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Experiment 1 - Common Laboratory Operations
Experiment 1 - Common Laboratory Operations
Experiment 1 - Common Laboratory Operations
Materials: potassium iodide (KI) solution, lead (II) nitrate [Pb(NO3)2] solution
Welcome to the chemistry laboratory! For the next few months in your life, you will be spending some of your
memorable times here. To make your stay in the chemistry lab a memorable one, you need to avoid accidents.
Avoiding accidents mean strictly following all necessary rules of operations.
For this experiment, you will be introduced to basic experimental techniques and associated glassware and
apparatus that are commonly used in the biochemistry laboratory. You need to remember that in the future, when
conducting experiments, you need to strictly follow the rules written here.
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Whenever flame or heating is required in the chemistry lab, we commonly use the Bunsen burner. Thus, it is
imperative that you identify its parts, know its functions, and operate the burner itself. Shown on the previous
page is a diagram of a Bunsen burner. Label the parts accordingly before the start of the lab period.
Guide questions:
2. What does it mean if you have bright yellow flame? How do you correct the problem?
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3. Why is a luminous flame not used during heating?
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Solid chemicals are generally kept in reagent bottles. Removal of solid chemicals from the reagent bottle should
be done by spatula or paper, not by bare hands. Any excess chemical that is already taken out from the bottle
should not be returned but should be disposed in designated waste disposal bin.
Procedure:
1. Turn on the top-loading balance and wait until you see a 0.0 g in the screen.
2. Place a small beaker on the pan of the balance. This will serve as your weighing container. Wait
until the digits in the screen stop moving.
3. Press “Tare”. Taring automatically zeroes the mass of the container.
4. Open the lid of the reagent bottle containing salt and lay the flat side of the lid on the table.
5. From the reagent bottle provided, transfer salt into the beaker using a spatula, small amount at a
time until the screen of the balance read 1.0 g. Do not return any excess sand back into the reagent
bottle.
6. Remove the beaker and set aside.
Procedure:
1. Cut a piece of paper with a width like the opening of a test tube and height that is like that of the test
tube with at least 2 cm excess. Fold the paper lengthwise.
2. Using a provided spatula, scoop the previously weighed salt in the beaker and transfer it on the
trough of the folded paper.
3. Fold the paper to secure the sand and carefully insert it inside the test tube until the tip touches the
bottom of the tube.
4. Gently tap the body of the test tube to deliver the solid directly to the bottom.
5. Close the reagent bottle. Keep the test tube with the sand for the following experiments.
Guide Question:
1. Why should any excess chemical not be returned to the reagent bottle?
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2. Why is the use of funnel no longer advisable when transferring solid into a test tube?
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Some of the chemicals you will encounter in the chemistry lab are in the form of solutions. It must be put to mind
that most solutions, even the hazardous ones, look like just water. Therefore, you need to handle all solutions
with care.
Procedure:
1. Half-fill a beaker with tap water from the faucet.
2. Measure 10 mL of water from the beaker using the graduated cylinder following the procedure below:
a. Touch mouth of the beaker to the mouth of the graduated cylinder and slowly pour water until
it reaches the line just a little below the 10 mL mark.
b. With a dropper, add water into the graduated cylinder until the lower meniscus of the water
inside the cylinder touches the 10 mL mark.
indentation
Fig. 2: Beaker
Source: https://cdn.images.fecom-media.com/HE1788994_1424793-PHE-PHY-P01.jpg?width=348&quality=75%201x,%20https://cdn.images.fecom-
media.com/HE1788994_1424793-PHE-PHY-P01.jpg?width=696&quality=75%202x
Procedure:
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3. Deliver water from the Erlenmeyer flask into the test tube by carefully running the water down through
the stirring rod until the test tube is filled not more than 1/3 of its total volume. Label the test tube “for
heating” and set aside.
Most reactions in the chemistry laboratory occur above room temperature. In this case, heating is necessary.
The flame during heating, as discussed previously, should be a non-luminous flame of a Bunsen burner.
Illustrated below are 2 set-ups for heating liquids:
Set up A is used to heat non-volatile and non-flammable liquids, such as water. On the other hand, set up B is
heating in a water bath and is used for heating volatile and flammable liquids, such as alcohol. The set-up is
applicable when heating 1-3 test tubes. If you are required to heat 4 or more test tubes, use the water pan that
is provided to you for more space.
Procedure:
1. Obtain the test tube from transferring liquid procedure that is labeled “for heating”. Note that this test
tube contains water that occupies not more than 1/3 of the test tube’s total volume. This volume
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should be followed every time you are heating. Heat the liquid in the test tube using Set up A. Follow
the procedures below:
a. Operate the Bunsen burner to give a non-luminous flame.
b. Securely fasten the labeled test tube with water with a test tube holder.
c. Do not cover the test tube with anything.
d. Heat the test tube at the surface of the water while slanting it at 45o angle. Make sure that
the mouth is pointing away from you or from anybody.
2. Fill another test tube with water not more than 1/3 of its total volume. Pretending the water inside is
a flammable solution, such as ethanol, heat the test tube using Set Up B. Follow the procedures
below:
a. Half-fill a 500 mL beaker with water.
b. Construct a set up similar to Set up B making sure to use non-luminous flame.
c. Heat the water in the beaker until boiling.
d. Secure the test tube with a test tube holder and place in the water inside the beaker.
Guide Questions:
1. Why is not good to cover the test tube with a cork while heating?
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2. Why are flammable liquid not heated using Set up A (direct heating)?
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3. When heating liquid using Set up A, what is the importance of moving the test tube back and forth through the
flame?
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V. FILTRATION
Filtration is a process of separating solid from liquid solution using a filtration membrane, in most cases a filter
paper. It has two main purposes. The first is to remove solid impurities from a liquid. The second is to collect a
desired solid from the solution from which it was precipitated. The following illustration shows a filtration set up,
known as gravity filtration:
Fig. 5: Filtration
Source: https://www.bitlanders.com/blogs/filtration/195691
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The solid that is left on the filter paper after filtration is called residue. The liquid that comes out from the filter
paper is called filtrate.
The filter paper should be folded properly to ensure efficient filtration. The following illustration shows the proper
way of folding filter paper:
Procedure:
1. In a clean and dry test tube, mix the contents of the test tubes labeled “KI” and “Pb(NO3)2” from the
previous procedure of transferring liquids. Note that a colored solid is formed upon mixing. The solid
that is formed is called a precipitate.
• What is the color of the precipitate? _____________________
2. Construct a gravity filtration set up similar as the illustration presented before using properly folded
filter paper.
3. Pour the mixture containing the colored precipitate into the filter paper on the filtration set up. Notice
that the colored precipitate remains on the filter paper and a colorless solution comes out from the
filter paper.
4. Wash out the remaining precipitate from the test tube with small amount of water and pour into the
filter paper.
5. Set aside the filtrate and label the flask with “for evaporation.”
Guide Questions:
1. What type of reaction has occurred when you mixed the 2 solutions together? What evidence of chemical
reaction is observed?
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2. What is the chemical name and formula of the residue on the filter paper?
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3. What is the chemical name and formula of the soluble component of the reaction that is present in the filtrate?
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VI. EVAPORATION
Evaporation is a process of separating soluble solids from a solution. This is carried out by evaporating the
solvent to dryness leaving the solute residue behind. The following illustration shows the set-up for evaporation:
Fig. 7: Evaporation
Source: https://abbathetwiter.blogspot.com/2019/12/diagram-bunsen-burner-evaporation.html
As the solvent from the solution dries up, a solid product remains. This is called residue.
Procedure:
Guide Questions:
The solubility of a solute (a dissolved substance) in a solvent (the dissolving medium) is the most important
chemical principle underlying some of the basic techniques in the organic chemistry laboratory, such as
recrystallization, extraction, and chromatography.
Although we often describe solubility behavior in terms of a substance being soluble (dissolved) or insoluble
(not dissolved) in a solvent, solubility can be described more precisely in terms of the extent to which a substance
is soluble. Solubility may be expressed in terms of grams of solute per liter (g/L) or milligrams of solute per
milliliter (mg/mL) of solvent. Consider the solubilities at room temperature for the following three substances in
water:
Cholesterol 0.002 mg/mL
Caffeine 22 mg/mL
Citric acid 620 mg/mL
In a typical test for solubility, 40 mg of solute (a pinch) is added to 1 mL of solvent. Therefore, if you were testing
the solubility of these three substances, cholesterol would be insoluble, caffeine would be partially soluble, and
citric acid would be soluble.
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When the solubility of a liquid solute in a solvent is described, it is sometimes helpful to use the terms miscible
and immiscible. Two liquids that are miscible will mix homogeneously (one phase) in all proportions. For
example, water and ethyl alcohol are miscible. When they are mixed in any proportion, only one layer will be
observed. When two liquids are miscible, it is also true that either one of them will be completely soluble in the
other one. Two immiscible liquids do not mix homogeneously in all proportions, and under some conditions they
will form two layers. Water and diethyl ether are immiscible. When mixed in roughly equal amounts, they will
form two layers.
A useful generalization in predicting solubility is the widely used rule “Like dissolves like.” This rule is most applied
to polar and nonpolar compounds. According to this rule, a polar solvent will dissolve polar (or ionic) compounds,
and a nonpolar solvent will dissolve nonpolar compounds. Below is a list of organic compounds with their
corresponding polarities:
Procedure:
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Water Ethyl alcohol Hexane
Organic Compounds
(highly polar) (intermediate polarity) (nonpolar)
Benzoic acid
Citric acid
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