ST.
PAUL’S COLLEGE,
KALAMASSERY
CHEMISTRY
LABORATORY
MANUAL
LABORATORY MANUAL
LABORATORY MANUAL
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LABORATORY MANUAL
CONTENTS
Page
Sl. No. Title
No:
1 UG/PG Chemistry lab 3
2 Guidelines for carrying out experiments 4
3 Lab rules 4
4 Lab safety 5
5 First aid & emergency measures 7
6 Laboratory notebooks 9
7 Recording significant figures in your notebook 10
8 Effectively communicating through a laboratory report 10
9 Experimental instructions 11
10 Volumetric analysis 12
11 Centrifugation 16
12 Filtering a precipitate 17
13 Qualitative inorganic analysis 18
14 Qualitative organic analysis 19
15 Physical analysis - conductometry 24
16 Instrumentations 26
17 Sonicator 27
18 Muffle furnace 28
19 Hot air oven 29
20 Microwave oven 30
21 Mechanical stirrer 31
22 Magnetic stirrer 32
23 UV spectrophotometer 33
24 Colorimeter 34
25 Deep freezer 36
26 Four digit balance 37
27 Homogenizer 37
28 Conductivity meter 38
29 PH Meter 39
30 Laboratory glasswares 40
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LABORATORY MANUAL
UG/PG CHEMISTRY LAB
The Department of Chemistry offers courses in M. Sc. and B. Sc. Chemistry
along with Chemistry as a subsidiary programme for the students who
have taken Physics as their main subject. The College has two labs for
Chemistry practical. Each lab has sufficient number of equipment and
facilities. The chemical stockroom, instrumentation room and a balance
room are situated within the UG chemistry lab. The PG lab consists of
physical, organic, inorganic labs and a computer lab. Both the labs are
equipped with fume hoods, working benches and specialized equipment.
Each student is assigned to his/her own locker which contains laboratory
glassware to perform experiments.
Our laboratories with advanced equipment and facilities aid and
stimulate our students for them to learn best with practical knowledge.
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LABORATORY MANUAL
GUIDELINES FOR CARRYING OUT EXPERIMENTS
LAB RULES
Bring the laboratory manual and a laboratory notebook (not loose leaf or spiral) to
every scheduled laboratory session.
Careful notes should be taken during each laboratory lecture. The instructor will
generally provide information on the chemistry underlying the project, as well as
advice on the techniques that you will use. Some of this information should be
included in your laboratory report.
You may work in the Chemistry PG and U G laboratories only during your
regularly scheduled laboratory period and only when class is in session.
If you miss a laboratory for a legitimate reason, you must obtain permission
from your regular laboratory instructor to make‐up the lab at another time. Make-
up labs are only allowed when space allows and with the approval of the host
professor. During the make-up laboratory, you must move your equipment to an
unoccupied lab bench.
During the first scheduled laboratory period, you will be assigned a laboratory
locker to which you alone will have the combination. The locker equipment is
your responsibility while you are in the course and you should be diligent to keep
the equipment clean.
Test tube brushes and soap solutions are available at each sink.
The Chemistry Department maintains a stockroom to store the chemical and
apparatus. This stockroom is open during all scheduled laboratory periods for the
acquisition of equipment necessary to replace broken items.
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LABORATORY MANUAL
LAB SAFETY
TRAINING AND SAFETY RULES
Attendance is required at a presentation on laboratory safety that will be
shown during your first scheduled laboratory. Each student must give the
instructor a signed form indicating that the presentation was attended and that
any associated training materials were examined.
The laboratory is equipped with fire blanket, showers, eye wash, and first aid
supplies.
Learn the locations and proper use of these items.
At all times when you are working in the chemistry laboratory you should use
prudent practices. Recognize that safety is, ultimately, everyone's individual
responsibility. Never work alone in any laboratory.
Avoid the most common causes of accidents
o Exercise care when picking up potentially hot objects.
o Insert glass objects into rubber stoppers and corks with extreme care.
Avoid contact with laboratory chemicals
o Wear clothing that protects as much of your body as possible. Closed-toe shoes
are required. All skin below the waist must be covered.
o Use department-approved eye-protection at all times.
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LABORATORY MANUAL
o Keep the laboratory bench and work area orderly, clean, and free of items not
related to the experiment at all times. Specifically, electronic devices are not
allowed on the bench.
o Never sit on or lean against the laboratory bench.
o Use a fume hood when directed to do so.
o Food or drink should only be consumed in the lecture area of the room. Do not
chew gum during laboratory sessions.
o Dispose of waste materials and excess chemicals in the appropriate containers
as indicated by your instructor.
When emergencies do occur
o Always keep in mind that the first response to the exposure of the eyes or skin
to a chemical is immediate, thorough irrigation with water.
o Report all accidents, however minor, to the laboratory instructor immediately.
o Know the exact location of all safety equipment and how to use it.
Preparation is important
o Perform only assigned experiments. Do not attempt to modify the written
procedures unless instructed to do so.
o When conducting experiments ask yourself, "What are the worst possible things
that could go wrong?" and "How will I deal with them?" Don't do the experiment
until you are certain of your answers.
o Read the label on the container to be certain it contains the required chemical.
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LABORATORY MANUAL
FIRST AID & EMERGENCY MEASURES
[1] Acid on clothing: Neutralize with dilute ammonium hydroxide. Then wash
thoroughly with water
[2] Alkali on clothing: Neutralize with dilute acetic acid. Then wash thoroughly with
water.
[3] Acid in eye: Wash thoroughly and profusely with running water. Bathe the eye
with a 2 % sodium bicarbonate solution, using an eye cup. Dry with sterile gauze
and put several drops of olive oil into the eye.
[4] Alkali in eye: Wash thoroughly and profusely with running water and the eyelids
should be held widely open especially when caustic alkalies have entered the eye.
Bathe with boric acid solution. Dry and add a drop of olive oil into the eye.
[5] Ordinary heat burns: Don’t use water. Apply sodium bicarbonate, Vaseline paste or
burnol and consult a doctor
[6] Acid burns: Wash first with running water and then with sodium bicarbonate
solution. Cover with solid sodium bicarbonate for 10 minutes. Wash off and apply
carron oil (a mixture of equal parts of lime water and linseed oil).
[7] Alkali burns: Wash first with running water and then with boric acid solution.
Cover with powdered boric acid for 10 minutes. Wash off and apply sodium
bicarbonate Vaseline paste.
[8] Cuts: Remove particles of glass, if any are present. Wash the wound with water.
Then apply tincture of iodine and cover with a sterile bandage
[9] Poisoning by strong acid: Give plenty of water or milk. Then give two table spoons
of lime water
[10] Poisoning by caustic alkalies: Give plenty of water or milk. Then give orange or
lemon juice
[11] Fire: Extinguish gas burners in the vicinity. Use buckets of dry sand/fire-
extinguishers to cease the fire.
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LABORATORY MANUAL
LAB SAFETY RULES
Avoid skin and eye contact with all chemicals
Minimize all chemical exposures
Do not engage in practical jokes or boisterous conduct in the laboratory
Never run in the laboratory. No horseplay will be tolerated
The use of personal audio or video equipment is prohibited in the laboratory
The performance of unauthorized experiments is strictly forbidden
Do not sit on laboratory benches
Always wear a lab coat
Laboratory safety glasses or goggles should be worn in any area where chemicals
are used or stored. They should also be worn any time there is a chance of splashes
or particulates to enter the eye
Avoid skin and eye contact with all chemicals
Do not taste or intentionally sniff chemicals
Never consume and/or store food or beverages or apply cosmetics in areas where
hazardous chemicals are used or stored
Long hair and loose clothing must be pulled back and secured from entanglement
or potential capture
Know emergency procedures
Never work in the laboratory without the supervision of an instructor
Always perform the experiments or work precisely as directed by your instructor
Never leave experiments while in progress
Never attempt to catch a falling object
Never point the open end of a test tube containing a substance at yourself or others
Do not leave the Bunsen burners unattended. Make sure no flammable solvents are
in the surrounding area when lighting a flame
Turn off all heating apparatus, gas valves, and water faucets when not in use
Keep the floor clear of all objects (eg. Ice, small objects and spilled liquids)
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LABORATORY MANUAL
LABORATORY NOTEBOOKS
One of your goals in this laboratory course should be to learn to keep proper
records of your work. Your laboratory reports will be based on the data in your
notebook, and the more complete the data are the more likely it is that you will be
able to prepare a good report. Furthermore, discrepancies and unexpected results can
be accounted for only by referring to complete records of your work. In a broader
sense, a notebook is essential in any research laboratory where it may be necessary to
review data months or years after they were taken; hence full details are necessary.
You will be required to keep your laboratory records in a hard-cover, bound
notebook. The notebook should contain all experimental data and pertinent
observations recorded in ink at the time they are obtained. Data may not be recorded
elsewhere for later recopying in the notebook, and, in particular, loose scraps of
paper are not permissible for records. The following are the requirements for your
notebook:
o Each day's work should be dated. The project being performed should be
indicated clearly.
o No erasures should be made, and mistakes should be crossed out with a
single line but remain legible.
o Pages must not be removed from the notebook.
o The notes must be neat and orderly enough for someone else to follow them.
o Use tables to organize data whenever possible.
o The following should be included in the laboratory notebook:
o All experimental data, such as masses, buret readings, temperature, etc.
o Notable occurrences (especially phase or color changes).
o Full details of a procedure need not be recorded, but each step should be noted
as it is performed.
o All mathematical computations during and after the laboratory session.
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LABORATORY MANUAL
RECORDING SIGNIFICANT FIGURES IN YOUR NOTEBOOK
When recording a numeric measurement, the number of significant figures
conveys how accurate the measurement is.
o When massing, record all digits on the balance. The last place has uncertainty in
it (you may even see the digit change).
o When measuring volumes using graduated glassware, estimate and record one
digit beyond the markings, as shown below in the figure.
EFFECTIVELY COMMUNICATING THROUGH A LABORATORY REPORT
Writing is ubiquitous in the sciences, and students primarily develop their
writing skills through writing laboratory reports. As a scientist‐in‐training, you
ultimately need to learn how to make a reasoned and articulate argument that is
persuasive and based on scientific evidence; the foundation of that argument needs to
be grounded in data that are presented in an organized and thorough manner. The
laboratory report communicates to others the results and conclusions you obtained in
performing an experiment. You should explain why the experiment was performed,
how the experiment was performed, what results were obtained, how the results were
analyzed, and what conclusions were reached.
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LABORATORY MANUAL
EXPERIMENTAL INSTRUCTIONS
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LABORATORY MANUAL
VOLUMETRIC ANALYSIS
Volumetric analysis is a widely used quantitative analytical method. As the
name implies, this method involves the measurement of volume.
VOLUMETRIC PROCEDURE
[1] A solution is prepared from an accurately weighed sample of the material to be
analyzed.
[2] A substance is chosen that will react rapidly and completely with the constituent
that is to be determined. A standard solution of this substance is prepared. A
standard solution is one of accurately known concentration, usually expressed as
molarity with a precision of ± 0.0001 M.
[3] Some of the standard solution is poured into a buret. The buret is graduated
(usually in tenths of a mL) so that the volume of solution that passes through the
stopcock may be accurately measured.
[4] Standard solution is added slowly from a buret to the "unknown" solution,
allowing the reaction to occur. This process is called titration, and the solution
in the buret is known as the titrant. Ideally, the titration is continued until the
reaction is complete; that is, until the amount of reactant added is exactly the
amount required to react with the entire constituent that is being determined.
This point is called the equivalence point. The equivalence point is detected
by adding an indicator to the "unknown" solution before the titration is begun.
An indicator is a substance that gives a color change at or near to the
equivalence point. The point at which this change occurs is called the
endpoint. The particular indicator that is used depends on the specific
reaction involved. The titration is stopped when the endpoint is reached.
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LABORATORY MANUAL
[5] The exact volume of standard solution required can be measured, from buret
readings before and after the titration. Since the molarity of the standard solution
is known, the number of moles of titrant can be calculated. Furthermore, from
knowledge of the equation for the reaction, the number of moles of constituent
present in the sample can also be calculated.
STANDARD SOLUTION
The most accurate and convenient way of preparing a standard solution is to
weigh the reagent accurately, dissolve it, and dilute the solution to a definite
volume in a volumetric flask. This method can be employed only if the reagent is a
primary standard. In order to qualify as a primary standard, a substance must meet
the following requirements: it must be obtainable in pure form; it must be stable both
in pure form and in solution; it must be easy to dry and keep dry; and it must be
soluble in a suitable solvent.
Unfortunately, many useful reagents do not meet these requirements. In such a
case, the reagent is dissolved and made up approximately to the concentration
desired. This solution is then standardized by titrating it against a primary standard.
A solution standardized in this fashion is a secondary standard.
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LABORATORY MANUAL
TITRATION PROCEDURE
[1] Carefully clean the buret with Alconox solution and a brush to remove all
dirt and grease. Rinse the buret with several portions of tap water by partially
filling it, draining a small portion through the tip, and pouring the bulk of the
rinse from the top of the buret while rotating it. If any drops of water collect
on the walls when the rinse is poured from the buret, the cleaning is
unsatisfactory and must be repeated. Finally, rinse the buret with two or three
portions of deionized water.
[2] Before filling the buret, rinse it with titrant solution 2-3 times, using about
10 mL portions.
[3] Place the buret in a buret clamp attached to a large ring stand. Using a funnel,
fill the buret with titrant to a level above the zero mark. Place a beaker under
the buret and open the stopcock for a few seconds to remove all air from the
tip. The top of the solution should now be below the zero mark.
[4] Read the buret to ± 0.01 mL. (Because the buret is graduated to 0.1 mL, the
second decimal place must be estimated.) To make this reading, it is necessary
to locate the meniscus (that is, the surface of the liquid) with respect to the
markings. The reading is considerably affected by the position of the eye and by
the color of objects behind the buret. The variation of the apparent position of
the meniscus is called parallax. To minimize errors due to parallax, the
meniscus should be level with the eye (see the Figure given below).
Avoid parallax error by using correct eye position.
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LABORATORY MANUAL
The variation of colors behind the buret can be eliminated by mounting a
piece of black tape on a white card and holding it behind the buret as shown in Figure
10. If a highly colored liquid is used, it is more convenient to read the position of the
top of the meniscus.
Reading card correctly held.
[5] Place the solution that is to be titrated in an Erlenmeyer flask and add the
appropriate indicator. Position the flask under the buret. Add the titrant
slowly from the buret while swirling the contents of the flask to assure
adequate mixing. As the endpoint is approached, the titrant must be added
very slowly-a drop at a time. Usually there is warning as the endpoint is
approached. If the endpoint is a color change, the change is produced
momentarily where the reagent drops into the solution, but fades with
stirring into the bulk of solution. This fading occurs more slowly as the
endpoint is approached.
[6] If the indicator change is a very sharp one, it may be desirable to add standard
solution only a half drop at a time near the endpoint. This may be done by
opening the stopcock slightly until a drop begins to form on the buret tip.
When the droplet has grown to a few hundredths of a mL (one drop is about
0.05 mL), it is touched to the side of the titration vessel and rinsed down with a
little deionized water from the wash bottle.
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LABORATORY MANUAL
[7] If an endpoint is not distinct, or if it is unfamiliar, it may be difficult to decide
when the endpoint has actually been reached. In this case, record the buret
reading, add another drop, and note the change produced. If the observer is still
uncertain, another reading should be recorded, and another drop added. When
a series of such readings have been recorded it is easier to select the
endpoint in retrospect than by direct approach.
[8] When the endpoint has been reached, subtract the initial buret reading (step 4
above) from the final reading to obtain the volume of titrant used.
CENTRIFUGATION
Precipitates are separated from their mother liquors by centrifugation. Keep
the centrifuge balanced by placing a counterbalancing test tube, filled with an equal
volume of water, directly opposite to the test solution. The solution should be
centrifuged for several minutes to pack the precipitate in the bottom of the tube. The
mother liquor can be withdrawn carefully with a capillary pipet.
Counterbalance the solution to be centrifuged.
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LABORATORY MANUAL
FILTERING A PRECIPITATE
The most convenient device for collection of the precipitate is a filter crucible,
which is a glass crucible with a porous disc in the bottom, or a Büchner funnel with
filter paper. The filter crucible, using a crucible holder or the Büchner funnel, is
mounted on a filtering flask and the filtration is accomplished by suction.
As much of the mother liquor as possible is decanted through the filter without
disturbing the precipitate in the beaker, so that the major portion of the liquid may
be filtered rapidly and before the precipitate begins to clog the filter. Figure 24
illustrates the pouring operation. It is good to keep the filter crucible always fairly full
of liquid. After the filter crucible is filled, it may be necessary to interrupt the pouring
and to set the beaker on the table while waiting for the crucible to empty. When
pouring is interrupted, the beaker is not turned upright immediately, because there is
a tendency for a drop to adhere to the outside of the spout and to run down and be
lost. Instead, the beaker is tipped back only slightly and the clinging drop is
transferred to the rod by touching the rod to the beaker spout. The drop adhering to
the end of the rod is removed by touching it to the side of the crucible. The rod is laid
across the top of the beaker with the wet end resting on the spout.
A filtering apparatus crucible
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LABORATORY MANUAL
Correct method of transferring a solution to a filter
QUALITATIVE INORGANIC ANALYSIS
Qualitative chemical analysis is a branch of chemistry that deals with the
identification of elements or grouping of elements present in a sample. The techniques
employed in qualitative analysis vary in complexity, depending on the nature of the
sample. In some cases it is necessary only to verify the presence of certain elements or
groups for which specific tests applicable directly to the sample (e.g., flame tests, spot
tests) may be available. More often the sample is a complex mixture, and a systematic
analysis must be made in order that all the constituents may be identified. It is
customary to classify the methods into two classes: qualitative inorganic analysis and
qualitative organic analysis.
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LABORATORY MANUAL
QUALITATIVE ORGANIC ANALYSIS
The analysis and identification of unknown organic compounds constitutes a
very important aspect of experimental organic chemistry. There is no definite set
procedure that can be generally applied to organic qualitative analysis. Various books
have different approaches, but a systematic approach based on the scheme given below
will give good results. Students should, however, consult the laboratory manual and
Textbook of Practical Organic Chemistry, A.I. Vogel (4th Edition).
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LABORATORY MANUAL
PHYSICAL ANALYSIS - CONDUCTOMETRY
Aim: To determine the strengths of strong (HCl) and weak acid (AcOH) in a given
mixture conductometrically.
Apparatus: Conductivity Bridge, Conductivity cell, beaker, Pipette, Micro burette, Glass
rod
Chemicals required: 0.1M HCl, 0.1M CH3COOH, 0.5M NaOH
Principle: Conductometric titration is a type of titration in which the electrolytic/ionic
conductivity of the solution continuously monitored as one reactant is added. The
principle of conductometric titration is based on the fact that during the titration, one of
the ions is replaced by the other and invariably these two ions differ in the ionic
conductivity with the result that conductivity of the solution varies during the course of
titration. The main advantages to the conductometric titration are its applicability to
very dilute, homogeneous suspension, coloured solutions and to system that involve
relative incomplete reactions, which cannot be used with normal indicators.
The conductivity of the solution is inversely proportional to the size of the ions .if
the size of the ions is increasing then the conductivity of the solution will decrease
because the mobility of the ions will decrease by increasing the size of the ions. By
increasing the temperature, the mobility of the ions in the solution will increase. So
temperature has a direct effect on conductance of solution.
Strong base (NaOH) neutralizes the strong acid (HCl) first rather than weak acid
(AcOH) indicated by decrease in conductance. This is due to comman ion effect. Due to
this, dissociation of weak electrolyte is suppressed. Hence, AcOH remains un-
neutralized till the complete neutralization of strong electrolyte (HCl). Then start the
neutralization of AcOH indicated by increase in conductance values. When the acid
mixture is completely neutralized, further addition of base will results the increase in
conductance.
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LABORATORY MANUAL
Procedure: Take 25 mL of 0.1M HCl and 25 mL 0.1M AcOH in a clean 100 mL beaker.
Connect the conductivity cell to the conductivity meter. Once the conductivity meter is
standardized, add 1mL of 0.5M NaOH from the burette to solution (acid mixture)
containing beaker. Stir the solution carefully and note down the corresponding
conductance value. Continue the addition of NaOH solution from the burette and
record the conductance after every addition and tabulate the data.
Tabular form:
Model graph:
Plot a graph between conductance values against the volume of the NaOH added.
Three straight lines are obtained. The intersection of the first two lines gives the end
point of strong acid and the intersection of the second and third lines gives the end
point of the weak acid.
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LABORATORY MANUAL
INSTRUMENTATIONS
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LABORATORY MANUAL
SONICATOR
Sonication is the process of using energy to move particles around in a solution
given. Typically, we do it for the purpose of cleaning or separating different substances.
In the science laboratory, sonication is used to disrupt cellular membranes and as a
result, release the contents of the cell. Sonication can also be used to fragment DNA,
and preventing it from interfering with further sample preparation. Moreover, its other
biological uses include the production of nanoparticles, liposomes, extraction of
anthocyanins and antioxidants.
A sonicator is a powerful piece of lab equipment with an ultrasonic electric
generator which creates a signal to power a transducer. This transducer converts the
electric signal using piezoelectric crystals i.e. crystals that respond directly to electricity
by creating a mechanical vibration. The sonicator preserves and also amplifies the
vibration until it passes to the probe. The sonicator operator can easily control
amplitude based on properties of solution. A small probe tip produces a much intense
reaction than a large probe tip. On the other hand, a large tip reaches more of the
solution.
This process uses ultrasonic sound waves. During the sonication process cycles
of pressure form, thousands of microscopic vacuum bubbles in the solution. These
bubbles collapse into the solution in the process of cavitation. This causes powerful
waves of vibration which release an enormous energy force in the cavitation field. This
disrupts molecular interactions such as interactions between molecules of water. Hence
it separates clumps of particles and facilitates the mixing. For example, in dissolved gas
vibrations, bubbles due to the gas come together and more easily leave the solution. The
energy from the sound waves creates friction in the solution, which as a result creates
heat. To stop a sample from heating up and degrading, keep it on the ice before, during
as well as after the sonication. If the cells and proteins are too fragile to withstand
sonication, a gentler alternative is enzyme digestion or grinding with sand.
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LABORATORY MANUAL
MUFFLE FURNACE
Muffle furnace refers to a type of jacketed enclosure that is used to heat a
material to significantly high temperatures while keeping it contained and fully isolated
from external contaminants, chemicals or substances. Muffle furnaces are usually lined
with stainless steel, making them largely corrosion resistant. Muffle Furnace is box type
heat treatment equipment used to change physical properties of samples at very high
temperature; for example 1100 °C, 1200 °C, 1300 °C, 1600 °C and 1700 °C. These
laboratory furnaces are widely used in scientific experiments in physics/chemistry
laboratories, steel and paint industries, biotech companies and small industrial
production etc. Their major applications include general laboratory testing, annealing,
ash determination, coal analysis, leaves carbonization and lime calcination etc.
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HOT AIR OVEN
Hot air ovens use extremely high temperatures over several hours to destroy
microorganisms and bacterial spores. The ovens use conduction to sterilize items by
heating the outside surfaces of the item, which then absorbs the heat and moves it
towards the center of the item. Hot air oven is widely used in the medical industry to
sterilize the equipment and other materials that are used in a laboratory. It is used for
delivering the heat treatment to the product. They do not require water and there is not
much pressure build up within the oven, unlike an autoclave, making them safer to
work with. This also makes them more suitable to be used in a laboratory environment.
They are much smaller than autoclaves but can still be as effective. Items that are
sterilized in a hot air oven include: Glassware (like petri dishes, flasks, pipettes, and test
tubes), powders (like starch, zinc oxide, and sulfadiazine), materials that contain oils
and metal equipment (like scalpels, scissors, and blades). Place the articles at sufficient
distances so as to allow free circulation of air in between them and to ensure
uninterrupted airflow. Shut the door and switch on the hot air oven.
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LABORATORY MANUAL
MICROWAVE OVEN
Microwave ovens can be used in laboratories for the rapid heating of material –
either to dry them completely or to subject a workpiece to sudden thermal stress or
electric field stress. Microwaves used for general processing may be used for heating
laboratory samples, preparing solutions, drying, and heating samples or products.
Determinations of the moisture content levels in soil or leaf tissue samples, for example,
can be made within tens of seconds rather than hours. It is often assumed that placing a
load within a microwave oven will result in it being heated evenly as well as quickly,
but this is not always the case. The size and shape of a sample as well as its physical
properties determine the power absorption. The range the microwave can be used for
industrial, research, quality control processing is almost unlimited. The discussion on
the use of microwave units specially designed for synthesis use, which are often quite
expensive, becomes rather heated at times.
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The water molecule is the target for microwave ovens; like any other molecule with a
dipole, it absorbs microwave radiation. Microwave radiation is converted into heat with
high efficiency, so that "superheating" becomes possible at ambient pressure. Enormous
accelerations in reaction time can be achieved, if superheating is performed in closed
vessels under high pressure; a reaction that takes several hours under conventional
conditions can be completed over the course of minutes.
MECHANICAL STIRRER
Mechanical stirrer it's laboratory equipment consisting of an electric motor that
drives the blades ended metal rod immersed in the mixed liquor. Laboratory
mechanical stirrers are commonly used in industrial laboratories, research, cosmetic
mixing and dispersing solid and liquid material, mixing at liquid-liquid system with
different viscosities - from low to high. Mixers are available with different speed and
advancement, equipped with a digital display or without display- depending on the
requirements and needs of the client.
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LABORATORY MANUAL
MAGNETIC STIRRER
A magnetic stirrer is a device widely used in laboratories and consists of a
rotating magnet or a stationary electromagnet that creates a rotating magnetic field.
This device is used to make a stir bar, immerse in a liquid, quickly spin, or stirring or
mixing a solution. Most laboratory stirrers provide a speed range, such as 12-1800 rpm
or 40-6000 rpm, but there are some single speed options. Place metal objects of any kind
in a microwave oven. This includes aluminium foil and plastic coated magnetic stirrer
bars. A magnetic stirrer or magnetic mixer is a laboratory device that employs a rotating
magnetic field to cause a stir bar immersed in a
liquid to spin very quickly and thus stirring the
liquid. The rotating field created by a rotating
magnet placed beneath the vessel with the
liquid.
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LABORATORY MANUAL
UV SPECTROPHOTOMETER
Ultraviolet-visible (UV-Vis) spectrophotometry is a technique used to measure
light absorbance across the ultraviolet and visible ranges of the electromagnetic
spectrum. When incident light strikes matter it can either be absorbed, reflected, or
transmitted. The absorbance of radiation in the UV-Vis range causes atomic excitation,
which refers to the transition of molecules from a low-energy ground state to an excited
state.
Before an atom can change excitation states, it must absorb sufficient levels of
radiation for electrons to move into higher molecular orbits. Shorter band gaps typically
correlate to absorption of shorter wavelengths of light. The energy required for
molecules to undergo these transitions, therefore, are electrochemically-specific. A UV-
Vis spectrophotometer can use this principle to quantify the analytes in a sample based
on their absorption characteristics.
The instrument used in ultraviolet–visible spectroscopy is called a UV/Vis
spectrophotometer. It measures the intensity of light after passing through a sample (I),
and compares it to the intensity of light before it passes through the sample (I o). The
ratio I/Io is called the transmittance, and is usually expressed as a percentage (% T). The
absorbance, A, is based on the transmittance. The UV–visible spectrophotometer can
also be configured to measure reflectance.
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The basic parts of a spectrophotometer are a light source, a holder for the sample,
a diffraction grating in a monochromator or a prism to separate the different
wavelengths of light, and a detector. The radiation source is often a Tungsten filament
(300–2500 nm), a deuterium arc lamp, which is continuous over the ultraviolet region
(190–400 nm), Xenon arc lamp, which is continuous from 160 to 2,000 nm; or more
recently, light emitting diodes (LED) for the visible wavelengths. The detector is
typically a photomultiplier tube, a photodiode, a photodiode array or a charge-coupled
device (CCD). Single photodiode detectors and photomultiplier tubes are used with
scanning monochromators, which filter the light so that only light of a single
wavelength reaches the detector at one time. The scanning monochromator moves the
diffraction grating to "step-through" each wavelength so that its intensity may be
measured as a function of wavelength. Fixed monochromators are used with CCDs and
photodiode arrays. As both of these devices consist of many detectors grouped into one
or two dimensional arrays, they are able to collect light of different wavelengths on
different pixels or groups of pixels simultaneously. Samples for UV/Vis
spectrophotometry are most often liquids, although the absorbance of gases and even of
solids can also be measured. Samples are typically placed in a transparent cell, known
as a cuvette. Cuvettes are typically rectangular in shape, commonly with an internal
width of 1 cm.
COLORIMETER
A colorimeter is a device used in colorimetry that measures the absorbance of
particular wavelengths of light by a specific solution. It is commonly used to determine
the concentration of a known solute in a given solution by the application of the Beer–
Lambert law, which states that the concentration of a solute is proportional to the
absorbance.
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LABORATORY MANUAL
The essential parts of a colorimeter are: a light source (often an ordinary low-
voltage filament lamp); an adjustable aperture; a set of colored filters; a cuvette to hold
the working solution; a detector (usually a photoresistor) to measure the transmitted
light; a meter to display the output from the detector. In addition, there may be: a
voltage regulator, to protect the instrument from fluctuations in mains voltage; a second
light path, cuvette and detector. This enables comparison between the working solution
and a "blank", consisting of pure solvent, to improve accuracy. There are many
commercialized colorimeters as well as open source versions with construction
documentation for education and for research. Changeable optics filters are used in the
colorimeter to select the wavelength which the solute absorbs the most, in order to
maximize accuracy. The usual wavelength range is from 400 to 700 nm. If it is necessary
to operate in the ultraviolet range then some modifications to the colorimeter are
needed. In modern colorimeters the filament lamp and filters may be replaced by
several (light-emitting diode) of different colors. In a manual colorimeter the cuvettes
are inserted and removed by hand. An automated colorimeter (as used in an Auto
Analyzer) is fitted with a flow cell through which solution flows continuously. The
output from a colorimeter may be displayed by an analogue or digital meter and may
be shown as transmittance (a linear scale from 0-100 %) or as absorbance (a logarithmic
scale from zero to infinity). The useful range of the absorbance scale is from 0-2 but it is
desirable to keep within the range 0-1
because, above 1, the results become
unreliable due to scattering of light. In
addition, the output may be sent to a chart
recorder, data logger, or computer.
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LABORATORY MANUAL
DEEP FREEZER
Deep freezers are the testing equipment that are used to preserve and store food
products, chemicals, etc. for a long period of time. Deep Freezers are used for industrial
purposes as well as for household purposes. These devices are available in different
sizes and shapes sometimes it is designed with compact designs and sometimes with
regular designs. The specifications and functions of the instruments vary as per the
requirements of the test application.
Deep freezer is highly sophisticated testing machine which designed and fitted
with a cooling compressors and CFC free refrigerants. These freezers are installed to
create highly effective cooling consistently inside the cabinet. The air cooling
compressors of the freezer are designed with aerodynamic fans and washable condense
filters which keep the internal environment free from dirt and dust. The instrument
helps to look into the mechanical behavior and characteristics of the rubber and
polymer and other medical or industrial products at low temperatures. A deep freezer
focuses on maintaining low temperatures that help keep the products at extremely low
temperatures to not only extent shelf life, but to also make sure the product does not
loss quality. In contrast to a regular freezer, a deep freezer can reach temperatures of –
50C to -60 Degrees Celsius within an hour to a few minutes. This helps to prepare ice to
carry out various organic syntheses in lab.
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LABORATORY MANUAL
FOUR DIGIT BALANCE
The 4 decimal weighing scale, normally known as Analytical Scale, or Analytical
balance. The balance indicates the measured result to 4 decimal places. All our 4
decimal weighing scale has functions of units conversation, percent and counting parts.
This balance used to take accurate weighing of compounds for various analyses, such as
titrimetric, gravimetric analysis etc.
HOMOGENIZER
Homogenization or homogenisation is any of several processes used to make a
mixture of two mutually non-soluble liquids the same throughout. This is achieved by
turning one of the liquids into a state consisting of extremely small particles distributed
uniformly throughout the other liquid. A homogenizer is a piece of laboratory or
industrial equipment used for the homogenization of various types of material, such as
tissue, plant, food, soil, and many others. Many different models have been developed
using various physical technologies for disruption. The mortar and pestle, already used
for thousands of years, is a standard tool even in modern laboratories.
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LABORATORY MANUAL
CONDUCTIVITY METER
An electrical conductivity meter (EC meter) measures the electrical conductivity
in a solution. A conductance of a solution can be measured by applying an alternating
electrical current to the two electrodes present in the probe. While this electrical current
is applied to the solution, the cations (+ charge) move to the negative electrode and the
anions (- charge) move to the positive electrode. This movement of the ions leads to the
solution to be conductive. Conductivity meter allows us to measure the level of
conductivity in solutions. Conductivity is an ability of materials (solutions, metals or
gases) to pass an electric current. While all materials possess the ability to pass electric
currents, the degree of such ability can vary. Substances with conductive aqueous
solutions are referred to as electrolytes. These electrolytes are able to break down into
ions when dissolved in water, thus creating free ions in solution. Acids, bases, and
salts are examples of electrolytes. Substances with non-conductive aqueous solutions
are referred to as nonelectrolytes. These substances are often composed of covalent
bonds, and examples include carbon-containing compounds. Solutions with high
concentration of ions will exhibit high conductivity. Solutions with low concentration of
ions will result in small conductivity reading. A few factors that affect conductivity
measurement are temperature, concentration of ions, and the nature of ions present in
solution.
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LABORATORY MANUAL
PH METER
PH meter, electric device used to measure hydrogen-ion activity (acidity or
alkalinity) in solution. Fundamentally, a pH meter consists of a voltmeter attached to a
pH-responsive electrode and a reference (unvarying) electrode. The pH-responsive
electrode is usually glass, and the reference is usually a silver–silver chloride electrode,
although a mercury–mercurous chloride (calomel) electrode is sometimes used. When
the two electrodes are immersed in a solution, they act as a battery. The glass electrode
develops an electric potential (charge) that is directly related to the hydrogen-ion
activity in the solution (59.2 millivolts per pH unit at 25 °C [77 °F]), and the voltmeter
measures the potential difference between the glass and reference electrodes.
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LABORATORY MANUAL
LABORATORY GLASSWARES
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LABORATORY MANUAL
BOTTLE, WEIGHING BURRET
CONDENSER
CRUCIBLE HOLDER, WALTER CRUCIBLE, PORCELAIN, WITH LID
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LABORATORY MANUAL
DISH, EVAPORATING DISH, RECRYSTALLIZING
FLASK, DISTILLING FLASK, FILTER FLASK, VOLUMETRIC
GLASS, WATCH PIPET
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LABORATORY MANUAL
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LABORATORY MANUAL
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ST. PAUL’S COLLEGE,
KALAMASSERY
Re-accredited with ‘A’ Grade (Third Cycle) by NAAC
(Affiliated to Mahatma Gandhi University, Kottayam)
HMT P.O., Kalamassery, Ernakulam, Kerala 683503
