liquid chromatography experiment no: date

AIM: To analyze the liquids by LIQUID CHROMOTOGRAPHY

APPARATUS: 1.Gas cylinder(H2,N2,O2)

2.Samples (Methanol)

3.Flame Ionization Detector

4.DAS

5.Plastic Syringe

PRINCIPLE:

Chromatography is a technique of physically separating the elements present in a

sample and analyzing them. Liquid chromatography is used to analyze transformer oil.

Waste water, chemical etc. when a sample is mixed with a carrier gas at a constant

temperature then it will be burns and ionized, ions will be emitted and the sensor senses

these ions.

PRINCIPLE OF CKT DAIGRAM:

LIQUID CHROMATOGRAPHY

Experiment no:

Date:

PROCEDURE:

1. Open the gases N2,O2,&H2

2. Ensure that the column is connected to FID port

3. Carrier gas should be set 30Psi

4. Set 15 psi column A& column B

5. H2 flow should be set to 14 psi and O2 flow should be set to 7psi

6. Switch on the programmable controller and select PR1

(Current more than 130ma)

7. Switch on the DAS

8. Open the software &create new file

9. Inject the liquids(standard) in column B

10. Press CHN6 to run system

11. Observe the chromatogram on pc & note down the standard peak area

12. Repeat the above steps (8, 9&10).

13. Calculate the % of concentration of liquid (sample) as follows.

Percentage of concentration liquid =(sample area/ standard area)*100.

Where area=(1/2)*base*height.

PRECAUTIONS:

1. Avoid loose connections

2. Don‟t open the oven during experiment.

CONCLUSION:

The experiment is conducted and the amount of H2 in the sample is determined.

VIVA VOCE Questions:

1. Explain the operation of liquid chromatography?

2. Which technique is used for qualitative and quantitative analysis?

3. What are the gases required in liquid chromatography?

4. What are the types of detector used in liquid chromatography?

5. What are the applications of liquid chromatography?

AIM: To analyze the liquids by GAS CHROMOTOGRAPHY

APPARATUS: 1.TCD

2. Gas Chromatography Equipment

3. .DAS

4. H2&N2 gases

5.Micro-Lyte Syringe

PRINCIPLE:

Gas analyzers are used in mines to identify the amount of gases coming from the

earth and in drug industry and also are used whether the transformer is in good condition

or not. When a sample is mixed with a carrier gas at a constant temperature then it will be

burns and ionized, ions will be emitted and the sensor senses these ions.


GAS CHROMATOGRAPHY

Experiment no:

Date:

PROCEDURE:

1. Ensure that the column is connected to TCD port.

2. Open N2 and switch on TCD.

(without N2 flow TCD should not be switched ON)

3. Switch on the programmable controller and select PR1

(Current more than 130ma)

4. Switch on the DAS

5. Open the software &create new file

6. Inject the liquids(standard) in column B

7. Press CHN6 to run system

8. Observe the chromatogram on pc & note down the standard peak area

9. Repeat the above steps (8, 9&10).

10. Calculate the % of concentration of liquid (sample) as follows.

Percentage of concentration liquid =(sample area/ standard area)*100.

Where area=(1/2)*base*height.

PRECAUTIONS:


2. Don‟t open the oven during experiment.

CONCLUSION:

The experiment is conducted and the amount of H2 in the sample is determined.


1. Define chromatography?

2. What is diference between gas & liquid chromatography?

3. What are the gases required in gas chromatography?

4. What are the types of detector used in gas chromatography?

5. What are the applications of gas chromatography?

AIM: To determine the Transmission and absorbance of liquid sample

APPARATUS: 1 Given Sample

2. Distilled Water

3. .Cavettos

4. UV-VIS Spectrometer equipment

PRINCIPLE:

A selectable light beam in UV-VIS Spectrum from the light source module gets

focused on to the entrance slit of monochromater module. The incident light beam of

light gets tuned to key board settable wavelength by motorized slewing of the halo

graphic grating in Czerny turner mount and reflecting optics and emerges as a

monochromatic light of narrow band width from the exit slit of the mono chromate this

narrow band light from mono chromate is switched between the two paths by a rotating

chopper. One for the reference cell (i.e., distilled water) and the other for sample cell. The

transmitted portion if the light thourgh the media(blank,standard,and sample solution) in

the two paths is combined on to a single photo detector. The output of detector pre

amplifier module is processed in the electronics module and the absorbance %

transmittance concentration of the sample medium is present in scan , photometric

concentrations time scan modes.

UV- VIS’SPECTROPHOTOMETER

Experiment no:

Date:


PROCEDURE:

1. Switch On The Instrument

2. Screen will be display “ELICO LTD” & enter

3. Wait till “start base line scan” will be display press “yes”

4. Open the software

5. New file/ setting/ comm. Port /comm. 1.

6. Press “6 pc” mode in spectrometer &press “ok” in software(pc) for interface

7. Now base line scan successfully completed

8. Insert the sample in cavettos

9. Goto . UV-VIS Spectrometer /scan/spectrum/ enter the wave length

10. Click on the “start scan”

11. The spectrum will be displayed

12. Note down the transmittance and absorbance of given sample.

PRECAUTIONS:

1. Check whether the sample empty or not before start the experiment.

2. Clean the cavetti‟s with distilled water after completion of the experiment.

CONCLUSION:

The transmittance and absorbance of the sample was determined.

TABLE:

S.NO SAMPLE

NAME

AT

WAVELENGTH

% OF

ABSORANCE

%OF

TRNASMISSION


1. What is the principle of UV spectrometer

2. What is a Monochromator?

3. What are the samples that can be analyzed by this spectrometer

4. What is the function of detector?

5. What is the light source used to produce UV rays?

AIM: To determine the calorific value of solid or liquid or fuel with Bomb Calorie Meter Equipment

APPARATUS: 1.bomb Calorimeter

2. Benzoic Acid

3. .O2 Gas

4. Nichrome Wire

5. Thread

PRINCIPLE:

Bomb calorimeter is used to find the calorific value of fuel. For this purpose a

known mass of fuel is burnt and the quantity of heat produced by its measure. Which

gives the calorific value of that fuel bomb calorie meter is a strong stainless steel cylinder

in which the fuel is allowed to undergo combustion. Now the temperature of water is

measured, which gives the calorific value of fuel. For proper distribution of heat in the

water chamber stirrer is used.

BOMB CALORIMETER

Experiment no:

Date:

Block diagram of bomb calorimeter:

Where

1. strong cylinder bomb made of stabilized automatic steel

2. stainless steel rod electrode

3. stainless steel rod electrode

4. release valve

5. thermometer

6. battery & firing terminal

7. calorimeter

8. nichrome wire

9. thread

10. air jacket

11. water jacket

12. pellet is placed in crucible

PROCEDURE:

A) Determination of water equivalent of apparatus

For determine the calorific value of solid with bomb calorimeter, the water

equivalent of apparatus must be first asserted. This can be done by burning known

weight of standard benzoic acid in the form pellet and noting the value of benzoic

acid is taken as 6319 cal/ gm. Then the water equivalent can be calculated as

follows

W=HM +(CVt + CVw)

T

Where W----water equivalent in cal /OC H----known calorific of benzoic acid

M---mass of sample in gms CVt---calorific value of thread

CVw-- calorific value of wire T----final rise of temperature

B) Determine Of Calorific Value of sample:

1. Take about 1 gm of sample and place in pellet making device.

2. Apply the compression to produce a pellet.

3. Take the pellet and place in crucible.

4. Attach the piece of nichrome wire to the electrodes of bomb and place the

crucible in the supporting ring between the electrodes

5. A thread of known weight is tied out at the middle of the wire and the end of

the thread is placed in crucible.

6. Pour few drops of water in crucible.

7. Apply the oxygen to bomb.

8. Weigh the calorimeter and pour enough water into it so that the bomb will

submerged but the terminals will remain above the water level.

9. Make the electrical connection and place the cover in a position and switch on

the stirrers.

10. Note the initial temperature then press the fire button.

11. Note down the rise temperature and calorific value of a sample is calculated as

follows

CVs = T *W –(CVt +CVw)

T

CONCLUSION: The process of finding the calorific value of a fuel by using bomb

calorimeter was observed and the calorific value of benzoic acid was measured


1. Define calorific value?

2. What is the value of pressure of O2 in the bomb vessel?

3. Explain the operation of bomb calorimeter?

4. What is the metal wire used for ignition of bomb?

5. Which sensor is used to measure temperature of water?

6. What is the formula for calorific value?

AIM: To determine the content of Na & K in a liquid sample.

APPARATUS: 1.Flame Photometer

2. Gas Cylinder

3. .Distilled Water

4. Standard Na & K Of 40 & 100ppm

5. Small Beakers

6.Capillary

7.Cleaning Wire

PRINCIPLE:

Air at a given pressure is passed into the nebulizer. The suction produced by it

draws the solution of the sample into the nebulizer, from where it emerges as a fine mist

and passes into a mixing chamber this fine mist of sample mixes evenly with gas strem at

a given pressure and the mixer burns at the top of burner.

Radiation from the resulting flame passes through the lens systems and an optical

filter which permits only the radiation characteristics of the element under investigation

in the sample to the photo detector. The output signal from the photo detector is

processed to display of the element in this units desired.

FLAME PHOTOMETER

Experiment no:

Date:

Block diagram:

PROCEDURE:

1. Switch on the instrument and compressor.

2. Set the air to 7 psi through air regulator knob.

3. Then the following operation is performed in the instrument.

4. When the screen displays as “1.Read 2. Calibrate 3.View 4.Print

5. Press “2” for calibrate the instrument with given standards/

6. Now the screen will be display as” 1.General 2.Serum 3.Urine”

7. Press “1” for general mode and then “enter”.

8. Select “1” ,”2” to determine Na and K and “Enter”.

9. Now display will “ 1.segmental 2.quadratic”.

10. Press “1” and “Enter”.

11. Enter the no.of samples.(Min -2 &max -20)

12. Press “2” and then “Enter”.

13. Standard -1 ,Na 40 “Enter” K 40. “Enter”.

14. Standard -2 ,Na 100 “Enter” K 100. “Enter”.

15. Your mid range is 1 &”Enetr”,

16. Feed the blank keep in distilled water “Enetr”.

17. Feed the distilled water to clean and “Enetr”.

18. Save the curve “NO” and the screen will be display as

1.sample 2.rapid 3.view 4.print 5.normal 6.save

19. Now the instrument was calibrated &check with samples.

20. Press “1” for sample determine of Na and K.

21. Enter sample 1 and then sample 2.

22. Press “MODE” for checking the result.

23. Note down the concentration of sample in PPM.

CONCLUSION: The content of Na &K are determined.

PRECAUTIONS:

1. Avoid loose connections.

2. Make constant pressure (9 or 10 psi) during an experiment.

3. After the completing experiment switch off the gas regulator then Gas knob be in off

position

TABLE:

S.NO SAMPLE NAME CONCENTRATION OF

Na(PPM)

CONCENTRATION OF

K (PPM)


1. What is the principle of operation of flame photometer?

2. What is the nebulizer function?

3. Which types of sample are analyzed by this photo meter?

4. What is the color of flame produced in flame produced in flame PM for

different samples?

5. Explain the parts of flame photometer?

AIM: Interfacing of two microcomputers through the serial interface using a serial port.

APPARATUS: 2 Personal Computers &RS-232 cable


PC-TO-PC INTERCONNECT

Experiment no:

Date:

PRINCIPLE:

The electronic industry association (EIA) has produced standard for RS -232 that

deal with data communications. Standard 232 specifies as the interface between data

terminal equipment (DTE) and data communication equipment (DCE) employing serial

binary data “interchanging”

A serial data transmission as shown in fig 1. The DTE is the component that wants

to communicate with another some where else, such as PC communicating with another

PC. The DCE is the component actually doing communication or performing the

functions of generator and receiver. A MODEM (modulator &demodulator) is common

example of DCE. Here RS-232 allows for serial

Data transmission from one transmitter to one receiver. The word serial means the

information is sent to bit at a time data bits are sent with pre defined frequency baud rate.

Both the transmitter and receiver must be programmed to use the same bit frequency.

After first bit readed , the recorder calculates the moments at which other data bit will be

recived

The DB-25 connector (male /female) is standard RS-232 connector with enough

pins to cover all the signals specified in the standard.

PROCEDURE:

1. Switch on the computers.

2. Open the software

3. Select transmit mode for one pc and receive mode in another PC

4. Enter the drive & file name of which you transmit.

Example : d:\eie.doc

5. At receiver side and enter any name of the file.

6. Wait until the dialogue box showing “Transmission over “and

“Receiver” in both transmitting and receving Pc respectively.

7. Check whether the file is received or not in the receiver Pc.

.

PRECAUTIONS:

1. Check whether the RS-232 cable connected or not.

2. Insert the cable carefully

CONCLUSION: Data is transferred between two microcomputers using RS-232C serial

Interface


1. How can you connect PC to PC?

2. What is the difference between RS-232C&GPIB?

3. Explain the pins of RS-232C cable?

4. What is meant by MODEM?

5. What is baud rate?

AIM: a).To prepare the pellet of given sample .

b)To analyze the given sample by using FTIR spectrometer

APPARATUS: 1.Anvil

2. Plunger

3. Top and Bottom guide

4. KBr (potassium Bromide)

5. FTIR Spectrometer


FTIR SPECTROMETER

Experiment no:

Date:

PRINCIPLE:

When we place the sample in sample compartment of IR spectrometer. The

infrared beam is passes through the sample, the energy that transmit through the sample

is measured and spectrum is generated. FTIR spectroscopy is another way of analyzing

the sample. In some ways, it is simpler than dispersive i.e,it has only one moving part

and the entire spectrum can be scanned in few seconds,but the concept behind FTIR is

fairly complex.

PROCEDURE:

A)TO PREPARE THE PELLET

1. Clean the plunger and anvil with solvents to remove grease

2. Assemble the top and bottom guide

3. Insert anvil with polished surface facing with upwards in top guide

4. Fill KBr +2 mg sample (KBr should contain 90% of sample ) on the anvil

surface and spread it using plunger

5. Insert plunger facing polished surface downward

6. Place the small „O‟ ring around the plunger and push it up to the top SS

guide.

7. Place the assembled die on the cover plate if the cylinder o fthe press

8. Apply the vacuum.

9. Close the release knob tuning clockwise

10. Apply the pressure using pump handle. Normal pressure is used is 8 to 10

psi

11. Dismantle top and bottom guides and using extractor ring provided apply

pressure from the receiver side to remove pellet

12. Clean all traces of KBr and store the die desiccators

B)TO ANALYZE THE GIVEN SAMPLE

1. Take the pellet

2. Open the software of FTIR spectrometer and the following operation is

performed

3. Collect the background and “enter”

4. Then “clear” the background

5. Insert the PELLEt into a sample the compartment

6. Click on the “collect the sample”

7. Now the spectrum will be generated

8. Analyze /library set uo/set all the library /add/search and “enter”

9. The sample is measured &spectrum also generated

PRECAUTIONS:

1. Check whether the sample empty or not before start the experiment

2. Clean the plunger and anvil after completion of the experiment

CONCLUSION: The given sample is analyzed


1. Explain the principle of operation of FTIR spectrometer?

2. Which types samples can be analyzed using this FTIR spectrometer?

3. What is the source used to produced IR beam?

4. Which type of detector is used in this spectrometer?

5. What is the filter section used &explain about it?

6. What is the Michelson interferometer technique?

AIM: To the working of ADC by using internal analog inputs that are given to channel.

APPRATUS:

1. Trainer Kit

2. Software And Pc

3. Pates Cards

4. DMM

THEORY:

The analog input is given to DAS and conversion performed with is the system

The principle behind ADC is quantization through the given input. The given input is

splitted into number of levels & each level assigned with a unique digital value.ADC can

be done by using flash type or successive approximation or other method .

PROCEDURE:

1. Connect the circuit diagram

2. Invoke the software

3. Select the analog inputs

4. Choose output channel and type of display required

5. Give the input from DAS board and the output on screen by varying the input

voltage.

PRECAUTIONS:


2. Avoid parallax errors

CONCLUSION: The workings of ADC by using internal analog inputs are observed.

INTERFACING OF AN ANALOG SIGNAL TO THE

MICRO COMPUTER THROUGH ADC

Experiment no:

Date:


PIN DIAGRAM OF ADC0808:

SUCCESSIVE APPROXIMATION TYPE(SAR);

AIM: To study the working of D/A converter when the digital signal are given by the

software

APPRATUS:

1. Trainer Kit

2. Software And Pc

3. CRO

4. Multimeter

THEORY:

The DAS is interfaced with the PC and so the digital signal can be generated by using a

Pc and recorded by using a multimeter or CRO at the output channel. The actual D/A conversion

is performed by weighted resistor or by using R-2R ladder

PROCEDURE:

1. Enable the software and select F2 for giving the input

2. Connect the CRO or multimeter at the DAC output in “AD/DA

converter” block.

3. Vary the TTL or CMOS inputs from PC to either high or low

4. View the output analog voltage an a CRO or multimeter

CONCLUSION: The digital data is converted into analog form and is observed on a

multimeter


1. Explain about Data Acquisition system?

2. Which type of ADC is used,explain it „s conversion process &mention it „s

analog input range?

3. Explain about DAC?

4. Give the details about interfacing?

5. What is the need of DAS?

INTERFACING OF DIGITAL SIGNAL FROM

MICRO COMPUTER THROUGH DAC

Experiment no:

Date:


PIN DIAGRAM OF ADC0800:

AIM: To study the digital input panel and analog input panel by giving inputs to the data

acquisition system

APPRATUS:

1. Trainer Kit

2. Software And Pc

3. Pates Cards

4. DMM

THEORY:

Data Acquisition system is used to collect the data from its input terminals and

display it in user defined from user friendly form. DAS is used to collect the information

a data from various terminals and do the necessary manipulation before the data is final

recorded.DAS consist of several circuits such as A/D,D/A, clippers, clampers , rectifier,

filters and display drivers circuit etc….to convert the data into required form.

PROCEDURE:

1. Switch ON DAS trainer and open the software

2. Close the switches D1 and D2

3. Patch 24v input to D3 and D4

4. Invoke the software and give the supply to the Vref.

5. Now select F3 for viewing status of switches

6. Select F4 for viewing status of 24 v supply

7. Now select F5 for viewing status of D15 and D16

CONCLUSION: The data acquisition system was studied and status of various inputs

was observed


1. What is DAS?

2. What are the types of displays used in DAS?

3. Why should use 4-20mA signal in channel 1?

4. What are the types of transducer used in DAS?

DATA ACQUISTION SYSTEM

Experiment no:

Date:

liquid chromatography experiment no: date

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