Download as pdf or txt
Download as pdf or txt
You are on page 1of 34

ANALYTICAL CHEMISTRY

Types of Titration &


G20 Titrator

Ahmed Talaat Elnagar


Chemist (EHC) , Organic Instructor ,
Analytical Chemistry pre-Master(SU),
Master degree Student
Index
1. Types of Titration
2. Introduction to G20 Autotitrator
3. Titrator configuration
4. Installation
5. Procedure
6. Calibration
7. Measuring samples
8. Recognizing of the end points.
What is Titration?
● A quantitative and volumetric technique, to determine the unknown
concentration of a solution by the known concentration of a solution in the
presence of indicator is called Titration.

Types of Titration.
 Acid-base Titrations
 Redox Titrations.
 Precipitation Titrations.
 Complexometric Titrations.
1. Acid-Base Titration
● The strength of an acid can be determined using a standard
solution of a base. This process is called acidimetry.

● The strength of a base can be found with the help of a standard


solution of an acid, which is known as alkalimetry.

Acid + Alkali → Salt + Water


2. Redox Titrations
● The redox titration is also known as oxidation-reduction
reaction.

● In this type of titration, the chemical reaction takes place with a


transfer of electrons in the reacting ions of aqueous solutions.

● The titrations are named after the reagent that used as follows;
 Permanganate Titrations
 Dichromate Titrations
 Iodimetric and Iodometric Titrations
Permanganate Titrations
● the potassium permanganate is used as an oxidizing agent.

● It is maintained with the use of dilute sulphuric acid.


Here is the equation.
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]

● the solution remains colourless before the endpoint.

● The potassium permanganate is used to estimate


oxalic acid
ferrous salts
hydrogen peroxide
oxalates
Dichromate Titrations
● potassium dichromate is used as an oxidising agent in acidic medium.

● The medium is maintained acidic by the use of dilute sulphuric acid.


● The potential equation is:
K2Cr2O7 + 4H2SO4 → K2SO4 + Cr2(SO4)3 + 4H2O + 3[O]

● The solution of potassium dichromate can be directly used for titrations.

● It is mainly used for the estimation of


 ferrous salts
 Iodides
 Chloride by Moher
Iodimetric and Iodometric Titrations
● The reduction of free iodine to iodide ions and oxidation of iodide ions to
free occurs in these titrations.

l2 + 2e →
– 2l …………….
– (reduction)
2l → I2 + 2e ……………. (oxidation)
– –

● The solution is used as an indicator.

● Free iodine is used in the iodometric titration.

● the iodometric titration an oxidation agent is used to react to liberate free


iodine.
3. Precipitation Titrations
● The titration is based on the insoluble precipitate formation
when the two reacting substances are brought into contact is
called precipitation titration.

● when the solution of silver nitrate is used to a solution of


ammonium thiocyanate or sodium chloride, it reacts and forms
a white precipitate of silver thiocyanate or silver chloride.

AgNO3 + NaCl → AgCl + NaNO3


AgNO3 + NH4CNS → AgCNS + NH4NO3
4. Complexometric Titrations
● The complexometric titration is where an undissociated complex
is formed at an equivalence point.

● It is greater than the precipitation titrations, and there will be no


error due to co-precipitations.

Hg2+ + → Hg(SCN)2
2SCN–

Ag + 2CN → [Ag(CN)2]
+ – –

● Ethylenediaminetetraacetic acid (EDTA) is an important reagent


that forms complexes with metals.
1. Introduction
● The Titrator in the Titration Compact Line perfectly combine
simple, easy-to-understand operation with an extremely high level
of precision and outstanding reliability.

● Titration Compact devices can either be controlled


by touchscreen or by using LabX PC software
2.Titrator configuration
3.Installation
Connecting the power supply :
The titrator is operated using an external power supply unit.

1. Connect the power supply unit to the "POWER SUPPLY"


socket on the rear of the titrator and to the mains supply.
2. Secure the connection at the
titrator by screwing the plug
connector firmly into place.
3.Attaching the titration stand to the titrator :
● The titration stand is already equipped with
a spacing ring, clamping ring and threaded
ring.

● The titration stand must be attached to the


titrator Position the titration stand over the
mounting hole and screw in tightly using the
clamping screw provided .
4.Connecting the titration stand :
● Equip titration stand with
 compact stirrer
 sensor
 dispensing tubes
 stoppers
5.Attaching and removing the titration vessel :
● To insert the titration vessel into the titration stand, first make sure that the threaded ring is loosened (a quarter
to half turn is sufficient).

● Then carefully guide the titration vessel upward into the titration stand A and tighten the threaded ring (B) B.

To remove the titration vessel from the titration stand, loosen the threaded ring approximately a quarter to half turn
C, and carefully pull the titration vessel downwards out of the titration stand D.
5.Inserting a burette :
● burettes are equipped with RFID transponder chip on holder (visible by the small, black cover plate D).
● This chip is used for reading and writing properties such as titrate name, concentration or usable life.
Screw the burette and holder onto the titrant bottle (see operating instructions for burettes).
● Turn the arrestment knob in the opposite direction to the arrow.
● Slide the burette either from the left (as illustrated) or from the right over the withdrawal position
B onto the titrator:
● The recesses on the driver arm A must be parallel to the slide-on part of the burette.
The piston rod C must be in the home position.
● Turn the arrestment knob in the direction of the arrow to secure the burette .
● Place the dispensing tube into one of the openings in the titration stand .

Note:
When rinsing burettes and tubes, place tips from dispensing tubes in a waste container.
6.Connecting the measuring electrode and the compact stirrer :
● Insert the measuring electrode into the correct opening in the titration stand.1

● Use the electrode cable to connect the measuring electrode to the "SENSOR" socket on the rear of the titrator.

● Insert the stirrer into the correct opening in the titration stand.

● Connect the stirrer to the STIRRER / PUMP outlet of the titrator .Both the turning on and off, as well and the
stirrer speed are controlled by the software.
Procedure :
1. Turn on G20 from on / off button.
2. Connect G20 to CPU if it not connected using USB Cable .
3. From CPU Click on Start menu >> All Programs >> Labx>>Labx Titration another easy Way Click on
Labx icon on the Desktop .
4. The Labx software is now Open , Click on + sign beside titrators to find our Titrator .
● The following Page will appear ,you will find Labx and titrators method on the left to activate them Click on
+ sign Beside Titrator and Methods also you can find Methods shortcuts on the right , and titration graph on
the middle ,on the top titrator Components menu you can use it to control titrators components individually .

Titrator Components

Measured Value Table

Labx & Titrator


Methods

Titration Graph

Methods shortcuts
Titration results
● before you run any method check the if connected Burette and sensor are suitable for
this method and check the dispensing tube if it Contain any bubbles or Air Dispense it
by Choosing Burette Symbol from titrator components menu on the top then choose
the volume then Click on Play Button .
● To run method go to Methods shortcuts and choose it by double click on it's icon the
following box will appear , if V (mL) Box is Active add your sample volume or Weight
then Click Start.
Notes
● The following message will appear on Titrator screen " add sample 1/1 " click ok to
start titration.

● After the titration is end the titrator will stop automatically and
give you results according to your method calculations .
● Clean your vessel , Stirrer , Dispensing tube , Sensor after Titration and keep your:
 DP 5 Phototrode in Demi water.
 DG 115 Potentiometric in Buffer 4 or 3M KCl solution .
Calibration
How to calibrate PH sensor
From Method icon, select M436 method “calibration DG 115-SC”, then press start.
Or from home screen , press Cal shortcut , then press start
Or from labx software press right click on calibration DG 115-SC method then select run
Then rinse the electrode with Demi water.
 Put buffer PH 4, then ok
 Then put buffer PH 7 then ok
 Then put buffer PH 10, then OK
 Wait unit the sensor finished updating results
 From the results, if slope of electrode from - 55 to - 65
 The calibration is Ok
Measuring Samples
How to analysis sulfuric acid sample
 Open method icon , select sulfuric content (EP) method.
 Or select method from home screen, select sulfuric shortcut.
 Or from labx software press right click on sulfuric content (EP)
method then select run.
 press start, insert weight of sample 0.5 to 1 g in sample size icon.
 Then start, put sample beaker in titrator, then OK .
How to measure PH for any solution
 Open labx software from desktop Pc
 From Manual operations (upper task bar of labx)
 Then select measure, select sensor type from table (PH; DG 115-SC;
PH, sensor, Pnp)
 Then press on play icon
 May be, you need to change time of stirring from table.

How to make manual titration to determine concentration of titrant 0.1 N NaOH

 Take volume of sulfuric acid std solution in conical flask, then put
mixed indicator.
 Then from manual icon, select burrette, then manual titration, then
press dispense drop by drop.
How to create new method from Labx software

 Press right click on methods, select new method, then Gx, then Mettler.
 Select any method will be comply with your application, for example
end point method or equivalence point.
 Then change title to create new method.
 Then change parameters in this method to adjust your method, for
example
 Titrant name
 Equation
 Sensor type
Recognizing the Endpoints of Automated Titrations
Different Detection Principles
● The endpoint (EP) can be detected in an automated titration in a number of ways.
● Aside from the visual endpoint recognition (e.g., by the appearance of turbidity, a color change, or appearance
of a precipitate), a titration EP can also be detected by the automated monitoring of a change in a chemical or
physical property which happens once the reaction is complete.
● The table below shows that there are many different detection principles:
Potentiometric Principle
● In the potentiometric principle, the concentration-dependent potential (mV) of a solution is measured against a
reference potential, as shown in the table. So, a silver-silver chloride (Ag/AgCl) reference electrode is utilized
together with a measuring electrode (pH-sensitive glass membrane or metal ring).
● Typically, a combined sensor (electrode) including both measuring and reference electrodes is employed.
Step 1: Start the titration before the titrant is added.
Step 2: Addition of titrant. As the titration nears the endpoint see signs of the color change start to be observed.
At this point in an automatic titration, the sensor will detect an alteration in mV signal, and the titrator starts to
dose the titrant in smaller volumes and at a slower rate.
Step 3: The EP is reached with a faint pink color that corresponds with the inflection point in the titration curve.
Step 4: Titrating beyond the endpoint results in over titration, and the mV signal is fairly constant.
The steps above outline how to achieve the characteristic S-shaped titration curve observed when carrying out
an automated titration. It is not just acid-base titrations that can be converted; Figure 2 demonstrates how a
simple chloride titration can be converted.
Photometric Principle
● Titrations that utilize color indicators are still widely employed, e.g., in pharmacopeias. When manually
performed, the results literally depend on the eye of the beholder.

● Photometric titration it possible to replace this subjective determination of the equivalence point with an
objective process completely independent of the human eye.

● The basis of photometric indication is the change in intensity at a certain wavelength of a light beam passing
through a solution.

● In photometry, the transmission is the primary measured variable and is supplied by the light transmission
(mV or % transmission) of a colored or turbid solution which is measured with a photometric sensor.
● An example of how to convert an EDTA titration of manganese sulfate from manual titration to
automated titration is shown above, and the procedure remains the same.

● One benefit of automated titration is that a lower volume of chemicals is required, resulting in less
waste. The photo electrode is used at a wavelength of 610 nm with the same indicator, Eriochrome
Black TS.
THANK YOU

Best regards,
Ahmed Talaat Elnagar
Lab. Junior Chemist

You might also like