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Instrumentation

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• pH Meter
• pH Electrodes
• Temperature Probe
• Magnetic Stirrer

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• 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.

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• 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.

•The pH electrodes have both H+ ion sensitive electrode and an additional reference electrode.5 •Usually within the electrode tube is a buffered solution of chlorides. .

. • This prevent the pH readings from oscillating. Temperature Probe • It is an inbuilt sensor which reads the temperature of the testing solution or sample.6 The Stirrer • It is an electromagnetic device which ensures that ions are distributed uniformly in solution.

Principle of Operation .

00 buffer and observe reading • Rinse electrode with distilled water • Immerse into the 2nd solution (pH 4.8 CALIBRATION / STANDARDIZATION • At least 2 buffer solutions of known pH are used • Commercially available buffers have pH of 4.01.00) and observe the reading 8 . immerse electrode into pH 7.01 or 10.00.00 • First step related to temperature correction • Secondly. 7. 10.

9 Measuring pH of Solutions • Put the temperature probe into the solution • Put the indicator electrode (say glass electrode) into the solution 9 .

10 •The thin walled glass bulb consist of a lattice of metallic ion which are + exchanged for H ions of the solution 10 .

1M HCl 11 .11 • 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.

12 • 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.Electrode constant 12 .Emf / potential difference • K.0592pH • E.

Care of Electrodes .

14 A faster response. more reliable measurements and a longer lifetime. • Care prior to use • Care in use • Care in storage • Preventive maintenance 14 .

15 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. 15 .

Do not rub! Keep the electrical parts of the electrode (the cable and connector) dry at all times.16 CARE IN USE The electrode should be rinsed with a wash bottle of purified water between measurements. Blot the electrodes dry with a Kimwipe. 16 .

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. • Never store the electrodes in distilled water. will result in measurement errors or slow response.17 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. 17 . • Contamination to the membrane and diaphragm.

depends on the hydration of the glass layer. . • The proper functioning of the electrode. • The best procedure for rehydrating the glass is to soak the probe in a buffer of pH 4.0.18 • Store dry if electrodes will not be used for 2weeks plus.0 solution does the trick. If this does not work then immersing the probe in hot buffer 4.

1M HCl briefly ▫ Immersing bulb in alkaline and acid solutions (reduces Na+ effect ) ▫ Immersing bulb in 20% NH4F for 3mins.19 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. .

20 Modern Advancement in Technology .

21 . some pH applications require temperature compensation to ensure standardized pH values. • Accuracy: accuracy of ± 0.21 pH Selection Considerations • Media conditions: pH values are temperature dependent.02 is most desirable.

22 Electrode compartm ent pH Dial Galvanometer gauge .

23 Waterproof MultiParameter Handheld Meters The ph -2100 PA 23 MP230 GLP Research pH/mV/°C Met .

• Simultaneous temperature display • Accuracy: +/.24 • The glass electrode comes complete with internal reference electrode and internal filling solution system. 32-176 °F • The meter can be recalibrated with digital calibration using the push buttons.02 pH • Electrode: Replaceable glass sensor and reference tube electrodes • Temperature Range: 0-80 °C.0. rather than a screwdriver. .

25 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 .

   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.27 • Other analytical tools. 27 .

.28 •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 28 point.

• Visual determination of the end point of a color indicator titration is relative. • Calibration of pH meter provides the most accurate and dependable measurement possible. 29 .29 • Color indicators only give the end point of a titration whereas potentiometry gives the equivalence point. • Multiple endpoints for polyprotic acids are identified.

Uses in Pharmacy .

31 • To determine the pH and pKa of weak acids • The use of the pKa to determine the extent of dissociation of some drugs.g. aspirin • To determine the body fluid tonicity 31 . 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.

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 32 .32 • To determine the concentration of potassium.

Potentiometric Titrations .

its pKa may also be determined graphically. • Depending on the analyte. thus be it a weak acid. .34 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.

at half neutralization point. . • pH=pKa+ log[base] [acid] • However this holds only for monoprotic acids and only when the [base]=[acid].35 Derivation of pKa Value • The pKa value is determined using the Henderson-Hasselbek equation. pH=pKa. It is said that.

36 • For diprotic acids. 2 • For triprotic acids. pH=pKa at V. pH=pKa at V. V=V1+(V2-V1) hence. V=V2+(V3-V2) hence. 2 .

37 Monoprotic Acid .

38 Diprotic Acid 38 .

39 Triprotic Acid .

Thank you .