Overview

This laboratory manual integrates some of the important characteristic reactions of inorganic
compounds and the qualitative predictions of their properties. Analysis of cations and anions as
well as the syntheses of inorganic compounds with therapeutic properties will be carried out
using careful laboratory techniques.
The volume of the solutions handled in carrying out qualitative analysis for ions is generally less
than 5 mL. Most often, reagents are added drop by drop to 2-3 mL of solution. The ions to be
identified are present in the unknown solution at concentrations of approximately 0.1 M to 0.001
M. Solid samples generally weigh from 0.01 to 0.1 g.
Some of the methods and apparatus used in the qualitative analysis laboratory are identical to
those used in laboratory work on a larger scale. Other methods and apparatus must be modified
because of the relatively small amounts of material being handled. The following sections are
intended to familiarize you with the equipment, reagents, and procedures necessary for
semimicro qualitative analysis.
Equipments, Reagents, and Glasswares in Qualitative Analysis
The apparatus for qualitative analysis includes beakers, flasks, graduated cylinders, and test
tubes. The sizes of these items are those appropriate to the semimicro scale:10 -400 mL for the
beakers and Erlenmeyer flasks; 10-50 mL for the graduated cylinders, 10 x 75 mm (3 mL) for the
centrifuge tubes, and 5-10 mL for the test tubes.

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1. Graduated cylinders: they are useful for measuring liquid volumes to within about 1%. They
are for general purpose use, but not for quantitative analysis. If greater accuracy is needed, use a
pipette or volumetric flask.

2. Burettes: It is used to deliver solution in precisely-measured, variable volumes. Burettes are

used primarily for titration, to deliver one reactant until the precise end point of the reaction is
reached.

3. Volumetric flasks: It is used to make up a solution of fixed volume very accurately. To make
up a solution in volumetric flask, first dissolve the solid material completely, in less water (or
solvent) than required to fill the flask to the mark. After the solid is completely dissolved, very
carefully fill the flask to the mark. Move your eye to the level of the mark on the neck of the
flask and line it up so that the circle around the neck looks like a line, not an ellipse. Then add
distilled water a drop at a time until the bottom of the meniscus lines up exactly with the mark on
the neck of the flask. Take care that no drops of liquid are in the neck of the flask above the
mark. Finally, cover the flask by its cover and remember to mix your solution thoroughly, by
inverting the flask and shaking.

4. Pipettes. A pipette is used to measure small amounts of solution very accurately. Two types
of pipettes commonly used are transfer pipettes and measuring pipettes.

a. Transfer pipettes include volumetric pipettes and are designed to deliver accurately a fixed
volume of liquid such as standard solutions and non-viscous samples, and consist of a cylindrical
bulb joined at both ends to narrowed glass tubing. These pipettes are allowed to drain by
gravity.

b. The second type of pipette is the graduated or measuring pipette. Two kinds are available: the
Mohr pipette and the serological pipette. Mohr pipette is calibrated between two marks on the
stem, and the other has graduation marks down to the tip. Some types of serological pipettes are
marked of blow-out, these types need to blowout the remaining drops of liquid in the tip.

5. Erlenmeyer flasks and beakers: They are used for mixing, transporting and reacting, but not
for accurate volume measurements, the marking on these pieces of glassware are generally only
accurate to within 5%.

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6.Wash bottle. A wash bottle is used to provide distilled water for diluting solutions, washing
precipitates, and rinsing glassware.

Handling Solutions and Reagents

Measuring and transferring solutions and reagents.
Relatively large amounts of solutions, say, greater than 2 to 3 mL, are measured and transferred
in graduated cylinders. When pouring a liquid from one container to another, direct the stream
of liquid down a stirring rod as shown in Figure 6.

To add a reagent dropwise to a test tube, hold the dropper vertically above the test tube so that
the drops fall in the center of the tube (Figure 7). Do not let the dropper touch the solution or the
side of the container to which the reagent is being added. This technique avoids carrying
contaminants back to the reagent bottle and also gives drops of uniform size. Contamination of
reagents is frequently caused when some of the solution to which the reagent is being added is
taken up in the dropper or when the reagent is allowed to bubble up into the rubber bulbs.

When you pour from a reagent bottle pick up the bottle so that the label faces the palm of your
hand. In this way, any reagent that drips a label soaked with a hazardous chemical. Among the
most common mistakes that students make are adding too little or too much reagent Either
mistake is serious. If too little reagent is used to precipitate an ion or a group of ions, some of
those ions will be left in solution and will interfere with tests for others. If too much reagent is
added the ions in question may form complexes that do not behave as expected. The directions
must be followed closely, and it is wise to test for completeness of precipitation by filtering or

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centrifuging and testing the filtrate with another drop of reagent. In other words, it is better to
add too little and then add more than to add too much at the beginning.
Weighing solid
Quantities of solid reagents are determined either by weighing the solid or by estimating the
mass of the solid. A triple beam balance can very easily be used to measure masses to +/- 0.01 g
and in qualitative analysis, greater precision is not needed. Many times the mass can be
estimated by the relative size of the sample, for example, a sample the size of a small pea weighs
about 0.1 g and a sample the size of a grain of rice weighs about 0.02g. The sample mass can
also be compared to a display of common reagent samples of various sizes. Samples of solids
should be poured slowly from the bottle onto a watch glass.
Diluting and Mixing Solutions and Reagents.
Only distilled water should be used for diluting a reagent or any solution used in qualitative
analysis. Remember that a concentrated acid is always added to water so that the heat generated
is taken up in the solution and spattering of the acid is avoided. In fact, it is always good practice
to add a concentrated solution to a dilute solution. Thorough mixing is necessary when reagent
s are being added to test solutions. When the reaction vessel is a beaker or a flask, the solution
can be mixed by gently swirling the solution around in the container. Solutions should be mixed
frequently during the addition of reagents.
Mixing in a test tube is a little more difficult, but it can be done in several ways. Tapping a test
tube that contains a relatively small amount of solution will agitate its content (see figure below).

Figure 9. Proper mixing solution in a test tube

Heating Solutions
Solutions in test tubes are most safely heated in a water bath. A convenient water bath consists
of a 250-mL beaker covered by a piece of metal or metal foil with holes cut in it that
accommodate test tubes (Figure 8). A rubber band wrapped around a test tube near the top will
make it easier to remove from the bath. Another way to support test tubes in the water bath is
with a rack made of twisted wire as shown in Figure 9.
Heat a solution in a test tube over a flame only if the test tube is less than one-third full, if you do
it very gently over a small flame, and if the end of the test tube is pointed so that no one can be
splattered if the liquid bumps out of the tube. By heating the liquid along the side of the test
tube, rather than at the bottom, superheating and bumping are avoided. Remove the tube from
the flame at the first sign of boiling. And one more reminder-always hold the test tube in a test
tube holder, never in your fingers.

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Solutions in beakers or flasks are placed on a wire gauze supported by a ring for heating over an
open flame. The beakers or flasks should be held in place by a second clamp or ring so that they
will not fall off the wire gauze.

Evaporating Solutions
An evaporating dish is placed on a wire gauze and heated with a flame. The flame can be moved
around so that the sides and bottom of the container are heated uniformly. A crucible is
supported on a wire triangle and heated in the same way or held in a pair of crucible tongs, with
the tongs on the outside of the crucible (Figure 10). Do not place one tip of the tongs on the
inside of the crucible or any other container that you are holding in this way. Move the crucible
around slowly so that the solution wets the walls, where it evaporates more. The walls of
porcelain vessels hold heat and the last bit of solution should be allowed to evaporate after the
vessel has been removed from the flame. In this way, overheating or igniting the residue is
avoided. Note that if the fumes from the evaporation are toxic or corrosive, the evaporation
must be done in the blood

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Testing Solution
For testing the pH, a drop of the solution being tested is removed on the end of a stirring rod and
touched to the litmus paper. Do not drop the test paper into the solution, for this will cause
contamination and the paper can soak up the unknown solution, which may be of small volume.
Handling Precipitates
The procedures of qualitative analysis are designed so that precipitation is as complete as
possible. This is achieved, for example, by using excess reagent, by controlling the temperature,
or by adjusting the pH of the solution. The directions should be followed carefully, but in each
case, after precipitation appears to be finished, the supernatant solution should be tested for
completeness of precipitation by adding another drop of reagent. This can usually be done after
centrifugation, but before separating the precipitate and the supernatant solution. If a precipitate
forms, more reagent should be added until precipitation again appears finished. The solution
should then be tested once more, and the precipitation repeated yet again if necessary.
Precipitates are sometimes classified on the basis of their appearance. Coarse precipitates vary
from regularly shaped, large crystals (similar to table salt or sugar crystals) to irregularly shaped,
smaller crystals (similar to coffee grounds). These precipitates settle rapidly and are easy to
separate from the supernatant solution. Fine precipitates are individual particles that are almost
invisible to the eye (similar to face powder or flour). These precipitates may be more difficult to
separate from the supernatant solution than the coarse precipitates.
Gelatinous precipitates are sticky, jellylike masses that are difficult to separate from the
supernatant solution without further treatment. Colloidal precipitates, which are very finely
divided , do not settle to the bottom of a solution and are not filterable. They are also
undesirable because they readily adsorb the ions of other substances. Sometimes gelatinous and
colloidal precipitates can be converted to more manageable crystalline forms by heating for a
period of time-a process called digestion. Colloidal precipitates can sometimes be flocculated by
adding an electrolyte such as NH4NO3 to the hot suspension.
Separating Precipitates by Centrifugation
In a centrifuge, a mixture in a tube is spun at the end of a rotor so that centrifugal force drives
any precipitate to the bottom of the tube (Figure 13). The length of time required for separation
varies with the density and the size of the precipitate particles, as well as with the speed of the
centrifuge. Dense, large crystals separate in a few seconds. Finely divided solids take longer to
settle out-up to several minutes for those that are almost colloidal. To use the centrifuge, place
the sample tube in one of the spaces in the rotor and in the opposite space place a balancing tube
of the same size filled with a volume of water equal to that of your solution.

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Washing the Precipitates
To wash a precipitate, introduce the washing liquid, stir up the precipitate so that it is thoroughly
mixed with the liquid, recentrifuge, and remove the supernatant solution as before. This solution
is usually added to the original one. Washing two or more times with small proportion. The
supernatant solutions from washings after the first one can usually be discarded. Incomplete
washing of a preciptate is a common source of error in qualitative analysis.
Separating precipitates by filtration
The technique for separating a precipitate by filtration is illustrated in Figure 16. The procedure
is as follows: Fold a circular piece of filter paper in half and then in half again, and tear one
corner off (Figure 17). Fit the paper into a funnel, preferable so that the fit is tight at the top and
loose at the bottom. Next, wet the filter paper and press it against the funnel. The stem of the
funnel should be in contact with the side of the vessel in which the filtrate is being collected. Put
some water through the funnel to be sure that it flows easily. Pour the mixture containing the
precipitate down a stirring rod as shown in Figure 16. The last traces of precipitate can be
washed out with some of the filtrate or scraped out with a rubber policeman(Figure 18).

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 Laboratory Safety Guidelines
Any experiment, no matter how often it has been performed in the past, has the potential to
fail with hazardous results. By knowing the hazards, you will develop a healthy respect for what
is happening around you, and with this respect, heightened levels of observation are sure to
follow. This implies that potential accidents can be spotted before they can occur. The
following sections present some general guidelines for your safety while performing General
chemistry experiments.
1. Safety goggles are required in the laboratory AT ALL TIMES.
2. Contact lenses are not permitted in the lab. Laboratory fumes can dry your contacts out and
may result in the necessity of an operation for their removal.
3. Laboratory gowns must be worn at all times.
4. Sandals, open-toed shoes and high heels are not permitted in the lab. This is to protect your
feet from splashes and spills.
5. Never wear clothes that hang such as loose sleeves. Be sure ties and scarves are tucked well
inside your laboratory apron. These pose fire hazards as well as chemical hazards.
6. Long hair is to be constrained.
7. Never smoke in the laboratory or use open flames in operations involving low-boiling
flammable solvents. Ethyl ether and petroleum ether are particularly hazardous, but other
common solvents such as Acetone and Ethanol can be dangerous as well.
8. Handle strong acids or bases, bromine, and other corrosive chemicals with great care and
never allow them in contact with skin or eyes. Spills of such chemicals must be cleaned up
immediately, using an appropriate neutralizing agent and plenty of water.
9. Use safe techniques for inserting and removing glass tubing. Great care must be exercised
when inserting or removing thermometers and glass tubing from stoppers and thermometer
adapters, since severe lacerations can result from accidental breakage.

General Reminders
1. Do Not Pipette By Mouth – Ever
2. Read the Chemical Safety Information
3. Dress appropriately
4. Identify the Safety Equipment
5. Don’t taste or sniff chemicals
6. Absolutely no horseplaying.
7. Always read the upcoming experiments carefully and thoroughly, being sure to understand all
of the directions before entering the lab.
8. Absolutely no food or beverages will be permitted inside the lab.
9. Wash your hands frequently.
10. Never pick up broken glassware with your bare hands, regardless of the size of the pieces.
11. Never put broken glass in a regular garbage can.
12. Always read the labels of reagents twice.
13. Never make unauthorized substitutions.
14. Never use reagents from an unmarked bottle.
15. If you are not feeling well, report it to the instructor immediately.

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16. Never heat a piece of glassware that is chipped or cracked unless otherwise told to do so by
your lab instructor. Heating defective glassware can cause that glassware to break, resulting in a
spill.
17. Light the burner properly..
18. Never take more of a reagent than you need.
19. Never return an unused portion of a reagent to its original container.
20. Never pour a waste chemical in the drain or put it in the garbage, unless otherwise instructed
to do so by your lab instructor. Waste bottles will be provided. Always pour waste in the
appropriate and labeled waste bottle.
21. To insert glass tubes or thermometers through stoppers or adapters, first lubricate both the
glass and the stopper with glycerin or stopcock grease. Then, using a towel, cloth or other hand
protection, and holding the glass tube or thermometer near the end closer to the stopper, insert
the glass tube into the stopper, a few mm at a time, using a rotating motion.
18. When heating in a test tube, hold the test tube at about 45o angle. Be sure the opening of the
test tube is pointing away from anybody else. Never heat the bottom of the test tube instead heat
the middle of the test tube just at the level of the liquid in the test tube, Move the test tube
horizontally back and forth across the flame to prevent the liquid from heating too quickly.
Should the liquid begin to overheat, remove the test tube from the flame and allow the contents
to cool for a minute or so.
22. Never look down the opening of ANY container, including beakers, flasks, and test tubes.
23. Do not use graduated cylinders for any purpose other than to measure a volume of a liquid
24. Never put a dropper into a reagent bottle. Instead, put the reagent in a beaker so you can
bring it back to your desk and use a dropper there.

FIRE

1. In the event of a fire, DON”T PANIC!

2. If a small portion of your clothes catches fire, the fire may be extinguished by patting it out.
3. If a larger portion of your clothes should catch fire, there are three options for putting the
flames out. (1) Drop to the ground and roll. (2) Use the safety shower. (3) Use the fire blanket.
4. Never use a fire extinguisher on a person.
5. If a fire should occur in a beaker or some other container, cover it with a glass dish or other
flame-retardant item.
6. Never move any object that is burning.
7. Never use water to extinguish a chemical fire. Many flammable liquids float on water,
meaning that the water will have no effect but to spread the fire.
8.If a fire is large enough to warrant the use of a fire extinguisher, the proper use of the
extinguisher is as follows 1) Be sure there is an exit behind you in case you cannot get the fire
under control; (2) pull out the restraining pin (which requires breaking the plastic seal); (3) point
the extinguisher hose at the base of the fire; (4) holding the extinguisher UPRIGHT, squeeze the
handle to release the extinguishing media; (5) sweep the spray back and forth at the front of the
fire.

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Reacting to Accidents: First Aid

Any serious accident involving poisoning or injury should be treated by a competent physician.
If you witness an accident, you should summon the instructor immediately and leave the first aid
to him or her unless (1) no instructor or assistant is in the laboratory areas; (2) the victim requires
immediate attention, (3) you have had formal training in emergency first-aid procedures.
1. Eye Injuries
If any chemical enters your eyes, they should be immediately be flooded with water from an
eyewash fountain, with the eyelids kept open. If foreign bodies such as glass particles are
propelled into an eye, the injured person should get immediate medical attention. Removal of
such particles is a job for a specialist.
2. Chemical Burns
The affected area should immediately be flushed with water, using a safety shower if the area of
injury is extensive or if it is inaccessible to washing from a tap. Neutralizing solutions,
ointments, or greases should not be used on chemical burns unless specifically called for in a
first-aid procedure. Unless the skin is merely reddened over a small area, a chemical burn should
be examined by a nurse or physician.
3.Thermal Burns
For small thermal burns such as those inflicted by handling hot glass, a sterile gauze pad should
be soaked in a baking soda solution (2 tablespoons of sodium bicarbonate to a quart of lukewarm
water, about 2.4% NaHCO3), placed over the burn, then bandaged loosely in place. If the skin is
not broken, the burned part can be immersed in clean, cold water, or ice can be applied to reduce
the pain. Blisters should not be opened. Unless the skin is merely reddened over a small area,
the burn should be examined by a nurse or physician.
4. Bleeding, Cuts, and Abrasions
In case of a minor cut or abrasion, the wound and surrounding skin should be cleansed with soap
and lukewarm water that is applied by wiping away from the wound. A sterile pad should be
held over the wound until bleeding stops and then be replaced by a clean pad, which should be
secured loosely with a triangular or rolled bandage. The pad and bandage should be replaced as
necessary with clean dry ones. Contact between the wound and the mouth, fingers,
handkerchiefs, or other unsterile objects hould be avoided. Antiseptics should not be used on an
open wound.
5. Poisoning
If poison is swallowed, a physician or ambulance should be called immediately, and the victim
should be given 2-4 glasses of water or milk to drink. If it is safe to do so, vomiting should be
induced by placing a finger at the back of the victim’s throat or by having the victim drink a
glass of warm water in which 2 teaspoons of table salt have been dissolved (10 g in 200 mL).

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Vomiting should not be induced if the patient is unconscious, in convulsions, or has severe pain
and burning sensations in the mouth or throat, or if the poison is a petroleum product or a strong
acid or alkali. When vomiting begins, the victim should be placed face down with head lower
than hips, and vomiting should continue to be induced until the vomitus is clear. When there is
time, the poison should be identified and an appropriate antidote given. If the poison cannot be
identified and a physician is not present, a heaping table spoon (15 g) of the following universal
antidote can be given in a half glass of warm water; 2 parts activated charcoal, 1 part magnesium
oxide (milk of magnesia) and 1 part tannic acid. A sample of the poison should be saved for the
physician if possible. If the poison is a highly toxic gas such as hydrogen cyanide, hydrogen
sulfide, or phosgene, the persons attempting to rescue the victim should wear gas masks while
they are in contact with the vapors.
6. Chemical Hazards
For your own health and safety, it is essential that you exercise caution while handling chemicals
and minimize your exposure to them. Read the Material Safety Data Sheet for each chemical
reagent that you handle in the lab.

Chemicals and Chemical Spills

1. Report all chemical spill IMMEDIATELY to your lab supervisor.
2. Should a chemical spills on your person, immediately remove all affected clothing and wash
the affected body area with copious amounts of water.
3. Small spills on the bench or floor must be cleaned up immediately. Sodium bicarbonate and
vinegar are included as part of the safety equipment for neutralization of acids and alkaline
solutions respectively. Neutralize all acid and alkaline spills before cleaning. If you are not sure
how to clean a spill, inform your professor immediately.
4. Be careful of spills around the balances. These electronic devices are extremely sensitive to
corrosion. Mercury poses a particular hazard as vapors from the liquid. Report any spills of
mercury as quickly as possible so it can be cleaned up immediately.
What to Do if a Mercury Thermometer Breaks
1. Tell the students to leave the room.
2. Put on nitrile or latex gloves.
3. If there are any broken pieces of glass or sharp objects, pick them up with care. Place all
broken objects on a paper towel. Fold the paper towel and place in a zip lock bag. Secure the bag
and label it as directed by your local health or fire department.
4. Locate visible mercury beads. Use a squeegee or cardboard to gather mercury beads. Use slow
sweeping motions to keep mercury from becoming uncontrollable. Take a flashlight, hold it at a
low angle close to the floor in a darkened room and look for additional glistening beads of
mercury that may be sticking to the surface or in small cracked areas of the surface. Note:

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Mercury can move surprising distances on hard-flat surfaces, so be sure to inspect the entire
room when "searching."
5. Use the eyedropper to collect or draw up the mercury beads. Slowly and carefully squeeze
mercury onto a damp paper towel. Place the paper towel in a zip lock bag and secure. Make sure
to label the bag as directed by your local health or fire department.
6. After you remove larger beads, put shaving cream on top of small paint brush and gently "dot"
the affected area to pick up smaller hard-to-see beads. Alternatively, use sticky tape, such as duct
tape, to pick up any remaining small glass fragments. Place the paint brush or duct tape in a zip
lock bag and secure. Make sure to label the bag as directed by your local health or fire
department.
7. OPTIONAL STEP: It is OPTIONAL to use commercially available powdered sulfur to absorb
the beads that are too small to see. The sulfur does two things: (1) it makes the mercury easier to
see since there may be a color change from yellow to brown and (2) it binds the mercury so that
it can be easily removed and suppresses the vapor of any missing mercury. Where to get
commercialized sulfur? It may be supplied as mercury vapor absorbent in mercury spill kits,
which can be purchased from laboratory, chemical supply and hazardous materials response
supply manufacturers.
Note: Powdered sulfur may stain fabrics a dark color. When using powdered sulfur, do not
breathe in the powder as it can be moderately toxic
8. Remember to keep the area well ventilated to the outside (i.e., windows open and fans in
exterior windows running) for at least 24 hours after your successful cleanup.

I, the undersigned student have read this safety document and understood it.

Name of Student: _____________________

callejas, shakira shane
Signature of Student: ______________________
Name of Professor:chistopher
_______________________
jay t. robidillo Date: _______________________
6/14/22

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