OIL BATH

PRECAUTION:

1. Know the bath material you are using. FP (Flash Point) of silicone oil is 150°C. For mineral oil, FP is
113°C. Do not set the oil-bath temperature above 130°C.

2. Set enough space for the operation. Keep all the flammable solvent or easily burned stuff far away
from the oil bath area.

3. Always wear protective eye-wear and gloves. Lab coats are mandatory when using oil baths.

4. Do not use oily hand to touch/adjust anything.

5. If you have more oil than needed, remove the excess oil from the bath. Liquids expand when
heated. Avoid overfilling the baths.

6. If your reaction mixture gets into the oil, immediately replace the oil. Notify safety officer of the
incident.

7. The oil will get dirty with normal use over the period. If you notice this, replace the oil.

8. If you spill any oil outside the bath, immediately wipe it up (preferably with some alcohol).

OPERATION:

1. Check the oil level in the oil bath. Switch on the instrument.

2. Make certain that the temperature probe is in the bath before turning on heat.

3. Make sure the glassware you are going to use in the bath is in good condition, no cracking or chips.

4. Do not put anything at the bottom of your oil bath container; it is much hotter than the
temperature you set. Use clips to stable your reactors.

5. Switch on the instrument and set the temperature knob to the desired temperature.

6. Double-check your oil bath’s performance within 10 minutes of setting it up to ensure it’s stable.

7. Turn stirring and heat off when not in use. If you see any oil bath is turned on without any label,
turn it off.

8. Switch off the instrument after the reaction is over. Keep the oil bath work area clean and safe.

DIGITAL PHOTOFLUORIMETER

OPERATION

Switch on the instrument 30 minutes prior to use.

Set the sensitivity control in LOW position, STANDARD and BLANK (coarse and fine) control to
minimum, i.e., counter clockwise.
Insert appropriate primary and secondary filters in their respective slots.

Switch on the instrument. Check the running of cooling fan. This can be noticed by slight noise from
the fan and the flow rate of air from the back side.

Set SENSITIVITY switch control in high position.

Do not press the SHUTTER, adjust display to zero by BLANK CONTROLS (coarse and fine).

Return SENSITIVITY switch control in low position. Readout should remain zero within ± 1 digit.

Insert test tube of standard. Depress the SHUTTER and adjust STANDARD controls (in conjunction
with SENSITIVITY control) till display reads standard reading or 100 counts for full scale. Always adjust
100 full scale at the lowest possible sensitivity. In case 100 full scale is not possible at low sensitivity,
try at medium and if still not possible try at high. Call this reading “S”.

Do not disturb the blank controls.

Replace the standard solution with blank solution. Depress the SHUTTER and note the display
reading “B”.

Replace the standard solution with the unknown solution. Depress the SHUTTER and note the display
reading “U”.

Calculate the concentration of unknown solution using the formula given below:

Unknown concentration = (U-B/S-B) x standard concentration

After completion of the work, clean the test tubes and place properly.

Switch off the equipment.

CALIBRATION

Operate the equipment.

Dissolve 100 mg Quinine sulphate in 0.1N sulphuric acid and dilute to 1000 ml with same solvent
(stock solution).

Further dilute to make the dilution 1, 2, 3, 4, & 5 ppm in 0.1N Sulphuric acid and measure the
intensity using primary wavelength 366 nm.

Plot a graph by taking the concentration on Y axis and intensity on X axis.

The correlation coefficient should be not less than 0.99.

SPECTROFLUORIMETER

FLUOROMAX plus - HORIBA

Instrument Startup:

1. Turn on power switch of FluoroMax-plus, from 0 to I (off to on).

2. Ensure that the software key is inserted into a USB port on the front of the computer.

3. Log in to open FluorEssence V3.8 software.

4. Click “Yes” to proceed.

5. Press Experiment Menu icon at the top left corner of window to initialize the instrument and bring

up the Main Experiment Menu.

Collection of Emission and Excitation Spectra and/or Determination of Optimal Emission and

Excitation Wavelength:

1. Choose “Spectra” from Main Experiment Menu.

2. Choose “Emission” from the Experiment Type menu.Click on the “Units” icon in the “Experiment”

menu on the left and select units for Time, Wavelength, and Slit Width.

3. Click on the “Detectors” icon in the “Experiment” menu on the left and enable the appropriate

detector(s) for your measurement

4. Click on “Monos” icon on the “Experiment” menu. Type an estimated excitation wavelength for
the

test substance under the excitation monochromator control, called “Excitation 1”.

5. Choose the range of wavelengths under the “Emission 1” monochromator section.

6. Insert sample to scan into the instrument sample compartment.

7. Click “Run”. The Intermediate Display will appear and provide a real-time output of the spectral

data.

8. From the resulting data, identify the wavelength of maximum emission.

9. Similar process is used to determine the optimal excitation wavelength.

10. Running a series of “Samples” (standards, blanks, unknowns) using calibration routines built in to
the

software. Click “Add Multiples” , and add as many samples as necessary for the experiment .

11. Return to “Monos” menu and click “Run”. After removing the previous sample and inserting the

next sample, click “OK” and repeat until experiment has finished all measurements.

12. Creating a Calibration Curve from data for the x and y axis in the Plot Setup window (x is

concentration and y is signal) and click OK. In the main menu, click the “Analysis” tab. Under

“fitting” choose the type of curve-fit you desire --- linear or polynomial. After choosing, click OK.

The chart displayed on the screen will have appropriate curve fit.
13. When finished, save files and experiments.

Turnoff:

14. Remove cuvettes and clean with distilled water and/or suitable solvents.

15. Close FluorEssence Program, place hardware key in safe place.

16. Turn off FluoroMax-plus, from I to 0 (on to off).

Digital Potentiometer

Specifications
Range: 0 to ±199.9 mV

Resolution: 0.1 mV

Repeatability: ± 1 mV

Accuracy: ± 1 mV ± digit

Input impedance: > 1010 ohms

Operating Temperature: 10 to 50 °C

Display: LED display with auto polarity indication

Selector Switch mv/STANDBY

This switch is at the extreme left of the instrument front panel at mV position. It reads millivolts on
the display. At this position, the instrument is in STANDBY mode and the electrode is disconnected
from the input. The display will read 000±1.

Range selector switch

200 mV: At this position, the sensitivity of the instrument will be 0.1 mV and the instrument can read
up to 199.9 mV in this range.

2000 mV: At this, the sensitivity of the instrument will be 1 mV and the instrument can read upto
1999 mV.

Back panel controls

Input: The input banana sockets accept the electrodes. The black socket is for the reference
electrode and the red socket for the glass or the platinum or silver electrode.

CAL: This control is used to calibrate the instrument reading to 000 mV when reference and glass
electrodes are connected and dipped in 7 pH buffer.

OPERATION

1. Fit the glass and reference electrodes in the electrode holder. Attach the electrode leads to the red
and the black socket of the instrument on the back panel.

2. Insert the main lead to 230V AC socket and switch On the instrument.

3. Put the selector switch to Standby position. Display shows 000±1.

4. Carefully dip both the electrodes into the solution under test.

5. Put the left selector switch to mV position.

6. Select the appropriate range, i.e., 200 mV or 2000 mV with selector switch.

7. The display shows the reading directly in mV’s.

8. Similarly, mV readings can be taken with other indicator and reference electrodes and other
electrode.

Digital Conductivity meter (SPECTRONICS INDIA SI-193)

Specifications
Range: 200 µS/cm to 1000 mS/cm in 5 ranges ( 1µS/cm = 1 µMho/cm)

Accuracy: ± 1% F.S. ± 1 digit

Resolution: 1.0 µS/cm

Measuring Frequency: 1000 Hz

Temperature Compensation: 0 to 50°C

Cell constant: 0.4 to 1.5 adjustable

Display: LED display

Standard conductivity reagents

1. Dissolve 0.7456 gm KCl (dried at 180°C for 1 hour) in distilled water and dilute to 1000 ml. The
distilled water used for preparing the standard solutions should have a very low conductivity.

2. Switch on the instrument and warm up for few minutes.

3. Put the function switch to CHECK position.

4. See that the display reads 1.000. If not, then adjust it to 1.000 with the help of CAL control
provided at the back panel.

5. Put the function switch to CELL CONST. position.

6. See that the display reads 1.000. If not, adjust it to 1.000 with the help of Cell Const. control
provided at the front panel.

7. The instrument is now ready for use.

Connecting the conductivity cell

1. Wash the conductivity cell thoroughly with distilled water (before use, the cell should be kept in
distilled water for at least 24 hours).

2. Fit the electrode leads to the input sockets provided at the rear of the instrument.

Precautions

1. Conductivity cell may be cleaned by using warm 50% detergent solution.

2. Platinum plates of the conductivity cell must be completely dipped in supernatant solution while
taking readings.

3. Check the cell constant as frequently as possible because deposition of film on the plates affects
the cell constant.

4. Rinse the cell in demineralized water.

5. Do not finger the cell electrodes.

6. The conductivity of most electrolyte solutions increases with rise in temperature.

HOT PLATE

1. Plug in the instrument.

2. Place the beaker on the plate of the stove.

2. The regulator knob can be used to increase the temperature of heating.

3. After use, switch off and unplug from the electric outlet.

4. Any glass apparatus with convex, concave, or uneven bottoms should not be used.

5. Avoid direct contact with hot surface of the plate.

DIGITAL FLAMEPHOTOMETER (SYSTONIC S-931)

Sensitivity: 0-100% for full scale (Na- 5mg/L; K- 2 mg/L; Ca- 50 mg/L; Li- 15 mg/L)
Accuracy: 5% of the reading

Display: LED

Detector: Photocell/Photodiode

Filters: Narrow band optical interference Glass filters direct mounting on rotating disc

Reproducibility: ±1 digit

Nebulizer: Black Bakelite, axial flow type

Flame system: LPG and dry oil free air

Combustion gas: LPG controlled by precision needle type regulator

Warm up time: 15 minutes

Pre-operating instructions

1. Prepare and keep ready the standard solution of respective elements.

2. Air out of the compressor unit and AIR IN of the main unit are connected properly with connecting
tube.

3. The LPG gas output from the gas cylinder is connected to the GAS in nozzle provided at the rear of
the main unit.

4. Make sure that all the connections are proper and there is not leakage of either air or gas.

5. Switch on the compressor.

6. Turn the Air control counter clockwise and adjust the air pressure to read 0.3 to 0.6 Kg/cm2 on the
air pressure indicator.

7. Keep igniter tip into flame chamber through view window.

8. Turn the gas control anti-clockwise slowly.

9. Press igniter to light the burner. Adjust Gas control to get silent flame close to the burner with
sharp blue cone. If required, adjust the air pressure and gas control to get a stable flame with sharp
blue cones.

10. Be sure that air is flowing through the burner before LPG is allowed into the burner and lighting
it.

11. Never view the flame form top of the chimney.

12. Less or no air flow and more flow and more fuel from the burner could result in build of the fuel
gas. This will cause flame to appear above the chimney and burn the mixing chamber.

13. All the safety precautions necessary for meeting the appropriate specifications for use of LPG
burner should be strictly followed.

14. Allow flame to stabilize for about 10 minutes.

15. Prepare samples in dissolved form of required dilution for the measurement and keep it handy.

16. Double distilled water should be used for getting good results.
17. Sample should neither be non-homogeneous nor highly viscous. It should not contain sediments.
Filter if needed, otherwise capillary will be clogged.

Operation and Calibration

1. Switch on the flame photometer.

2. Allow it to stabilize for 2 minutes.

3. Select the appropriate element for the filter disc (Na, K etc.).

4. The sensitivity is to be selected depending upon the element under test. Initially, set the sensitivity
switch to position 1.

5. Clean the capillary by double distilled water (take about 5 ml double distilled water on mixing
chamber platform. Dip loose end of the capillary in the double distilled water. It will start getting
aspired into the nebulizer and thus clean it).

6. Set zero on the display with set Zero knob.

7. Replace distilled water beaker with standard solution beaker (value of the standard solution
should be approximately near to the expected value of the sample to be tested).

8. Set the ppm value of standard solution on the display of the flame photometer by rotating the Cal
knob. If the display does not reach the value of the standard solution, increase the sensitivity to the
next position.

9. Replace the standard with blank (may be double distilled water to clean the capillary).

10. Now the instrument is ready for taking the reading of any unknown sample solution.

Sample measurement

1. After calibration of the instrument, clean the capillary with double distilled water as described in
the calibration procedure.

2. Take sample solution in the sample holder.

3. Keep it on the mixing chamber platform.

4. Dip the capillary tube in the sample.

5. Sample will be aspirated and color of the flame will be changed depending upon the sample.

6. Display will read the exact value of the sample in ppm units.

7. Before taking the readings for next sample, clean the capillary with blank solution for that
element. Only then the reading of the sample should be taken.

8. To measure the reading for samples of any other elements, the instrument will have to be
calibrated with standard solution to that element. Only then, the reading of the sample should be
taken.

Precautions:

1. After every 20-30 minutes of operation, the instrument should be recalibrated.

2. Clean the nebulizer with the cleaning wires.

3. For accurate results, the value of the sample and the standards used should be less than 40 ppm. If
it is more than that dilute appropriately.

Sodium standard solution

Weigh accurately 635 mg of Anal R grade of NaCl (dried at 180°C for 1 hour) and dissolve in exactly
250 ml of double distilled water. The solution so obtained will have 1000 ppm of Na. Dilute this
solution to 1:9 with double distilled water to make standard of 100 ppm.

Potassium standard solution

Weigh accurately 477 mg of Anal R grade of KCl (dried at 180°C for 1 hour) and dissolve in exactly 250
ml of double distilled water. The solution so obtained will have 1000 ppm of K. Dilute this solution to
1:9 with double distilled water to make standard of 100 ppm.

Calcium standard solution

Weigh accurately 624 mg of Anal R grade of CaCO3 and dissolved in minimum quantity of 1:1 HCl and
make up the volume to exactly 250 ml with double distilled water. The solution so obtained will have
1000 ppm of Ca. Dilute this solution to 1:9 with double distilled water to make standard of 100 ppm.

Lithium standard solution

Weigh accurately 635 mg of Anal R grade of Li2CO3 and dissolved in minimum quantity of 1:1 HCl
and make up the volume to exactly 250 ml with double distilled water. The solution so obtained will
have 1000 ppm of Li. Dilute this solution to 1:9 with double distilled water to make standard of 100
ppm.

DIGITAL pH METER
Connecting the electrode

Set up the electrode stand and fit the pH electrode into it.

Carefully remove the protective rubber cap from the filling hole of electrode. The level of KCl solution
should be a few mm below the hole. Top up, if necessary, with saturated KCl solution. Now put the
rubber cap back.

Preparation of buffer solution

Dissolve one buffer tablet or powder pack of 7 pH in 100 ml distilled water. The pH of this solution is
7. Place the solution in a bottle and store in a cool place.

Calibration of electrode

This electrode should be calibrated before beginning measurements or when pH readings are
doubtful.

Connect the combination pH electrode to the input socket, wash it with distilled water and switch on
the instrument.

Dip the electrode in 7 pH buffer solution.

Set the TEMPERATURE controls to the buffer solution temperature.

Set the Function Selector switch to pH position and adjust with CALIBRATE control till the digital
display shows the precise pH value of the buffer solution.

Now move the Function Selector switch to Stand By.

Remove the electrode from the buffer solution and wash it with distilled water.

Dip the combination electrode into another buffer solution (say 4 pH buffer).

Set the Temperature control to the temperature of the selected buffer solution.

Set the Function Selector switch to pH position. Adjust the Slope correction control at the front panel
until the display shows the pH value of the selected buffer solution. Check that the correct readings
are obtained with both the buffer solutions without further adjustment if necessary.

mV Measurements

Connect the combination pH electrode to the input socket.

Set the Function Selector switch to mV position.

Dip the combined electrode in solution under test.

The display will display mV value of the solution under test.

Brookfield Viscometer
Operation
Adjust the instrument level using the two leveling screws on the base and make sure that the bubble
on top of the viscometer is centered within the circle. Note: Check the level periodically during use.
Connect the RTD probe to the socket on the rear panel of the viscometer.
Connect the power cord to the socket on the back panel of the viscometer and make sure that the
AC power switch at the rear of the viscometer is in the OFF position.
Turn the power switch to the ON position and allow it to warm up for 10 minutes before performing
auto zero.
The screen will display the name of the instrument and its version of the operating firmware and a
two-digit alphanumeric code that indicates the model number.
The screen will then display “REMOVE SPINDLE, PRESS ANY KEY” after 10seconds.
Remove the spindle and press any key. The viscometer will flash “AUTOZEROING”.
After approximately 15 sec, the display will show “REPLACE SPINDLE, PRESS ANY KEY”.
Attach the required spindle for the specific test and dip the IRTD probe into the sample then press
any key.
The display will show the cP 0.0 (on the left corner) OFF RPM (below the CP), the temperature i.e.
20.1 °C (on the right corner), and the torques percentage % 0.0 (below the temperature).
Press the SELECT SPINDLE key and it will temporarily display the current selected spindle in place
temperature and cause the character S to blink.
Press the UP or DOWN ARROW Keys, While S is blinking, select the desired spindle code then press
the SELECT SPINDLE key again.
Press the SET SPEED Key, then press the UP or DOWN key arrows. Will cause the RPM letters to
blink.
Select the required speed by pressing the UP or DOWN arrows while the RPM is blinking. The
selected speed will blink for 3 seconds then it stops.
Dip the guard leg with the spindle into the sample slowly and make sure no air bubbles are trapped.
Press the MOTOR ON/OFF-ESCAPE Key to set the motor on or to stop the motor.
The display will show the viscosity on cP, the speed on RPM, the temperature, and the torque
percentage %.
To get the maximum calculated viscosity (full-scale reading) possible with the current spindle/speed,
press the ENTER AUTO RANGE Key.
The display will show EEE on both the cP and torque % when the operation is out of range.
The display will indicate “__________ C” if the RTD temperature probe is not connected.
When the torque % is below 10 it will keep blinking. Nonetheless, record the readings on the display.
Press the MOTOR ON/OFF-ESCAPE to stop the motor.
Remove the spindle and guard leg from the sample and clean the RTD probe spindle and guard leg
with distilled water.
Calibration
The Brookfield DV – II + Pro is to be calibrated once every six months, after repairs, before use
without a guard leg, and/or before use with any other beaker but the 600ml low form griffin beaker.
Brookfield silicone fluid viscosity standards with values: 10, 500, 1000,12500 & 60000cp using
respective spindles and record the results.
Set up the viscometer as per the operating procedure mentioned above on a level firm bench.
When carrying out the calibration process ensure the following;
1. The calibration log book is available.
2. The viscometer is set according to operating instructions.
3. The water bath is stabilized at a test temperature of 25°C.
4. The guard leg is clean and attached.
5. Only LV 1, 2, and 3 spindles (61, 62, and 63 respectively) are to be used.
6. Only the low-form Griffin beaker is used.
7. Select one viscosity standard fluid and place it in the low-form griffin beaker.
8. Lower the DV-II + Pro into the measurement position.
9. Attach the spindle to the viscometer while avoiding trapping air bubbles beneath the spindle by
immersing it at an angle and then connecting it to the viscometer.
10. Measure the viscosity and record the results as per Attachment-1.
Note: The spindle must rotate at least five times before readings are taken and the value of torque
should be more than 10%. Repeat the procedure for the remaining silicone fluid viscosity standards.

DIGITAL ULTRASONIC CLEANER

PRELIMINARY CHECK
1. Fill the Water in water bath up to the level which shown on the tank. Whenever the Ultrasonic
Water Bath is required with specific temperature then heater to be kept “ON”.
2. Ensure that there is no leakage of water from water bath.
3. Do not put any heavy objects on the bottom of the tank as it can damage the transducers. Always
use tray supplied with ultrasonic bath.
4. Ensure that liquid does not splash on the controls and switches.
Basic Operation
1. Connect the Ultrasonic Water Bath to the main power supply with the connecting plug the cleaner
into grounded outlet.
2. Press the “TIME +” key for increasing the time setting within 1 - 99 min working time. Press “TIME
-” for reducing the time. During working, you will hear the “sizzling” voice, that means the cleaner
running properly.
3. Set temperature: Press “Heating +” key to increase temperate within 0°C - 80°C. Press the
“TEMPERTURE –” key for reducing temperature.
4. Then press the “Heating” button “ON” begin to heat.
5. Press “Ultrasonic” button “OFF”, the cleaner will stop working, indicator light turns off. And then
disconnect the power supply.
6. Press “Heating” button “OFF”, the heating function will stop.
MAINTENANCE
1. Ensure system is off and disconnect the power cable from the main socket before cleaning.
2. Clean the water bath and replace the water on daily basis or as and when the water gets turbid.