RCS1601 Chemistry 1A

EXPERIMENT 2

Use of Laboratory Balances, Calibration of a Pipette and Error Estimation

1. INTRODUCTION

1.1 Laboratory Balances

In the chemistry laboratory, measurement of mass is usually undertaken using either a top-loading balance or
an analytical balance. The top-loading balance typically has a capacity of 2 or 3 kg and displays the mass to two
or three decimal places. It is often used for the approximate measurement of mass. The analytical balance
may often have a capacity of less than 200 g and displays the mass to four or five decimal places. The analytical
balance is therefore the more accurate of the two types of balance and should always be used for precise mass
measurement. A top-loading balance would therefore be used to weigh, say, 200 g of ice for a small cold bath
and an analytical balance would be used to accurately weigh a sample of material for quantitative analysis.

Considerable care must be exercised when using both types of balance. Gentle addition of objects to the
balance pan shows respect for the delicate nature of these instruments. Cleanliness is equally important; any
spills must be cleaned up immediately using a brush for solids and paper towel for liquids. Should any material
fall into the internals of the balance, your instructor MUST be notified immediately.

In the first part of this laboratory session, an analytical balance will be used to measure the mass of a metal
block and a digital Vernier caliper will be used to measure the dimensions of the block. From these data, the
density of the metal will be calculated using the formulae:

density = mass/volume
volume = length × width × height

1.2 The Correct Use of a Pipette

A pipette is a common but important piece of glassware that is used in the chemical laboratory for the accurate
delivery of a particular volume of liquid. Possibly the most accurate and most commonly used pipettes are the
"bulb" type which can be obtained in various sizes typically: 1, 2, 5, 10, 20, 25, 50 mL, etc.

The correct use of a pipette is embodied in the following notes:

• Pour some sample liquid into a beaker (sample beaker) from which liquid will be withdrawn using the
pipette. Ensure that there is sufficient volume of liquid in the sample beaker knowing the volume you
wish to withdraw. Prepare the receiving flask or vessel close at hand.
• Liquid is taken into the pipette using a safety filler to apply suction.
Important: Always take extreme care when connecting a safety filler to a glass pipette. Do not force the
end of the pipette into the safety filler and hold the pipette at a position close to the top – never near the
tip. You must consult with your demonstrator if you are unclear about this.
• Rinse the pipette by drawing enough liquid to enable washing of the entire internal surface of the pipette.
Laying the pipette horizontally and rolling in both hands is also a good technique for rinsing it. This liquid
is then run into a beaker labelled "WASTE". This step ensures that no dilution (however small) of the
sample will occur (in case there was any washing/rinsing water in the pipette).
• After rinsing, use the safety filler to draw liquid into the pipette well above the graduation mark (GM).
• Carefully rest the tip of the pipette on the bottom of the sample beaker to reduce the rate of draining,
then remove the safety filler whilst quickly placing your index finger on the top of the pipette. You may
need to practice this manoeuvre several times using only distilled water until you can perform this step
confidently.
 RCS1601 Chemistry 1A – Experiment 2, cont’d.

• Holding the pipette vertically, reduce the pressure of your index finger on the end of the pipette and so
allow the level of the bottom of the meniscus to fall slowly until it coincides with the GM when viewed
level with your eye. Rest the pipette tip against the wall of the tilted sample beaker during this operation.
• Important notes are: (i) the bottom of the liquid meniscus should be adjusted to coincide with the GM
when viewed level with the eye, (ii) a pipette must be operated using one’s index finger to control the
drainage and not one’s thumb and (iii) a pipette must be held vertically whilst is drains.
• Remove the pipette from the sample beaker and keep your index finger firmly in place. Carefully remove
any droplets of liquid adhering to the outside of the pipette with a tissue. Under normal circumstances
this should not be necessary but, if it is necessary, take care to avoid touching the tip of the pipette with
the tissue.
• Place the tip of the pipette in the opening of the receptacle vessel (flask, beaker, etc.).
• Keep the pipette vertical, place its tip on the side of the receptacle vessel to avoid splashing, and release
your index finger to allow the liquid to drain into the receptacle.
• After the volume of liquid has been delivered, the pipette must be allowed to drain for a specified time.
Often, the time to be allowed for draining is printed on the pipette; it is quite commonly 15 s.
• Any liquid remaining in the pipette after this procedure is left in the pipette and is NOT forced out by
blowing down the pipette, etc.
• Excessive handling of the pipette bulb during its use should be avoided as this will cause a slight expansion
of the glass and will affect the volume of liquid that the pipette delivers.

1.3 Uncertainty in a Measurement

When one carries out a scientific measurement it is usual to quantify in some way the uncertainty (or "error")
associated with that measurement. If " replicate determinations $! , $" , $# , … $$ are carried out, then a
commonly used estimate of the error in the data is the standard deviation, '. This can be calculated using
Equation (1):

' " = [∑$%&!($̅ − $% )" ]/(" − 1) (1)

where $̅ is the mean of the data which is calculated in accordance with Equation (2):

$̅ = ($! + $" + $# + ⋯ + $$ )/" = (∑$%&! $% )/" (2)

In the second part of this experiment, the volume of a pipette will be accurately determined by weighing the
mass of water it delivers. The procedure will be repeated at least two times and the standard deviation of the
results will be used as an estimate of the error.

2. EXPERIMENTAL SECTION
Before starting this experiment, you will be instructed on the correct use of the analytical balance. Further
practice at using the analytical balance will be obtained in later exercises. Care must always be exercised when
using this instrument. All mass readings must be recorded to four decimal places.

You will also be instructed on the correct use of the pipette and this exercise will give you practice in its
operation.

2.1 Using the Analytical Balance

This short experiment will familiarize you with the operation of an analytical balance capable of weighing a
sample of up to approximately 200 g with an accuracy of either 0.1 mg or 0.01 mg. These types of balance are
commonly referred to as "4 and 5 decimal place" balances.

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 RCS1601 Chemistry 1A – Experiment 2, cont’d.

You will weigh each of two small metal blocks, measure their dimensions and hence calculate the density of
each metal.

(1) Obtain two metal "cubes" that are of different metals and a digital Vernier caliper (DVC). This device
enables accurate length measurements (up to about 150 mm) to be made. Take the DVC from its case and
turn on the display. Gently close the two sliding jaws and confirm that the display reads 0.0 mm. If it does
not, press the zero button.

(2) Gently open the jaws of the DVC, place them across one dimension of the first metal cube and slide the
jaws until they JUST touch the two opposite faces of the cube. Read the measured dimension of the cube
on the display. Repeat this process a few times until you are confident of the technique. Try to decide if
the cube has three parallel pairs of faces.

(3) Record in Table 1 in the laboratory report sheet (LRS) the three dimensions (4 × 5 × ℎ) of each of the
two cubes you have chosen. Do not forget to record in the LRS the type of metal of which each cube is
made. [See Question (1) in Section 3.]

(4) Wipe each metal cube with a tissue or paper towel to remove any dirt or fingerprints.

(5) Ensure that all glass sliding doors of the analytical balance are closed. The balance will probably be turned
on; if not, press the "ON" button and wait while it initializes itself (by turning on every element of the
display for a moment then displaying 0.0000 g (4 decimal place mode) or 0.00000 g (5-decimal place
mode).

(6) Using a pair of forceps, pick up the first metal cube and with great care, place it gently in the centre of the
balance pan. Close the sliding door. Allow the reading to become stable and record the mass reading in
Table 1 of the LRS. [See Question (1) in Section 3.]

(7) Repeat the weighing procedure with the second metal cube. [See Question (1) in Section 3.]

2.2 Calibration of a Pipette

In the following steps, you will use an analytical balance to accurately determine the mass of an empty weighing
bottle and its stopper. [N.B. During all weighing procedures in this experiment, avoid excessive handling of the
weighing bottle as grease or moisture from your fingers can be deposited on the bottle and this may affect the
reading.]

(1) Measure the temperature of the distilled water to the nearest 0.1°C. [See Question (2) in Section 3.]

(2) Record the mass of a dry, empty weighing bottle complete with its stopper (i.e. mass (bottle)/g) in Table 2
of the LRS. [See Question (3) in Section 3.]

(3) Pour some distilled water (more than 20 mL) into a clean beaker and rinse a 20-mL pipette with distilled
water using the recommended procedure given in Section 1.2.

(4) Remove the stopper from the bottle and, following precisely the procedure recommended in Section 1.2,
deliver 20 mL of distilled water to the pre-weighed weighing bottle using the pipette.

(5) Immediately replace the stopper on the weighing bottle and reweigh it. Ensure the balance has been
"tared" (i.e. re-set to read zero) before you place your weighing bottle on the pan to make your
measurement of its mass. Record in Table 2 of the LRS the mass of the weighing bottle plus the water
delivered by the pipette (i.e. mass (bottle + H2O)/g). Don’t forget the mass of the weighing bottle includes
the mass of it stopper! [See Question (3) in Section 3.]

(6) Repeat the procedure given in Steps (2) to (5) two more times and record all of your results in the LRS.

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 RCS1601 Chemistry 1A – Experiment 2, cont’d.

3. QUESTIONS AND CALCULATIONS

Instructions
• Answer ALL questions using the space provided in the LRS. Attach a separate sheet, clearly labelled with
the question number/s, if you have insufficient space in the LRS.
• Reports that are not submitted using the LRS will NOT be accepted.
• Answer Question (1) in Box (1), Question (2) in Box (2) and so on.
• Marks awarded for each question are shown at the bottom of each box along with the assessment
criteria.
• Show all working and/or reasoning for every question. Answers that are given as a single word, number,
letter, etc., will score zero.
• Final numerical answers should be quoted to the correct number of significant figures.

Questions
(1) From the measurement made in Steps (3) and (6) of Section 2.1 calculate the density of each of the metals
that you had chosen in units of g mL-1. Perform these calculations in the space provided below Table 1 of
the LRS, expressing your answer to the correct number of significant figures.
(2) Table 1 below lists the density of water as a function of temperature. If necessary, interpolate these data
to determine an accurate value of the density of water at the temperature of your experimental work.
Express this result to the correct number of significant figures. Referring to the data in Table 1 below,
does the density of water decrease or increase with increasing temperature? Explain briefly.

Table 1. Variation in the density of water with temperature

Temp/°C Density/g mL-1 Temp/°C Density/g mL-1
16 0.99897 23 0.99756
17 0.99880 24 0.99732
18 0.99862 25 0.99707
19 0.99843 26 0.99681
20 0.99823 27 0.99654
21 0.99802 28 0.99626
22 0.99780 29 0.99597

(3) In Table 2 of the LRS calculate the mass of water delivered by your pipette (i.e. mass (H2O)/g) in each of
the runs performed in Steps (2) to (6) in Section 2.2. Use the value of the density calculated in Question
(2) to determine the volume of water delivered in each case. Write these values in the appropriate
column in Table 2 of the LRS. Below Table 2 in the LRS, provide the full working (including units) of one of
the calculations of the volume delivered by your pipette as an example.
(4) Use the volume data calculated in Question (3) to determine the standard deviation in these data in
accordance with Equation (1) in Section 1. To do this, firstly transfer the volume data calculated in
Question (3) to the appropriate column of Table 3 in the LRS. Next, calculate the sum of the entries in the
first column (i.e. ∑$%&! $% ) and enter this at the bottom of that column as indicated. The value of the mean
of the data (i.e. $̅ = (∑$%&! $% )/") is entered at the bottom of the second column, as indicated, and can be
used to calculate each of the entries in that column. Each of the entries in the third column of Table 3 is
obtained by squaring the corresponding entries in the second column and the sum of the latter values is
calculated and placed at the bottom of the third column. Use the last value to calculate the standard
deviation in accordance with Equation (1) and show your working in the space provided below Table 3.
The final result should be expressed to the correct number of significant figures.
(5) Using the standard deviation as your estimate of the uncertainty, report in the LRS, the volume delivered
by your pipette as $̅ ± ' mL where $̅ is the average of the volume determinations, and ' is the standard
deviation. Ensure your result is reported to the appropriate number of significant figures and state the
temperature at which your result applies.
(6) Explain why it is important to keep the stopper on the weighing bottle after the water has been delivered
to it. [See Step (5) in Section 2.2.]

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 RCS1601 Chemistry 1A – Experiment 2, cont’d.

Detailed Marking Scheme for LRS

Assessable Detail Allocation

Aim Learn & practice correct use of particular laboratory equipment 1
Apply these skills in practical instances (two @ 1 ea) 2
Total 3
Q1 Correct observation of dimensions (three values @ ⅓ ea, x 2 metals) 2
Correct calculations on those dimensions (two calcs. @ ½ ea, x 2 metals) 2
Correct recording of masses (two values @ 1 ea) 2
Correct calculation of density incl. sig. figs. (2 metals @ 1 ea) 2
Correct unit of density 2
Total 10
Q2 Correct interpolation of density vs temperature data 3
Correct use of sig. figs. 1
Explanation of density variation with temperature 2
Total 6
Q3 Correct recording of masses (six times) 2
Correct calculation of mass of water (three times) 1
Correct calculation of volume of water (three times) 2
Total 5
Q4 Correct transcription of volume (three times) 1
Correct calculation of mean volume 1
Correct calculation of differences 1
Correct calculation of squares of differences 1
Correct calculation of sum of squares of differences 1
Correct calculation of standard deviation 4
Total 9
Q5 Correct statement of volume (incl. unit) 1
Correct use of sig. figs. 1
Total 2
Q6 Correct reason for including the stopper of the weighing bottle 1
Total 1
Conclusion Mention of each of the aims (three @ ⅔ ea) 2
Reasonable spelling & sentence construction 2
Total 4
Grand Total 40

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 Name and Student ID
Student: ____________________________________
RCS1601 Chemistry 1A Partner: ____________________________________

EXPERIMENT 2
Use of Laboratory Balances, Calibration of a Pipette and Error Estimation
LABORATORY REPORT

Aim

Aim/s clearly identified and stated. ___/3

Method
As per laboratory manual
Changes:

Results and Calculations

Q1 Table 1

Dimensions/mm
Metal (" × % × ℎ) Volume/mm3 Volume/mL Mass/g

1. _______ __________________ _________ _________ _________

2. _______ __________________ _________ _________ _________

Correct calculation of densities with correct units and significant figures. ___ /10

Q2

Correct interpolation of data, correct sig. figs. and complete answer to question. ___ /6

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 RCS1601 Chemistry 1A – Experiment 2, cont’d.

Q3 Table 2

Run # Mass (bottle+H2O)/g Mass (bottle)/g Mass (H2O)/g Volume (H2O)/mL

1. ___________ ___________ ___________ ___________
2. ___________ ___________ ___________ ___________
3. ___________ ___________ ___________ ___________

Correct calculation of volume including manipulation of units and sig. figs. ___ /5

Q4 Table 3

Volume (H2O)/mL
Run # (̅ − (! ((̅ − (! )"
(!
___________ ___________ ___________
___________ ___________ ___________
___________ ___________ ___________
Σ = __________ (̅ = __________ Σ = __________

Correct calculation of volume including manipulation of units and sig. figs. ___ /9

Q5

Correct statement of volume including sig. figs. ___ /2

Q6

Correct answer. ___ /1

Conclusions

Succinct and accurate conclusions ___ /4