❖ First, Cl- precipitated by excess AgNO3 (titrant)
Ag+ (aq) + Cl- (aq) → AgCl(s)
❖ Excess Ag+ is titrated with KSCN in the presence of Fe3+
Ag+ (aq) + SCN- (aq) → AgSCN(s)
❖ When Ag+ has been consumed, a red complex forms
Fe3+ (aq) + SCN- (aq) → FeSCN2+ (aq)
Chloride
➢ Endpoint of Titration
➢ Volhard’s method using thiocyanate , SCN- , as titrant. Iron (III) is
the indicator as it forms a red complex ion with thiocyanate ,
SCN- , Fe (SCN)2+
AgNO3 is added in excess. The AgCl precipitate is often filtered
off. Then the excess Ag+ back-titrated with thiocyanate, SCN-
➢ Adsorption – Fajan’s method
A red dye attaches to the silver salt, on the surface of the analyte
precipitate particle.
This happens only when the silver ion Ag+ is in excess, i.e. just
after the equivalence point.
Chloride
One kind is the acid dyes, for example fluorescence yellow and its
derivative, they are the organic weak acid, dissociates the
indicator anion.
Another is the alkalinity dye, like the gentian violet, Luo Danming
6G and so on, dissociates the indicator positive ion.
Chloride
➢ Precipitation Titrations
Analytical Reaction is a Precipitation
❑ Precipitate is not collected and weighed
❑ Calculations are identical to acid-base titrations
❑ Precipitation must be fast
❑ Indicators are difficult to find
❖ Argentometric Titrations involve precipitation of AgX with
AgNO3
❑ Mohr Method: Direct titration of X− with primary standard AgNO3
❑ Volhard Method: Excess AgNO3 used to precipitate AgX. Excess
Ag+ is back-titrated with standardized KSCN.
(Typical analytes include: Cl− , Br− , I− , CN− , SCN− , …)
Chloride
➢ Direct titration of X− with a standard solution of AgNO3
ANALYTICAL REACTION:
AgNO3 + X− → AgX(s) + NO3−
INDICATOR: CrO4 2− ion from K2CrO4
2AgNO3 + CrO42− → Ag2CrO4 (s) + 2NO3−
Yellow Red

AgX(s) precipitates before Ag2CrO4(s)


Titration Error is Important
Titration of a sample containing only K2CrO4 (“blank”) affords
correction: Veq. pt. = Vend pt. − Vblank
Chloride
➢ ANALYTICAL REACTIONS:
1. Add excess Ag+ as standard AgNO3 :
Ag+ + X− → AgX(s)
2. Back-titrate with standard KSCN:
white
Ag+ + SCN− → AgSCN(s)
3. INDICATOR: Fe3+
white
Fe3+ + SCN− → Fe(SCN)2+
AT THE EQUIVALENCE POINT:
red
mmol Ag+ = mmol X− * S.R.X + mmol SCN− * [Link]
Chloride
❑ End-Point Detection
❖ Determine [Cl-]:
▪ First ppt. Cl- by titration with Ag+ and filter off solid
Titrate excess Ag+ with thiocyanate (SCN-).
▪ When all Ag+ is consumed, thiocyanate binds Fe3+.
Appearance of Red color is endpoint.
Total amount of Ag+ is known, so amount consumed by Cl- can be
calculated
Subtract excess [Ag+] from total [Ag+] used to ppt. Cl-
Chloride
➢ Procedure:
➢ Dissolve 2.395 g of AgNO3 in distilled water and dilute to 1000 mL.
Label, “Standard (0.0141 N) AgNO3 Solution”. (This solution will be
available in the laboratory). Store AgNO3 in brown bottle.
➢ Dissolve 50 g K2CrO4 in a little distilled water. Add AgNO3 solution
until a definite red precipitate is formed. Let stand 12 hr, filter, and
dilute to 1000 mL with distilled water.
➢ Label, “Potassium Chromate Indicator Solution”. (This solution will
be available in the laboratory).
➢ Prepare 100 mL aliquots containing 0, 10, 50, 100mg/L chloride. Also
prepare a 100 mL aliquot of sample.
Chloride
➢ To each aliquot add 1 mL K2CrO4 indicator solution
➢ Titrate with standard silver nitrate titrant for chloride
determination, to a definite pinkish-yellow endpoint.
Fluoride
➢ Introduction:
❑ Fluoride is present in most natural waters.
❑ Concentrations vary from 0.05 to 100 mg/L but less than
0.1mg/L is much more common.
❑ Some groundwaters have very high concentrations of fluoride.
❑ In India, at many locations in Rajasthan, Andra Pradesh and
Tamil Nadu the concentration of fluoride is found to be up to 10
mg/L.
❑ 85 % of rural population of the country uses ground water for
drinking and domestic purposes, which contains a high
concentration of fluorides (> 1.5 mg /liter).
Fluoride
➢ Significance:
❑ Skeletal Fluorosis is a chronic bone and joint
disease caused by long term consumption of
Dental fluoride.
❑ As fluoride accumulates in the bones it begins
Caries,
to negatively alter processes of bone formation
Mottling of and resorption- affecting the entire skeleton.
❑ Gradually bones become weaker and more
Teeth, Dental brittle, while joints increase in pain and
stiffness due to skeletal changes.
Fluorosis & ❑ On-going fluoride exposure can lead to
“crippling skeletal fluorosis” the most severe
Skeletal
case of the disease. A result of calcification of
Fluorosis ligaments, immobility, muscle wasting, and
neurological problems related to spinal cord
compression.
Fluoride
➢ Significance:
❑ Fluoride is both beneficial and toxic to humans (Dual
significance in water)
❖ High concentration of F- causes Fluorosis
❖ At too low Concentration (< 0.8 mg/L), results in dental
Caries
❖ Essential to maintain F- concentration between 0.8 mg/L to
1.0 mg/L in drinking water
▪ At low concentrations ( ≈ 1.0 mg/L) it prevents dental caries
▪ At high concentrations (> 4.0 mg/L) it causes dental/skeletal
fluorosis
▪ At intermediate concentrations it causes mottling of teeth
Fluoride

→Dental Caries

Mottling of Teeth←
Fluoride

→Dental Fluorosis

Skeletal
Fluorosis←
Fluoride
➢ How does fluoride affect & What does fluoride do in the
body?
❑ When fluoride is ingested, it is absorbed into the blood through
the digestive tract.
❑ With approximately 50% of fluoride being removed through
urinary excretion, the rest is free to roam and accumulate in the
body.
❑ When fluoride gets into the blood, uptake by bone removes it
from circulation.
❑ This is due to fluoride’s negatively charged nature that allows it
to react with positively charged ions like calcium. Thus,
Fluoride
➢ When fluoride reacts with calcium in your bones, it forms
calcium fluoride (CaF2).
➢ Through this process, fluoride takes the place of naturally
occurring calcium hydroxyapatite in the bone-altering normal
bone formation and resorption.
➢ Leading to weaker and more brittle bones.
Fluoride
➢ Determination of fluoride
❑ Fluoride reacts with certain zirconium dyes to form a colorless
complex that bleaches (removes color) another colored dye.
❑ The dye becomes progressively lighter as fluoride concentration
increases.
❑ The commonly-employed SPADNS method for the
determination of fluoride in waters is based on the effect of the
fluoride ion on the absorbance of the complex formed by
zirconium ion and 2- (parasulfophenylazo)-1,8-dihydroxy-3,6-
naphthalene-disulfonate (SPADNS)
Fluoride
➢ 1). Colorimetric SPADNS Method
➢ Principle:
❑ Under acidic conditions fluorides (HF) react with zirconium
❑ SPADNS solution and the Dark Red-Violet Colour (colour of
SPADNS reagent) gets bleached (faded) due to formation of
ZrF6 . Since bleaching is a function of fluoride ions, it is
directly proportional to the concentration of fluoride.
❑ It obeys Beer’s law in a reverse manner.
Fluoride
➢ Procedure:
1. Preparation of the reagent: 958 mg of SPADNS is dissolved in
distilled water and diluted to 500 ml. 133 mg of zirconyl
chloride octahydrate (ZrCl2.8H2O) is dissolved in 25 ml distilled
water and 350 ml of conc. HCl is added and diluted to 500 ml
with distilled water. Equal volumes of SPADNS solution and
zirconyl acid solutions are mixed.
2. Preparation of calibration curve: 0.221 g of anhydrous sodium
fluoride is dissolved in water and diluted up to one liter. The
stock solution is further diluted to get standard solution having
10 mg per liter of fluoride.
Fluoride
3. The absorbance of the solutions is measured at 570 nm against
a reagent blank and a calibration plot is constructed by plotting
absorbance against concentrations using colorimeter.
4. Suitable aliquot of water sample is taken, and the Step-3
repeated.
➢ SPADNS Spectrophotometric Method – Interference
❑ Substance causing 0.1 mg error at 1.0 mg F- /L
Fluoride
➢ 2). Ion Selective Electrode Method
❑ The fluoride sensitive electrode is of the solid-state type,
consisting of a lanthanum fluoride crystal; in use it forms a cell
in combination with a reference electrode, normally the calomel
electrode.
❑ The crystal contacts the sample solution at one face and an
internal reference solution at the other.
❑ A potential is established by the presence of fluoride ions
across the crystal which is measured by a device called ion
meter or by any modern pH meter having an expanded milli volt
scale.

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