Potentiometer

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Instrumentation

pH Meter
pH Electrodes
Temperature Probe
Magnetic Stirrer

pH-meter is a voltmeter connected to


the ph electrode and measures the
electromotive force across the
electrodes.
Most widely used pH electrode is the
glass electrode
pH electrode have internal resistance
in the range of 10-100Mohm.

Typical model is made of glass tube


ending in a small glass bubble.
Active part of the electrode is the
glass bubble.
The tube is made up of strong thick
glass walls.
But the bubble is made to be as thin
as possible. Its made from Zn and O.

Usually within
the electrode
tube is a
buffered solution
of chlorides.
The pH
electrodes have
both H+ ion
sensitive
electrode and an
additional
reference
electrode.

The Stirrer

It is an electromagnetic device which ensures


that ions are distributed uniformly in
solution.
This prevent the pH readings from oscillating.

Temperature Probe

It is an inbuilt sensor which reads the


temperature of the testing solution or
sample.

Principle of
Operation

CALIBRATION /
STANDARDIZATION

At least 2 buffer solutions of known


pH are used
Commercially available buffers have
pH of 4.01, 7.00, 10.00
First step related to temperature
correction
Secondly, immerse electrode into
pH 7.00 buffer and observe reading
Rinse electrode with distilled water
Immerse into the 2nd solution (pH
4.01 or 10.00) and observe the reading
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Measuring pH of Solutions
Put the temperature probe
into the solution

Put the indicator electrode


(say glass electrode) into the
solution
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The thin walled


glass bulb
consist of a
lattice of metallic
ion which are
+
exchanged for H
ions of the
solution

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A potential difference develops across


the glass membrane
This potential difference developed is
proportional to the H+ ion conc. in the
test solution
To measure this pd is a silver wire
coated with AgCl and immersed in a
0.1M HCl
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The reference electrode produces


a constant ref potential so
changes in emf of setup are direct
indication of variations in pH
The pH meter records the pd in
pH unit
Formula
E=K-0.0592pH

E- Emf / potential difference

K- Electrode constant

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Care of Electrodes

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A faster response, more reliable


measurements and a longer
lifetime.

Care prior to use


Care in use
Care in storage
Preventive maintenance
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CARE PRIOR TO USE


The electrode should be gently
shaken down in the manner of a
fever thermometer.
The electrode should always be
held vertically
For liquid-filled electrodes the fill
hole aperture should be open to the
atmosphere during measurement.
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CARE IN USE
The electrode
should be rinsed
with a wash bottle
of purified water
between
measurements.
Blot the electrodes
dry with a Kimwipe.
Do not rub!

Keep the electrical parts of


the electrode (the cable and
connector) dry at all times.
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CARE IN STORAGE
The pH electrode should be stored in a solution
that is designed to maintain the integrity of the
electrode and prevent the electrolyte solution from
leaching out.
Never store the electrodes in distilled water, as
this will discharge the electrode glass measuring
membrane and make the electrode slow to respond

PREVENTIVE MAINTENANCE

Take care not to allow it to physically bang into the


wall or rim of your testing vials.
Contamination to the membrane and diaphragm,
will result in measurement errors or slow response.
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Store dry if electrodes will not be


used for 2weeks plus.
The best procedure for rehydrating
the glass is to soak the probe in a
buffer of pH 4.0. If this does not work
then immersing the probe in hot
buffer 4.0 solution does the trick.
The proper functioning of the
electrode, depends on the hydration
of the glass layer.

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Rejuvenation of the
Electrode

Deterioration of the glass layer may


cause

Slow response
Failure to check against pair of buffer
solutions

Rejuvenation is done by:


Immersing bulb in 0.1M HCl briefly
Immersing bulb in alkaline and acid
solutions (reduces Na+ effect )
Immersing bulb in 20% NH4F for 3mins.

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Modern Advancement
in Technology

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pH Selection
Considerations
Media conditions: pH values are
temperature dependent, some pH
applications require temperature
compensation to ensure
standardized pH values.
Accuracy: accuracy of 0.02 is most
desirable.
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Electrode
compartm
ent

pH Dial

Galvanometer gauge

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Waterproof MultiParameter
Handheld Meters

The ph -2100 PA

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MP230 GLP Research pH/mV/C Met

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The glass electrode comes complete


with internal reference electrode and
internal filling solution system.
Simultaneous temperature display
Accuracy: +/- 0.02 pH
Electrode: Replaceable glass sensor and
reference tube electrodes
Temperature Range: 0-80 C; 32-176 F
The meter can be recalibrated with
digital calibration using the push
buttons, rather than a screwdriver.

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MI129 ISFET Portable Meter

The ISFET electrode consists of a plastic


bodied probe containing a gel-filled reference,
temperature sensor and silicon microchip

This microchip replaces the fragile glass bulb


on traditional combination electrodes
Facilitates cleaning making ideal for
applications with viscous samples which are
difficult to remove
Unlike glass sensors the use of an ISFET probe
does not require great care or awkward
maintenance
Delivers a stable reading faster than a glass
sensor

Advantages Over Other


Analytical Tools Involved in
Titration

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Other analytical tools;

Colorimeter
Conductivity bridge
Color indicators

A colorimeter is an instrument
compares the intensity of color in
a substance with that of a
standard (control) preparation of
known concentration.
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The only true accurate method for


measuring pH is basically potentiometry.
Marked hydrolysis at the end point of
conductimetric titration reduces
accuracy.
End point is determined electrically
rather than visually hence more
accuracy
Samples under titration may be already
colored hence color change of colored
indicators may be masked at the end
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point.

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Color indicators only give the end point


of a titration whereas potentiometry
gives the equivalence point.
Visual determination of the end point
of a color indicator titration is relative.
Multiple endpoints for polyprotic acids
are identified.
Calibration of pH meter provides the
most accurate and dependable
measurement possible.
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Uses in Pharmacy

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To determine the pH and pKa of weak


acids
The use of the pKa to determine the
extent of dissociation of some drugs,
fatty acids in lipids
This can also be used to determine the
shelf life of some drugs
To determine the percentage active
ingredient in some drugs e.g. aspirin
To determine the body fluid tonicity

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To determine the concentration of


potassium, sodium and creatine in the
urine
Can be applied in redox titration
Concentration of each component in
mixture of strong acid and weak acid
Determination of anionic surfactant
End point of dyes or reactions in which
the salt formed is colored

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Potentiometric
Titrations

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pH Curves

A graph of volume of titrant


against analyte and a first
derivative curve is used to
determine the equivalence
points and hence the end points.
Depending on the analyte, thus
be it a weak acid, its pKa may
also be determined graphically.

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Derivation of pKa Value


The pKa value is determined using
the Henderson-Hasselbek
equation;
pH=pKa+ log[base]
[acid]
However this holds only for
monoprotic acids and only when
the [base]=[acid]. It is said that, at
half neutralization point, pH=pKa.

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For diprotic acids;


V=V1+(V2-V1)
hence, pH=pKa
at V.
2
For triprotic acids;
V=V2+(V3-V2)
hence, pH=pKa
at V.
2

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Monoprotic Acid

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Diprotic Acid

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Triprotic Acid

Thank
you

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