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Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

MODULE II
(Part II)
Sensors and their applications: Introduction, working principle and applications of
conductometric sensors, electrochemical sensors, Electrochemical sensors for the
pharmaceutical applications, electrochemical gas sensors for Sox, NOx and optical
sensors, Disposable sensors in the detection of biomolecules.

Sensors
A device which gives real time analytical information about a test sample is
known as sensor. Test sample is known as analyte. Sensors are designed to satisfy the
growing demand for development of new instruments, techniques, and procedures,
which makes analysis convenient, fast, reliable, and accurate

Need for Sensors


Detection of emissions of anthropogenic pollutants in to environment
contributing to increase in incidences of chronic diseases. Toxic gases, metals, pesticides,
and other dangerous chemicals have spread throughout our environment. Monitoring of
composition of air, water and soil has become an area of intense interest. In health sector,
for diagnosis and health monitoring, it is required to determine clinically important
chemicals present in body fluids. For various industrial and agricultural applications
qualitative detection and quantitative analysis of chemical species is the major
requirement.

Parts of Sensors:
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

Sensor is composed of three parts: Receptors, transducer and display


Receptor: Receptor detect changes in the environment. It is capable of interacting with
analyte specifically and selectively. It produces a signal corresponding to interaction in
the form of change in potential, conductivity, current, mass, heat.
Transducer: During the interaction of the sensing element with analyte, certain physical or
chemical properties of the sensing element changes proportionately to the analyte concentration.
Transducer is physicochemical device that converts chemical interactions into electrical signals
that could be detected and displayed easily. Most of the time sensing unit and transducer are
packed together in a single unit. In the case of electrochemical sensors, the electrode acts as the
transducer
Electrical signal and display: Electronic system analyses the given signal by the
transducer, helps in a signal amplification and converts the signal from analogue to digital
form. These amplified signals are then displayed. Signals can be displayed in various
forms such as numeric value, graphs images etc.,
Interaction between the receptors and analyte can be monitored by several
methods by measuring change in potential, conductivity, current, heat etc., For each type
of sensors different types of transducers are used. Based on the type of transducer
different types of sensors are reported. Some common examples for sensors which are
most commonly used for analytical applications are: Conductometric sensors,
electrochemical sensors, and optical sensors.

1.CONDUCTOMETRIC SENSORS
Conductometric sensor is based on the measurement of conductance of analyte.
Conductivity cell is used to measure change in conductance and it is connected to digital
conductometer
Unit of conductance: cgs unit: ohm -1 or mho
SI unit: Siemens (S) or milli Siemens (mS)

Most common way of expressing conductance of the electrolyte is specific conductance,


which is the conductance of 1cm3 of the electrolyte.
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

Factors affecting conductance:


1. Temperature: With increase in temperature conductance of the solution
increases. This is due to higher mobility of ions at elevated temperature.
2. The concentration of ions: Conductance is ionic property. Higher the number of
free ions present in the solution, greater will be the conductance. For example:
Hydrochloric acid (HCl)is a strong electrolyte. It dissociates completely in aqueous
solution. Its conductance is much higher when compared with same concentration
of acetic acid (CH3COOH) which is a weak acid. Weak acids dissociate partially in
aqueous solution by liberating minimum number of free ions.
3. The mobility of ions: Mobility of ions refer to the ability of ions to conduct current.
Smaller the size of ions greater will be the mobility and vice versa. For eg: Higher
conductance of HCl is due to highly mobile H+ ions, whose size is very small. When
NaOH is added to HCl highly mobile H+ ions are replaced by less mobile Na+ ions.
Ionic size of Na+ is larger than that of H+ ions. Hence decrease in conductivity is
observed.

Schematic representation of conductivity cell

Conductivity cell consists of a glass tube which is closed at one end (top) and open
at the another end. Inside the glass tube there are two platinum foils each with area of
cross section (a = 1cm2). They are separated by a distance of 1cm (l =1cm). Platinum
plates are covered with finely divided platinum black to increase the efficiency. (It is done
by electrolysis of chloroplatinic acid). Platinum wires, fused to platinum foils are used to
establish contact with digital conductometer.
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

The conductivity cell must be immersed in experimental solution in such a way


that platinum foils are completely immersed in the solution. The ratio between distance
of separation and area of cross section (l/a) is known as cell constant. It is constant for a
given conductivity cell and its unit is 𝑐𝑚−1

Applications of Conductometric Sensors


• In the estimation of acids, bases, and their mixtures by conductometric titration
• To check presence of ionic impurities in water samples.
• To measure acidity or alkalinity of sea water and fresh water.
• Conductometric biosensors are used in biomedicine, environment monitoring, bio
'technology and agriculture related applications.

Conductometric titration of weak acid against strong base


Aim: To determine concentration of a weak acid by conductometric titration with a
strong base.
Principle
In the titration of acetic acid (weak acid) with sodium hydroxide (strong base),
initially for first addition of alkali the conductance falls due to replacement of highly
mobile H3O+ ions by less mobile Na+ ions. Then the conductivity rises as the weak acid
(feebly ionized) is converted into its salt highly ionized sodium acetate and finally it rises
more steeply as excess of strong alkali (highly ionized giving highly mobile OH- ions) is
introduced. This results in one break point on the conductometric titration curve,
corresponding to equivalent points; which is neutralization of acetic acid.
CH3COOH + NaOH → CH3COONa + H2O
Procedure:
50 mL of the acetic acid (CH3COOH) is pipetted into a 100 mL beaker and the initial
conductance of the solution is measured. Then every time 0.5 mL of NaOH is added from
the burette. The solution is stirred well and conductance values are measured. Titration
is continued well beyond the equivalence points. A graph of conductance (L against
volume of NaOH is plotted and equivalent point is determined.
Result:
Concentration of weak acid = ---------------------------- N
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

OBSERVATIONS AND CALCULATIONS


Volume of weak acid pipetted = 50mL Concentration of sodium hydroxide =1.0 N

Volume of NaOH Conductance(L) Volume of NaOH Conductance (L)


( mL) ( m Siemen) (mL) (mSiemen)
0.0 5.5
0.5 6.0
1.0 6.5
1.5 7.0
2.0 7.5
2.5 8.0
3.0 8.5
3.5 9.0
4.0 9.5
4.5 10.0
5.0 10.5
Equivalent points from the graph, V1 = mL.

𝑉1 𝑥 1.0
Strength of the weak acid, N CH3COOH =
50
= -------------N

Advantages of conductometric titration:


1. No visual indicator is required hence results are more reilable and acccuarate
2. Suitable for titration of mixture of acids where no suitbale indicator can be used
Disadvantages of conductometric tiration:
1. Conductometric titration cannot be performed for nonpolar solvents
2. Conductometric titration do not give satisfactory results when concentration of
electrolyte is high
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

2.ELECTROCHEMICAL SENSORS:
Electrochemical sensors use electrodes as the transducer component. Eg:
Potentiometric sensor, electrochemical gas sensors etc.,
Major components of potentiometric sensors are:
• Sensing electrode (working electrode): facilitates redox reaction or change in pH
of the analyte
• Reference electrode: To complete the cell unit

Applications of electrochemical sensors


1. In detection of dissolved oxygen in water boiler and to monitor dissolved oxygen
concentration in metal melts, glasses and in hydrogen fuel
2. In security and defence applications like detection of toxic gases, warfare agents
etc.
3. In water analysis and environmental monitoring, like measurement of toxic metal
concentration in water, detection of oxides of nitrogen and sulphur, CO, pH of
water etc.
4. In diagnostic and health-care applications, like in situ monitoring serum uric acid,
blood Ca2+, Fe2+, Acetylcholine etc.
5.. In soil parameter analysis, evaluation, and in agriculture applications

TYPES OF ELECTROCHEMICAL SENSORS


(a) Potentiometric sensors
Potentiometric sensor mainly determines the analyte concentration by measuring
the variation of potential difference between working and reference electrodes at
different analyte concentrations.
It uses combination of an indicator electrode (working electrode) and a reference
electrode. Indictor electrode can be either inert electrode or ion selective electrode.
Reference electrode is usually saturated calomel electrode. Platinum is an example for
inert indicator electrode which is mainly used for measuring redox potential. Glass
electrode is an example for ion selective electrode. Using ion selective electrode as an
indicator electrode, concentration of particular ion can be measured with good
selectivity. In potentiometric sensors measurement of potential is done zero current
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

[ In amperometric sensors, on the other hand measurement of current is done at


the applied potential. Here, constant potential needs to be maintained between working
electrode and reference electrode. This is achieved by making use of counter
electrode/auxiliary electrode. Thus, amperometric sensors make use of three electrode
system. Pls refer: disposable sensors]
Schematic representation Potentiometric sensor:

In potentiometry surface of sensing electrode is usually modified. A layer catalysts


or enzymes which can facilitate redox reaction are coated. This modification makes
sensor more selective. Recently, miniaturized microelectrodes are used which show fast
response 'time and, can measure small current. Materials commonly used for these
electrodes are noble metals, fluorine-doped tin oxide (FTO) coated glass, indium-tin-
oxide conductive glass (ITO), and different forms of carbon. Now a days, nanomaterials
based on carbon such as graphene, carbon nanotubes and nanofibers, and graphitic
carbon nitride are gaining more attention due to their low cost, appealing electrochemical
properties, ease of functionalization, and wide potential window.

Application of Potentiometric sensors:


In analytical chemistry potentiometric sensors are mainly used for :
(i) Potentiometric titrations: to determine the concentration of unknown solution
(ii) pH determination: of solution, soil sample etc using ion selective electrode
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

Potentiometric titration of Mohr’s salt with standard K2Cr2O7


Aim:
To estimate the weight of Mohr’s salt dissolved in a liter of the given solution by
potentiometric method using standard solution of potassium dichromate
Principle
The estimation of amount of substance present in a solution by the measurement
of EMF is known as Potentiometric titration. Here, emphasis is laid on the change in EMF
of cell with the addition of titrant. A simple arrangement for potentiometric titration has
a reference electrode (saturated calomel electrode) and an indicator electrode (platinum
electrode).
The EMF of the cell containing the solution is determined by adding increments of
the titrant solution until the equivalence point reached and EMF is determined after each
addition. After reaching equivalence point, EMF increases slightly on the excess addition
of titrant.
For the redox potentiometric titration of FAS against K2Cr2O7 the indicator
electrode is a bright platinum wire and the oxidising agent (K2Cr2O7) is placed in the
burette. The reaction proceeds as follows.
3Fe2+ + Cr6+ 3Fe3+ + Cr3+
Presence of Fe2+ and Fe 3+ in the solution gives rise to an oxidation-reduction
reaction at the interface of the electrode and electrolyte, potential of which is picked up
by platinum electrode.
Electrode potential so formed is given by:
0.0591
0
𝐹𝑒 3+
𝐸= 𝐸 + log [ 2+ ]
1 𝐹𝑒
Thus, electrode potential of the indicator electrode depends upon the ratio of the
concentration of oxidized and reduced species in the solution. As the titration proceeds
concentration of Fe2+ decreases and Fe3+ increases. As a result, electrode potential
increases and becomes very large near the end point. At the end point all Fe 2+ will get
converted to Fe3+ .With slight excess of dichromate added, potential now shifts to
Cr6+/Cr3+ resulting in maximum change in the potential.
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

Procedure:
Potentiometric titration: Pipette out 25 mL of the given FAS solution into a clean beaker
and add 5mL of 4N H2SO4. Immerse platinum electrode and saturated calomel electrode
assembly, connect to a potentiometer note down potential value. Fill a clean micro
burette with the given standard K2Cr2O7 solution. Add K2Cr2O7 solution with an increment
of 0.5 mL to FAS solution in the beaker. Stir the solution thoroughly and measure the EMF
after each addition. When the reaction reaches equivalence point, there is a maximum
increase in the EMF value. After the equivalence point, continue addition of K 2Cr2O7 and
take 5 more readings. Plot a graph of ∆E/∆V against volume of K2Cr2O7. From the graph,
determine the volume of K2Cr2O7 at the equivalence point.

Result:
Weight of FAS present in litre of solution = ---------------------------g
Observations and calculations
Volume of FAS solution pipetted: 25mL
Concentration of potassium dichromate: 0.5N
Volume of Potential Change in Change in EMF
K2Cr2O7 ( mV) volume ∆E (mV) ∆E
(V mL) ∆V (mL) ∆V
0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0.
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

7.5
8.0
8.5
9.0
10.0

From the graph volume of K2Cr2O7 at equivalence point = V mL _________ mL


Normality of K2Cr2O7 = 0.5N
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐾2 𝐶𝑟2 𝑂7 𝑋 𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 𝑜𝑓 𝐾2 𝐶𝑟2 𝑂7 0.5𝑥𝑉
Normality of FAS = =
25 25
= ---------------------- N
Weight of FAS in 1 litre = Normality of FAS × Equivalent weight of FAS (392.24)
= N × 392 g
= g

Advantageous of potentiometric titration


1. Potentiometric titrations can be carried out in coloured solution and non polar
solutions
2. More than one graphical method is available for accurate determination of end
point
Disadvantageous of potentiometric titration
1. The procedure takes longer time when compared with volumetric titration using
indicators
2. Slight variation in pH of solution, or concnetration generally alters the result of
the experiment
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

pKa value of vinegar using pH meter and Glass electrode


Aim
To determine the pKa value of vinegar ( weak acid) by pH titration method using standard
solution of sodium hydroxide.
Principle
Vinegar is commercial name for acetic acid which is a weak acid. It dissociates in
its aqueous solution only slightly, as follows;
CH3COOH + H2O ⇌ H3O+ + CH3COO-
The equilibrium constant of dissociation of the acid known as dissociation
constant of the
acid, Ka is given by:
[𝐻3 𝑂+ ] [𝐶𝐻3 𝐶𝑂𝑂 − ]
𝐾𝑎 =
[𝐶𝐻3 𝐶𝑂𝑂𝐻]
𝐾𝑎 [𝐶𝐻3 𝐶𝑂𝑂𝐻]
[𝐻3 𝑂+ ] =
[𝐶𝐻3 𝐶𝑂𝑂− ]
Multiply by (− 1) 𝑎𝑛𝑑 take log on both sides:
[𝐶𝐻3 𝐶𝑂𝑂𝐻]
−𝑙𝑜𝑔[𝐻3 𝑂+ ] = −𝑙𝑜𝑔𝐾𝑎 − 𝑙𝑜𝑔
[𝐶𝐻3 𝐶𝑂𝑂− ]
[𝐶𝐻3 𝐶𝑂𝑂− ]
𝑝𝐻 = 𝑝𝐾𝑎 + 𝑙𝑜𝑔
[𝐶𝐻3 𝐶𝑂𝑂𝐻]

This is Henderson’s equation.


When acetic acid (titrate) is titrated with NaOH solution (titrant), pH of the
titrated solution increases in accordance with the above equation; since concentration of
sodium acetate, [CH3COO-] increases and concentration of unreacted acetic acid,
[CH3COOH] decreases as the titration progresses. When the acid is half - titrated,
[𝐶𝐻3 𝐶𝑂𝑂− ] = [𝐶𝐻3 𝐶𝑂𝑂𝐻]
and hence pH ≡ pKa
That is, pKa of the acid is pH of the half-titrated acid solution or pH of the titrated solution
at half way to the equivalence point or end-point.
Acetic acid can be titrated potentiometrically, using a pH sensitive glass electrode
as indicator electrode and saturated calomel electrode as reference electrode. These two
electrodes are connected to a pH meter to measure the pH of the titrated solution after
each addition of NaOH solution from a burette. A graph is plotted taking volume of NaOH
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

added along the X-axis and pH along the Y-axis. Volume of NaOH needed for the complete
neutralization of the acid must be determined from the graph by dropping a
perpendicular to the volume axis from the equivalence point (point of inflection or point
of maximum slope) on the graph (VmL). From the graph, with the knowledge of
equivalence point ( VmL) volume of NaOH needed to neutralize half the amount of acetic
acid is determined. ( V/2 mL) pH value measured at half equivalence point is the pKa of
acetic acid.
The pH meter should be standardised using a buffer solution of known pH in order
to set the pH meter to read the pH of the titrating solution directly from the meter as
accurately as possible. This is necessary as a glass electrode has to be standardized in a
buffer solution of known pH due to different asymmetric potential values of different
electrodes.
Procedure:
Standardization of pH meter: The combined electrode is dipped in the buffer solution of
known pH taken in a beaker. The electrode is connected to the pH meter. Now the meter
should show the pH of the buffer. If it does not show the correct pH, the control knob must
be operated until the meter shows correct pH. Now the pH meter is standardized.
Potentiometric titration: 25 mL of the given weak acid is pipetted into a beaker. The
combined electrode is dipped in the solution after rinsing it with distilled water. The
electrode is connected to the pH meter and the pH of the acid is noted down before adding
any NaOH to it.
Exactly 0.5 mL of NaOH is added from a semi-micro burette and solution is stirred.
pH of the resulting solution is noted down. Addition of NaOH is continued until
comparatively a large change in pH is observed. Addition is continued upto 10 mL.
Now a graph is plotted taking the volume of NaOH along the X-axis and pH along the
Y-axis. pKa value is determined from the graph.

Result
𝑝𝐾𝑎 of vinegar (weak acid) :
Observations and Calculations:
Volume of NaOH added (mL) 𝑝𝐻 ∆𝑽 ∆𝒑𝑯 ∆𝒑𝑯
∆𝑽
0.0
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10
11
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

(b) Electrochemical gas sensor:


Electrochemical sensors react with the measured gas and generate an electrical
signal proportional to the gas concentration. Most electrochemical gas sensors are
current sensors, producing a current that is linearly proportional to the gas
concentration.
Electrochemical gas sensor is used in monitoring of concentration of gaseous
analytes. They are used mainly to monitor the concentration of air pollutants, detection
of leakage of chemicals in industries, and in defence, military and space applications.
Working principle:
Gas passes through a diaphragm that prevents condensation, and this diaphragm
also has a dust-proof effect. The gas molecules then diffuse through the filter and reach
the working electrode. Here, the gas is oxidized or reduced, and this electrochemical
reaction causes a change in the current flowing through the external circuit.

Sensors based on electrochemical working principles, the simplest is a two-electrode


system. Its working electrode and opposite electrode are separated by electrolyte and
connected to the external circuit with a small resistance. When the gas diffuses into the
sensor, it reacts to generate an electric current. The more gas the greater the current

Detection of N02:
Indicator/sensing electrode: Au, Pt/Nafion (It is class of synthetic polymers with
ionic properties)
Reference electrode: Au
Electrolyte: 10 M H2SO4
𝑁𝑂2 + 2 𝐻 + + 2 𝑒 − → 𝑁𝑂 + 𝐻2 𝑂
Detection of NO:
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

Indicator electrode/ Sensing electrode: Au/NAFION,


Reference electrode: Au
Electrolyte: NaN02.
NO + 2 H2O → 𝑁𝑂32− + 4𝐻 + + 3𝑒 −
Detection of S02
Sensing electrode: Au/Nafion
Reference electrode: Au
Electrolyte: 0.5 M H2S04
𝑆𝑂2 + 2𝐻2 𝑂 → 𝑆𝑂42− + 4𝐻 + + 2 𝑒 −

(c) Electrochemical sensors for the pharmaceutical applications


Pharmaceuticals are basically organic compounds, which are used extensively by
human beings as a solution for various health issues. After usage these are excreted or
washed off by their hosts and enter into the environment through effluents of waste
water. Even though use of pharmaceuticals for various health conditions understood and
documented, there is limited knowledge about their unintended effects in the
environment. Majority of these are complex organic molecule with lower
biodegradability. Therefore, it is necessary to use, sensors ‘for the detection of
pharmaceuticals to monitor their concentration and know their toxic effects. Several
electrochemical sensors are available for the detection of pharmaceuticals in lower
concentration. These sensors are fast, low-cost, and sensitive and use disposable strips.

Electrochemical sensor for detection of diclofenac


Diclofenac with chemical, name 2-(2-((2,G-dichlorophenyl) amino) phenyl) acetic
acid, is one of the most frequently prescribed non-steroidal anti-inflammatory drugs
(NSAID) with antipyretic and analgesic effects. It is safe in prescribed dose, but may cause
adverse effects at higher doses. Due to wide usage and poor biodegradability, it can have
serious effects on the ecosystem.
Electrochemical sensor can be used to detect diclofenac in lower concentrations.
In the electrochemical sensor used to detect diclofenac, sensing (working) electrode is
graphite carbon coated with multi walled carbon nanotube (MWCNT) and gold
nanoparticles. In the detection, along with sensing electrode, counter electrode and
reference electrodes are used. When the sample containing diclofenac is put in the sensor,
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

the oxidation of diclofenac occurs on the surface of the sensing electrode. The change in
potential of the reaction gives the concentration of diclofenac.

Ref : https://doi.org/10.1016/j.talo.2020.100026

3. OPTICAL SENSORS
Sensors based on the transduction of interaction of electromagnetic radiation with
the chemical species are called as optical sensors.

Optical transduction can be based on emission, absorption, reflection or scattering


of light by the analyte. Interaction could results in emission, absorption, reflection or
scattering of light . Type of interaction depends on the wavelength of radiation and on the
structure of molecule. Intensity of light scattered depends upon the concentration of the
analyte. It is measured by optoelectronic instrumentation. Simple optical sensors are
used to determine the concentration of coloured chemical species in solution. They are
based on measurement of absorbance of transmittance of light of particular wavelength.
They are based on Beer-Lambert’s law.
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

Lambert’s law relates to the transmission or transmittance and the thickness of


the absorbing medium.
It = Io. 10−𝐾𝑡 (1)
where It = intensity of the transmitted light, Io = intensity of incident light, t = thickness of
the light absorbing medium and K = a constant called absorptivity.
Bear’s law relates to the transmission or transmittance and the concentration of
the colored constituent in solution.

It = Io. 10−𝐾 𝐶 (2)
where C = concentration of the coloured constituent in solution and 𝐾 ′ = a constant.
Combining equations (1) and (2):
′ 𝐶𝑡
It= Io 10−𝐾 𝐾 = It/Io = 10−𝜖𝑐𝑡 ∈ = 𝐾 𝐾′ (3)
∈ is called molar absorptivity.

Taking log, log Io/It = ∈ct (4)

This is the fundamental equation in colorimetry and is known as Beer-Lambert


Law. The ratio, log Io/It is called absorbance (A) of the light absorbing medium. The ratio
of intensity of transmitted light and intensity of incident light is called Transmittance (T).
Since ‘∈’ is a constant and if thickness of the medium ‘t’ is kept constant, then absorbance
is directly proportional to the concentration of coloured constituent in solution and the
path length or thickness of the medium
A ∝ 𝐶𝑡 (5)
Modern optical sensors uses lens, optical couples connectors for coupling light. It makes
the instrument portable.

Applications of optical sensors


1. Optical sensors can be used in the determination of any chemical species which
can interact with electromagnetic radiation.
2. Optical sensors find important and varied uses in environmental,
biotechnological, food, pharmaceutical, medical, and related applications.
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

Estimation of weight of copper in industrial effluent by colorimetry


Aim
To determine the weight of copper present in 50 mL of industrial effluent by colorimetry.
Principle
Colorimetric analysis depends upon the measurement of quantity of light
absorbed by a colored solution. According to Lambert’s _Beers law:
A ∝ 𝐶𝑡
Where
A = Absorbance
C= Concentration of electrolyte
t = path length through which light travels
The ammonium ion reacts with cupric ion to give the complex [Cu(NH3)4]2+ which
has an intense blue color. The quantity of light absorbed by these colored ions can be
measured using a colorimeter.
Cu2+ + 4NH3 → [ Cu(NH3)4] 2+
Series of solutions containing different known concentration of the cupric ions are
prepared and they are treated with ammonia solution to get cuprammonium complex.
Their absorbance is measured in colorimeter at maximum wavelength 𝜆𝑚𝑎𝑥 of 620nm.
The absorbance is plotted against the corresponding volume of copper solution taken. A
straight line is obtained. From the graph the volume and hence concentration of unknown
solution can be found out by measuring under similar conditions, its absorbance.
Procedure:
Prepare a series of copper sulphate solutions in 50 mL standard flasks by pipetting
5, 10, 15, 20, 25 mL of standard copper sulfate solution (containing 1mg of Cu per mL,
Mol wt of CuSO4 5H2O = 249.7) separately. Add 5mL ammonia to each flask. Dilute the
solution up to the mark with distilled water. Shake well for uniform concentration.
Take a 3N ammonia solution in a cuvette. Place in the proper position in the
colorimeter. Select a suitable filter and the adjuster is rotated to bring the scale reading
to 100 percent transmittance or ‘zero’ absorbance. This is called ‘blank setting’
Take each of this solution of known concentration in the cuvette and measure the
absorbance. Then take copper solution of unknown concentration in 50 mL standard flask
is diluted with 3N ammonia solution. Make up to the mark with distilled water Measure
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

the absorbance. Plot a graph of absorbance against volume of copper solution. From this
graph, calculate the concentration of copper in the given solution.
Result:
The weight of copper in given industrial effluent = ---------------mg

OBSERVATIONS AND CALCULATIONS:


Weight of CuSO4 5H2O present in 1mL of standard solution = ( 1/250) = 0.00401g

63.54 𝑥0.004𝑥1000
Weight of Cu present in 1 mL of standard solution: = = 1.0221𝑚𝑔
249.7

Volume of standard solution of CuSO4 Volume of


Sl. ( V mL) Ammonia
No. solution ( mL) Absorbance

1 0 ( blank) 5
2 5 5
3 10 5
4 15 5
5 20 5
6 25 5
7 30 5
8 Test solution 5

From graph : Volume of test solution = V mL


Weight of copper in the test solution = V x 1.0221 =
---------------mg
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

4. DISPOSABLE SENSORS:
Disposable sensors find majour applications in spot analysis and can be disposed
immediately after use. They should be economical, easy to use with small quantity of the
sample. It is a special type of paper, over which receptor and electrodes are coated. They
are coated using screen printing technology. All electrodes and bio receptor are printed
on a single plat form. These are called screen printed electrode.

Disposable sensors in the detection of biomolecules:


Monitoring of levels of biomolecules like carbohydrates, proteins, lipids, nucleic
acids, enzymes, hormones, etc. is very essential to maintain a healthy body. Any
deficiency or excess of these molecules may result in biological disorders such as
Alzheimer's disease, Parkinson's diseases, diabetes, heart attack, pregnancy
complications, osteoporosis, etc . These results in decreased average life-span of the
humans. Several types of disposable biosensors have been developed for continuous
monitoring of these bio analytes. Disposable pre-activated screen printing electrodes
have been developed for on spot analysis of glucose, ascorbic acid, uric acid, creatinine,
lactic acid and dopamine in human blood samples

Disposable sensors for Ascorbic acid


Sensing or working electrode: The ascorbate oxidase enzyme immobilized on a
screen printed carbon electrode with poly ethylelene glycol and diglycidyl ether as cross
linking agent.
Compiled and edited by : Dr Padmalatha Rao Prof & Head, Dept of Chemistry

It oxidises ascorbic acid into dehydroascorbic acid. Concentration of ascorbic acid is


determined by change in potential of the oxidation process.

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