FACULTY OF FOOD SCIENCE AND NUTRITION

NT10402
ANALYTICAL CHEMISTRY

EXPERIMENT 1 : LABORATORY TECHNIQUES

LECTURER/ : DR. NORLIZA BINTI
JULMOHAMMAD
DEMONSTRATOR SIR WILLIE YEN
SIR WILTER KISIN

GROUP NUMBER : GROUP 4E

DATE (DAY) OF EXPERIMENT : 21st FEBRUARY 2019 (THURSDAY)

NAME MATRIC NO. SECTION SIGNATURE

NORKHAIRUNNISA ZULLIZAWATI BN18110210 1

BINTI MOHD ZULKARNAIN
MUHAMMAD IRSYAD BIN BN18110060 1
HAMZAH
NILAM NADHIRAH BINTI LAMDIN BN18110213 1
RAZSYAFIQAH BINTI MAIDIN BN18110207 1
NORASHIMA BINTI PATRICK BN18110080 2
MELISSA BASILIUS BN18110141 2
EXPERIMENT 1 : LABORATORY TECHNIQUES

(a) The Laboratory and SI

Introduction

All chemical principles, tools, and techniques are developed in the laboratory. The
experience of observing a chemical phenomenon and then explaining its behaviour is
one that simply cannot be gained by reading a textbook, listening to a lecturer,
searching the Internet, or viewing a video. It is in the laboratory where chemical
principles are learned and applied to the vast natural “chemistry laboratory” that we
call our everyday environment. The objectives of a laboratory experience are to
design and build apparatus, develop techniques, observe, record and interpret data,
and deduce rational theories so that the real world of science is better explained and
understood.

Other than that, one of the main reasons to question the place of laboratory
teaching is that laboratory programme are very expensive in terms of facilities and
materials, but also, more importantly, in terms of staff time (Carnduff and Reid,
2003). In the laboratory, there are common equipment and safe chemicals going to be
used to perform experiments. The experimental observations will be recorded and the
data on the basis of sound chemical principles will be interpreted. A good scientist is a
thinking scientist trying to account for the observed data and rationalize any
contradictory data. In the first few laboratory sessions some basic common rules and
techniques and some situations will be introduced.

SI units are also important throughout the whole laboratory work since there are
many different units (e.g., inches, feet, centimeters), scientists developed SI units to
avoid confusion, therefore, by using common units, scientists from different countries
and cultures can easily interpret each others' result (Kevin Carr, 2018). Accuracy and
precision are important while taking scientific measurement. This is important since it
will identify either the result is exact or not due to errors occurring while taking the
measurement. Therefore, the skills in the use of SI units must be developed by doing
practicals to avoid inaccuracy while doing laboratory works.
Objective

i. To learn the rules of laboratory safety and necessity of practising these rules in
the laboratory.
ii. To learn how to properly organize and record laboratory data.
iii. To develop skills in the use of SI units.

Laboratory Questions Part A

(A) Read the Laboratory Safety and Guidelines section and answer the following as
true or false.

No Question True False

.
1 Prescription glasses, which are required by law to be “safety /
glasses,” can be worn in place of safety goggles in the laboratory.
2 Sleeveless blouses and tank tops are not appropriate attire for the /
laboratory.
3 Only shoes that shed liquids are permitted in the laboratory. /
4 Your laboratory has an eyewash fountain. /
5 A beaker containing an acidic solution has broken on the bench
top and spilled onto your clothes from the waist down and it
burns. Ouch! You should immediately proceed to the safety /
shower and let the water flow on the affected area.
6 You received a paper cut on your finger and it is bleeding.
Immediately go to the medicine cabinet to apply a disinfectant /
7 Cell phones, iPods, and other electronic equipment should be
turned off during the laboratory period. /
8 It is good laboratory protocol to inform other students when they
are not practicing good laboratory safety procedures. If they
continue to not follow the safety procedures, you should “rat” on /
them . . . tell the laboratory instructor.
9 Your friend is a senior chemistry major and thoroughly
understands the difficult experiment that you are performing.
Therefore, it is advisable (even recommended) that you invite /
him or her into the laboratory for direct assistance.
10 You missed lunch but brought a sandwich to the laboratory.
Since you cannot eat in the lab, it is okay to leave the sandwich
in the hallway and then go in and out to take bites while the /
laboratory experiment is ongoing.
(B) Write a short response for the following questions.

1. What does the phrase “neck to knee to wrist” mean with regard to laboratory
safety?
 Its refers to the clothing which should be wear in the laboratory.

2. The first action after an accident occurs is:

The first action after an accident occurs is report it to the instructor immediately.

3. You want to try a variation of the Experimental Procedure because of your

chemical curiosity. What is the proper procedure for performing the experiment?
Carefully consider what the propose of experiment to do and ask your instructor
for permission.

4. A chemical spill has occurred. What should be your first and second action in
treating the chemical spill?
Notify the instructor immediately and quickly identify the spilled material.

5. Describe how you will be dressed when you are about to begin an experiment in the
laboratory.
Approved safety goggles, wearing a shirt that covers the stomach and lower back as
well as the upper arms, long pants, and wearing shoes that completely cover the
foot.

(C) Read the Laboratory Data and answer the following as true or false.

No Question True False

.
1 “Quick data,” such as that of a mass measurement on a balance
located at the far side of the laboratory, can be recorded on a
paper scrap and then transferred to the Report Sheet at your lab /
station.
2 Data that has been mistakenly recorded on the Report Sheet can
be erased and replaced with the correct data. This is to maintain a /
neat Report Sheet.
3 All data should be recorded in permanent ink! /
4 The laboratory equipment and instrumentation determine the
number of significant figures used to record quantitative data. /
5 Zeros recorded in a measurement are never significant figures. /

(D) Convert each of the following using the definitions in Table 1 and unit conversion
factors. Show the cancellation of units.

(i) 10 g to pound (vi)

1g 0.0022lb
10 g 0.0022lb 0.0221lb 1Btu 1.054kJ
3
1.7 10 Btu 1.054kJ 1791.8kJ
(ii) 1.00 qt to cm3 (vii)
946.3 ml (viii) 14.70 psi to kPa
(iii) 1.00qt x x
1 qt
(ix)
1atm 14.70 psi
1 cm3 3
= 946.3 cm 1atm 101.325kPa
1 ml
(iv) 14.70 psi 101.325kPa
(x)
(v) 1.7 x 103 Btu to kJ
(xi) 4.76 pm to μm
4.76 10  12 m 4.76 10  12 m
4.76 10  12 m 10 6 4.76 10  6 m

b) Basic Laboratory Operations

Introduction

In this experiment, several common techniques that are used repeatedly throughout
the laboratory manual can be learned . Methods of using laboratory balance and
pipette can be learned and practiced. The objective in using laboratory balance is to
develop techniques to transfer samples of material from one container to another and
to get the amounts transferred to a precision of one tenth of a milligram or one ten
thousandth of a gram, ±0.0001 g ( Professor Emeritus, 2018). Pipette is a precision
instruments it may be, and the accuracy of the pipettes depends on the observer.
Practicing a good technique and have an understanding on how it work would help in
getting an accurate result (Oswald , 2016)

Objectives

i. To develop the skill for properly operating a balance.

ii. To develop a technique of using a pipette.
iii. To determine the density of an unknown substance.

Apparatus and Materials

Test tube Unknown liquid 2

Water Graduated cylinder
Spatula Balance
Unknown liquid 1 Pipette
Beaker
Methods

1. The mass of the test tube, spatula, beaker and graduated cylinder was determined
using balance. The results were expressed with the correct sensitivity. The top-
loading balance were used after the instructor explains its operation. The mass of
the objects recorded according to the sensitivity of the balance.
a. The mass of water was determined and the result expressed in the correct
sensitivity.
i. A 10 ml graduated cylinder were obtained and its mass (±0.001g)
were measured and tared on assigned balance. 7 mL (±0.1 mL) of
water was added and the combined mass were measured. The mass of
7 mL of water were calculated .
ii. The water was discarded and the graduated cylinder was filled
again to the 7 mL mark. The mass measurement was recorded on the
Report Sheet . The procedure was repeated at least five times.
2. Determination the density of an unknown substance
a. Liquid, water
i. The smallest laboratory beaker was cleaned and dried . Its mass
were measured and recorded using assigned balance. 5 mL of water
was pipetted into the beaker. The mass of the beaker and water were
measured and recorded. The density of water were calculated from
the available data . The density determination for trial 2 was
repeated . The average density of water was calculated at room
temperature.
b. Liquid, unknown
i. The beaker and pipette were dried. The instructor was asked for a
liquid unknown and its number were recorded. The pipette was
rinsed with two 1 mL quantities of the unknown liquid and then was
discarded. 5 mL of unknown liquid were pipetted into the beaker. The
mass of the beaker and unknown liquid were measured and recorded.
The experiment for trial 2 was repeated. The average density of the
unknown liquid was calculated.

Precautions Steps
An analytical balance is a delicate instrument that must be handle with care. Consult
with instructor for detailed instructions on weighing with the particular model of
balance. Here are several general rules for working with an analytical balance
regardless of make or model:
1. Center the load on the pan as well as possible.
2. Protect the balance from corrosion. Objects to be placed on the pan should be
limited to nonreactive metals, nonreactive plastics, and vitreous, or glass like,
materials.
3. Observe special precautions for the weighing of liquids.
4. Consult your instructor if the balance appears to need adjustment.
5. Keep the balance and its case scrupulously clean. A camel’s-hair brush is useful
for removing spilled material or dust.
6. Always allow an object that has been heated to return to room temperature
before weighing it.
7. Use tongs, finger pads, or a glassine paper strip to handle dried objects to
prevent transferring moisture to them.
By following the precaution steps, the mass of the objects can be recorded with the
correct sensitivity.

Pipettes are pieces of laboratory equipment used to measure out precise volumes of
solutions in quantities. They allow to collect a small sample from a larger batch of
solution and then transfer that precise amount to a different area. That new area could
be another solution for mixing purposes, a cell sample holder, microscope slide or
many other places. Before doing any pipetting, we should know the proper
precautions to take to protect us from possible mistakes and keep the validity of the
experiment intact.

1. Make sure there is no water droplets adhering to pipette inner wall and cleaned.
2. Make sure the pipette is free of chips and cracks.
3. Do not insert the pipette tip directly into the reagent bottle.
4. By using a clean, dust-free towel or tissue, dry the outside of the pipette tip.
5. By using the suction from a collapsed rubber bulb, draw a 2- to 3- mL portion
into the pipette as a rinse.
6. Make sure the tip of the pipette well below the surface of the liquid in the beaker.
7. Do not ‘jam’ the pipette bulb onto the pipette.
8. Make sure the pipette is hold in a vertical position over a waster beaker, control
the delivery of the excess liquid until the level is ‘at the mark’ in the pipette.
9. Make sure to drop the suspended from the pipette tip by touching it to the wall of
the waste beaker.
10. Dispense the liquid along the wall of the receiving vessel to avoid splashing.
11. To remove hanging drop from the pipette tip, touch the side of the receiving flask
for its removal.
12. Make sure to rinse the pipette with several portions of deionized water and drain
each rinse through the tip once it is no longer needed in the experiment.

Practice using the balances.

Result

Object Description Of Object Mass (g)

Test tube Good 3.7047
Spatula Good 26.6856
Beaker Good 46.6843
Graduated cylinder Good 84.9532

Table 1
Discussion

The first objective for this experiment was to develop the skill for properly
operating a balance. Based on the result obtained, the mass of each object was
determined using the laboratory balance which is analytical balance.Analytical
balances are designed for great precision in quantitative chemical analysis. It is a
highly sensitive lab instrument that gives accurate mass measurements with
readability range between 0.1 mg - 0.01mg.

Based on table 2.1, the mass of objects was obtained by following the instruction
given by the instructor. First off all, the balance was made sure leveled and at zero
before weighing anything. The leveling on the balance was checked by looking at the
leveling bubble on the floor of the weighing chamber. The weighing process was done
once the balance was in right condition. The door of the analytical balance was
opened and the object was then placed directly on the balance pan carefully to be
weighed without using the weighing container. The following objects are test tube,
spatula, beaker and graduated cylinder. Then, it was important to make sure that the
analytical balance door was closed and was let undisturbed for a few second until the
unit stabilized. The weight is then recorded as shown in table 2.1.

While conducting this experiment, there were some errors occurred affecting the
result obtained. The errors were, the vibration from the other equipment that produced
vibration affect the precision of an analytical balance. A small vibration might disrupt
the delicate machinery of analytical balance, thus, it was always significant to
recalibrate the analytical balance. Other than that, air currents had also affected the
intricate mechanisms of the analytical balance and altered the measurement of the
small sample size. It means that, any environmental factors such as the changes in air
pressure from ceiling fans, air conditioners, and open doors could cause the sensitive
equipment to show wrong measurements. So, it was made sure that the analytical
balance door was closed right after placing and taking out the objects Lastly, random
error caused by an individual might as well affect the result such as by not wearing
gloves while handling the sample. It is because the moisture, grease and dirt from bare
finger affect the weight of the sample. Therefore, it is important to always wear
gloves while handling any types of chemical.

Mass of graduated cylinder (if not tared):

Trial 1 Trial 2 Trial 3 Trial 4 Trial 5
Mass of cylinder + H2O (g) 91.9199 91.9184 91.8165 91.8914 91.8278
Mass of 7 mL H2O (g) 6.9667 6.9652 6.8633 6.9382 6.8746
Average mass of 7 mL H2O(g) 6.9667  6.9652  6.8633  6.9382  6.8746
6.9216
5

Table 2
The second objective of this experiment was to develop a technique of using a pipette. In
this experiment, this technique was applied by preparing 7 mL of water. This technique
consists of preparation of the pipette, filling the pipette with water and delivery of water from
the pipette into the graduated cylinder. The mass of 7 mL of water was then calculated by
measuring the combined mass of 10 mL of graduated cylinder and 7 mL of water. The result
obtained for the mass of 7 mL of water in Trial 1, 2 and 4 were 6.9667 g, 6.9652 g and 6.9382
g respectively. However, the mass of 7 mL of water obtained from Trial 3 and 5 were 6.8633
 g and 6.8746 g respectively, which were slightly lower than the other three trials. These
obtained results were caused by some errors during pipetting. In Trial 3, parallax error occur
where the observer’s eyes were slightly higher than the meniscus when taking a reading of the
volume of water in the pipette that would be delivered into the graduated cylinder. By using
the mass of 7 mL of water from the five trials, the mean and standard deviation can be
calculated. The calculated mean for the mass of 7 mL of water is 6.9216 g while its standard
deviation is 0.0991 g.

6.9667 g  6.9652 g  6.8633 g  6.9382 g  6.8746 g

Mean,   6.9216 g
5

Trial  X X- (X- )2
 
1 6.9216 6.9667 0.0451 2.0340 × 10-3
2 6.9216 6.9652 0.0436 1.9010 × 10-3
3 6.9216 6.8633 -0.0583 3.3989 × 10-3
4 6.9216 6.9382 0.0166 2.7556 × 10-4
5 6.9216 6.8746 -0.0470 2.2090 × 10-3

Standard deviation, s = , where N = total number of trials

 (X -  )
N -1
s=
(2.0340 10  3 )  (1.9010 10  3 )  (3.3989 10  3 )  (2.7556 10  4 )  (2.2090 10  3 )
5 1
= 0.0991 g

Determination the density of an unknown substance.

Result

Liquid Water Unknown Liquid 1 Unknown Liquid 2

Mass of beaker (g) Trial 1 Trial 2 Trial 1 Trial 2 Trial 1 Trial 2
Mass of beaker + liquid (g) 51.674 51.754 51.777 51.903 51.858 51.768
Mass of liquid (g) 4.990 5.070 5.093 5.219 5.174 5.084
Volume of liquid (ml) 5.000 5.000 5.000 5.000 5.000 5.000
Density of liquid (g/ml) 0.998 1.014 1.019 1.044 1.035 1.017
Average density of liquid (g/ml) 1.006 1.032 1.026

Table 3
Discussion

Density is an intensive property of a substance that does not depend on the amount of
the substance present (Dr. Michael Evans, 2019). Thus, density can be used to identify
an unknown pure substance if a list of reference densities is available, and the
experimenter can choose a convenient amount of substance to work with when
measuring density. By definition, all matter has their own mass and volume(Dr.
Michael Evans, 2019). The density of a substance is the ratio of its mass to volume.
At constant temperature and pressure, the density of a substance is constant. In this
experiment, the density of water and two unknown substances were determined.

For measuring the density of a sample of a substance, it is necessary to measure

its mass and volume. In this experiment, mass was measured using an analytical
balance, a precise instrument that relies on the force exerted by the sample due to
gravity. The container to hold the sample and also be used to measure volume of the
liquid. The container that contained the sample was weighed and tared, so only the
sample mass appeared on the balance display. It was important to do few trials of
measuring the mass because errors while taking the readings might occur, therefore,
the trials will help minimizing the impacts of errors done in any one trial by averaging
multiple trials together and also by minimizing random effects and the effects of
uncontrolled variables by averaging multiple trials together (Rick Hewitt, 2016).

It is well-known that density is a characteristic intensive property of a substance.

Thus, density measurements can be used to identify an unknown pure substance if a
list of possible reference densities is available. Thus, in this experiment, the density of
two unknown substances was distinguished which were unknown liquid 1 and
unknown liquid 2. The volume of water and another two unknown liquids was kept
constant for 5 ml, whereas the average mass obtained from this activity were used to
calculate the density by using the following formula of density :

Table 3 lists the results for determination of the density of three substances using a
50-mL beaker. The average density was 1.006 ± 0.001 g/ml (water), 1.032 ± 0.001
 g/ml (unknown liquid 1) and 1.026 ± 0.001 g/ml (unknown liquid 2). Table 4
shows how the calculation on density was done. Overall, the density of water
calculated from this experiment was approximately similar as the actual value of
water density which is 1.00 g/ml, whereas the densities of unknown liquid 1 and
unknown liquid

Calculation :
Liquid Water Unknown Liquid 1 Unknown Liquid 2
Trial 1 Trial 2 Trial 1 Trial 2 Trial 1 Trial 2
Mass of 4.990 5.070 5.093 5.219 5.174 5.084
liquid (g)
Volume of 5.000 5.000 5.000 5.000 5.000 5.000
liquid (ml)
Density of
liquid (g/ml)

4.990 5.070 5.093 5.219 5.174 5.084

     
5.000 5.000 5.000 5.000 5.000 5.000
0.998 1.014 1.019 1.044 1.035 1.017
Average 0.998  1.014 1.019  1.044 1.035  1.017
  
density of 2 2 2
liquid (g/ml) 1.006 1.032 1.026

Table 4
However, even though the density of water obtained from this experiment was
approximately similar to the actual value of water density, it is still very important to
conduct this activity very carefully since it involves the uses of analytical balance to
weigh mass and pipette to measure volume. As an example, the mass of unknown
liquid 1 for trial 1 and trial 2 shows the most obvious difference of values that was
probably caused by random errors. The sources of random could be due to
environment factor tilting slightly as people move around the laboratory. Thus, this
source of error could be minimized by placing the analytical balance on heavy table
with least motion around the place so that the pressure applied while taking mass
readings could be minimized. This prevention should be taken quite seriously since
mass is an influential factor towards determining the density of substances.Last but
not least, the volume of liquids would also affect the density of the substances,
therefore, it is important to get used to pipette by always practicing it so that accurate
volumes of substances could be measured. In this experiment, parallax error while
measuring the volume of water and another two unknown substances was made sure
not occur in order to get quite similarly 5 ml volume for each of them. Therefore, the
volume measured in this experiment did not really affect the density of the substances.

Laboratory Questions

1. Suppose that after delivery several drops of water cling to the inner wall of the
pipette (because the pipette wall is dirty). Will this technique error increase,
decrease, or have no effect on the reported density of water? Explain.

If there are several water droplets cling to the inner walls of the pipette after
delivery due to the dirt remains on the pipette wall, the overall result obtained will
be affected, in which, the volume of water will be much lower than the exact
volume. In this case, the density of water being calculated will then be higher than
the actual density of water. The reason is because when the mass of water remains
constant where the volume differs in value, the reported density will also differ,
for instance, when the volume is lower, therefore, the density of water will be
greater.

2. The unknown liquid is volatile. If some of the liquid evaporates between the time
the liquid is delivered to the beaker and the time its mass is measured, will the
reported density of the liquid be too high, too low, or unaffected? Explain.

If some of the liquid evaporates between the time it's delivered to the beaker and
the time its mass is measured, the reported density of the liquid would slightly
then be lower than the expected actual density. Even though the volume of the
liquid remains constant, however, the recorded mass is going to be lower than the
exact mass. Therefore, the recorded density of the liquid will be much lower than
the real value.

Conclusion
From the experiment that we have done, we can learned several general rules of
laboratory safety and necessity of practising these rules in laboratory to prevent and
eliminate hazards. Plus, we will also know the proper steps to take in the unfortunate
event that something does go wrong. Other than that, we also have learned on how to
properly organize and record laboratory data so that the reliability and credibility of
the experimental data are upheld. Next, skills in the use of SI units are developed, like
kilogram(kg) for mass, meter (m) is the SI base unit for length and kelvin (K) for
temperature. There are also some prefixes in SI unit that we have learned and will be
frequently used in all basic measurements.

Other than that, we can developed the skill for properly operating a balance in
order to get accurate readings. Next, technique of using a pipette also developed for
dispensing liquid from a pipette for any quantitative determination. Next, with the
skills developed in using balance and pipette, we can determined the density of an
unknown substances which is 1.032 g/ml and 1.026 g/ml. Despite that, there are some
precautions that need to be taken before, after and during the experiment. There are
also some method need to be taken in order to avoid some error and to get more
accurate results.

References
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laboratories, pre-laboratory and post-laboratory exercises, examples and advice,
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balance
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stop-pipetting-errors-ruining-your-experiments/
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