Physical Chem 1 (Combined)
Physical Chem 1 (Combined)
Physical Chem 1 (Combined)
DEPARTMENT OF CHEMISTRY
STK 1201- PRACTICAL PHYSICAL CHEMISTRY 1
DATE OF EXPERIMENT
LAB FACILITATOR
INTRODUCTION
The definition of volumetric calibration is the process of correcting or setting the
volumetric glassware. Generally, the volumetric glassware will be calibrated first before
commercialize in order to ensure that they produce accurate and precise readings. Unfortunately,
it is never safe to assume that the volume given by the volumetric glassware indicate the exact
value at calibration mark. (Volumetric Glass Calibration, 2009)
Besides, any of the glass containers which have the ability to measure volume accurately
can be considered as volumetric glassware. In this experiment, the volumetric glassware that we
use are volumetric flask, pipette and burette for the purpose of calibration. The volumetric
glassware is usually made to specification limits, particularly with regards to the accuracy of
calibration. We are required to calibrate the volumetric glassware that we used in this experiment
to ensure that they are accurate and within its specified tolerance. With the used of distilled water
and an accurate balance, the calibration of laboratory glassware can be carried out. Based on
Table 1.1, the density of water can be identified after the temperature of distilled water is
measured. Consequently, the volume contained in or delivered by a piece of glassware may be
accurately determined using equation as shown below:
=
m
V
Volumetric flask has a long neck with a fill line on the neck for accurate measure. A
volumetric flask is glassware used in laboratories for measuring volume in the preparation of
solution. It is calibrated to contain an exact volume of solution when the solution level is exactly
at the mark on the neck of flask. Bear in mind that the bottom of the meniscus should lie exactly
on the calibration mark.
Furthermore, pipette is a type of chemical dropper used in laboratory experiment to
measure and transport fixed volume of solution from one container to another. There are several
designs of pipettes which are performing the same function. Volumetric pipette is more accurate
as compared to Mohr pipette (graduated pipette). This is due to volumetric pipette has only one
calibration mark while Mohr pipette has graduated marks throughout the length of the pipette.
2
One of the easiest ways to calibrate pipette is initially overshoot the mark and then let the liquid
drain from the pipette until the bottom of the meniscus lies exactly on the calibration mark.
Lastly, burette is a narrow, hollow and cylindrical tube labelled with graduation marks and
equipped with a regulating device for a purpose to control the flow of liquid from the tip
(Macaulay, Bauer and Bloomfield, 2011). Burette is used to delivered volumes of liquid that
cannot be measured by volumetric pipette or micropipettors accurately. Before dispensing liquid,
we should top the sides of the tip to get rid of the air bubbles because the presence of air bubbles
might cause the reading to be inaccurate. The proper use of burette is essential for accurate
titration analysis.
OBJECTIVE
1.
To determine the accuracy and precision of some commonly used volumetric glassware
namely volumetric pipette, burette and volumetric flask.
2.
To deepen our understanding on the importance of accuracy and precision to measure
specific volumes of solution.
3.
Reagents
Distilled water
Apparatus
Volumetric pipette
Burette
Beaker
Volumetric flask.
PROCEDURES
The water temperature to the nearest C is recorded using the thermometer. The density of water
at various temperatures is summarized on the table 1.1.
Table 1.1 Density of water at various temperatures
Temperature (C)
20
21
22
23
24
25
26
27
28
29
30
A. Pipette calibration
Density (g/mL)
0.998203
0.997992
0.997770
0.997538
0.997296
0.997044
0.996783
0.996512
0.996232
0.995944
0.995646
RESULTS
A. Pipette
Water temperature, t (C)
Mass of empty beaker (g)
Mass of beaker with distilled water (g)
Apparent mass of water transferred (g)
True mass of water transferred (g)
Apparent mass refers to the measurement
under vacuum condition. The density of
air is 0.0012 g/mL. Therefore, the mass
of air displaced in the water transferred is
0.0012 times the volume of water
transferred. The calculated mass of air
displaced has to be added to the apparent
mass to give true mass of water.
Density of water at t C (g/mL)
Actual volume of water transferred (mL)
Average volume of water transferred
(mL) standard deviation
Trial 1
28
96.4863
116.2939
19.8076
19.8314
Trial 2
28
96.4860
116.3392
19.8532
19.8770
Trial 3
28
96.4857
116.3434
19.8577
19.8815
0.996232
19.9064
0.996232
19.9522
19.93840.02783
0.996232
19.9567
B. Burette Calibration
5 mL
Water temperature, t (C)
Initial reading of burette (to 0.01 mL)
Final reading of burette (to 0.01 mL)
Nominal volume of water transferred (mL)
Mass of empty Erlenmeyer flask (g)
Mass of Erlenmeyer flask with water (g)
Apparent mass of water (g)
True mass of water (g)
Density of water at t C (g/mL)
Actual volume of water transferred (mL)
Correction of nominal (labeled) volume (mL)
Average volume of water transferred (mL)
standard deviation
Trial 1
28
0.00
5.00
5.00
50.3800
55.3564
4.9764
4.9824
0.996232
5.0012
0.0012
Trial 2
28
5.00
10.00
5.00
50.3808
55.4445
5.0637
5.0698
0.996232
5.0890
0.0890
5.17310.2260
Trial 3
28
10.00
15.10
5.10
50.3810
55.7831
5.4021
5.4086
0.996232
5.4291
0.3291
10 mL
Water temperature, t (C)
Initial reading of burette (to 0.01 mL)
Final reading of burette (to 0.01 mL)
Nominal volume of water transferred (mL)
Mass of empty Erlenmeyer flask (g)
Mass of Erlenmeyer flask with water (g)
Apparent mass of water (g)
True mass of water (g)
Density of water at t C (g/mL)
Actual volume of water transferred (mL)
Correction of nominal (labeled) volume (mL)
Average volume of water transferred (mL)
standard deviation
Trial 1
28
15.10
25.20
10.10
50.3804
60.6227
10.2423
10.2546
0.996232
10.2934
0.1934
Trial 2
28
25.20
35.20
10.00
50.3803
60.3620
9.9817
9.9937
0.996232
10.0315
0.0315
10.15350.1319
Trial 3
28
35.20
45.20
10.00
50.3809
60.4662
10.0853
10.0974
0.996232
10.1356
0.1356
15 mL
Water temperature, t (C)
Initial reading of burette (to 0.01 mL)
Final reading of burette (to 0.01 mL)
Nominal volume of water transferred (mL)
Mass of empty Erlenmeyer flask (g)
Mass of Erlenmeyer flask with water (g)
Apparent mass of water (g)
True mass of water (g)
Density of water at t C (g/mL)
Actual volume of water transferred (mL)
Correction of nominal (labeled) volume (mL)
Average volume of water transferred (mL)
standard deviation
Trial 1
28
0.00
15.00
15.00
50.3809
65.4130
15.0321
15.0501
0.996232
15.1070
0.1070
Trial 2
28
15.00
30.00
15.00
50.3808
65.3230
14.9422
14.9601
0.996232
15.0167
0.0167
15.10420.08608
Trial 3
28
30.00
45.00
15.00
50.3804
65.4939
15.1135
15.1316
0.996232
15.1888
0.1888
20 mL
Water temperature, t (C)
Initial reading of burette (to 0.01 mL)
Final reading of burette (to 0.01 mL)
Nominal volume of water transferred (mL)
Mass of empty Erlenmeyer flask (g)
Mass of Erlenmeyer flask with water (g)
Apparent mass of water (g)
True mass of water (g)
Density of water at t C (g/mL)
Actual volume of water transferred (mL)
Correction of nominal (labeled) volume (mL)
Average volume of water transferred (mL)
standard deviation
Trial 1
28
0.00
20.00
20.00
50.3804
70.5177
20.1373
20.1615
0.996232
20.2378
0.2378
Trial 2
28
20.00
40.00
20.00
50.3803
70.3230
19.9427
19.9666
0.996232
20.0421
0.0421
20.22540.1774
Trial 3
28
10.00
30.00
20.00
50.3805
70.6755
20.2950
20.3194
0.996232
20.3963
0.3963
25 mL
Water temperature, t (C)
Initial reading of burette (to 0.01 mL)
Final reading of burette (to 0.01 mL)
Nominal volume of water transferred (mL)
Mass of empty Erlenmeyer flask (g)
Mass of Erlenmeyer flask with water (g)
Apparent mass of water (g)
True mass of water (g)
Density of water at t C (g/mL)
Actual volume of water transferred (mL)
Correction of nominal (labeled) volume (mL)
Average volume of water transferred (mL)
standard deviation
Trial 1
28
0.00
25.00
25.00
50.3795
75.4403
25.0608
25.0909
0.996232
25.1858
0.1858
Trial 2
28
25.00
50.00
25.00
50.3796
75.5139
25.1343
25.1645
0.996232
25.2597
0.2597
25.23430.04205
Trial 3
28
25.00
50.00
25.00
50.3795
75.5116
25.1321
25.1623
0.996232
25.2575
0.2575
Trial 1
28.0
59.8533
158.9380
Trial 2
28.0
59.8534
159.0762
Trial 3
28.0
59.8532
159.1699
99.0847
99.2036
0.996232
99.5788
99.2228
99.3419
0.996232
99.7176
99.70280.1173
99.3167
99.4359
0.996232
99.8120
10
CALCULATION
Apparent mass of water transfer (g) = Mass of beaker with distilled water (g) - mass of empty
beaker (g)
True mass of water transfer (g) = (0.0012 apparent mass of water)+ Apparent mass of water
transferred
=
m
v
V=
m
p
mL
g/
Density of water at 28 C
True mass of water transfer(g)
Standard deviation
Trial 1
116.2939-96.4863
= 19.8076
Trial 2
116.3392-96.4860
=19.8532
Trial 3
116.3434-96.4857
=19.8577
(0.001219.8076)
+ 19.8076
= 19.8314
(0.001219.8532)
+ 19.8532
= 19.8770
(0.001219.8577)
+ 19.8577
= 19.8815
19.8314
0.996232
19.8770
0.996232
= 19.9064
= 19.9522
19.8815
0.996232
=19.9567
mL
g/
Density of water at 28 C
True mass of water transfer( g)
Standard deviation, s
x=
(19.9064+19.9522+19.9567)
3
= 19.9384
s2= (19.9064-19.9384)2+ (19.9522-19.9384)2+(19.956719.9384)2/ 3-1
=7.7466510-4
s= 7.74665 104
= 0.02783
Average volume of water
transferred (mL) standard
deviation
19.93840.02783
12
B) Burette Calibration
5mL
Nominal volume of water
transferred (mL)
Trial 1
5.00-0.00
= 5.00
Trial 2
10.00-5.00
= 5.00
Trial 3
15.10-10.00
=5.10
55.3564-50.3800
= 4.9764
55.4445-50.3808
= 5.0637
55.7831-50.3810
= 5.4021
4.9824
0.996232
5.0698
0.996232
5.4086
0.996232
= 5.0012
= 5.0890
= 5.4291
5.0012-5.00
= 0.0012
5.0890-5.00
= 0.0890
5.4291-5.00
=0.4291
mL
g/
Density of water at 28 C
True mass of water transfer( g)
13
Standard deviation, s
x=
(5.0012+5.0890+5.4291)
3
= 5.1731
s2= (5.0012-5.1731)2+ (5.0890-5.1731)2+(5.42915.1731)2/ 3-1
=0.05107
s= 0.05107
= 0.2260
Average volume of water
transferred (mL) standard
deviation
10mL
Nominal volume of water
transferred (mL)
5.17310.2260
Trial 1
25.20-15.10
=10.10
Trial 2
35.20-25.20
=10.00
Trial 3
45.20-35.20
=10.00
60.6227-50.3804
=10.2423
60.3620-50.3803
=9.9817
60.4662-50.3809
=10.0853
(0.001210.2423)
+ 10.2423
=10.2546
(0.001210.2423)
+ 10.2423
=9.9937
(0.001210.2423)
+ 10.2423
=10.0974
10.2546
0.996232
=10.2934
9.9937
0.996232
=10.0315
14
10.0974
0.996232
=10.1356
mL
g/
Density of water at 28 C
True mass of water transfer( g)
10.2934-10.10
=0.1934
x=
10.0315-10.00
=0.0315
10.1356-10.00
=0.1356
(10.2934+10.0315+10.1356)
3
= 10.1535
s2= (10.2934-10.1535)2+ (10.0315-10.1535)2+(10.135610.1535)2/ 3-1
=0.01739
s= 0.01739
= 0.1319
Average volume of water
transferred (mL) standard
deviation
15mL
Nominal volume of water
transferred (mL)
10.15350.1319
Trial 1
15.00-0.00
=15.00
Trial 2
30.00-15.00
=15.00
Trial 3
45.00-30.00
=15.00
65.4130-50.3809
= 15.0321
65.3230-50.3808
=14.9422
65.4939-50.3804
=15.1135
(0.001215.0321)
+ 15.0321
=15.0501
(0.001214.9422)
+ 14.9422
=14.9601
(0.001215.1135)+
15.1135
=15.1316
14.9601
0.996232
15.1316
0.996232
=15.1070
=15.0167
=15.1888
15.1070-15.00
= 0.1070
15.0167-15.00
= 0.0167
15.1888-15.00
= 0.1888
mL
g/
Density of water at 28 C
True mass of water transfer( g)
x=
(15.1070+15.0167+15.1888)
3
= 15.1042
s2= (15.1070-15.1042)2+ (15.0167-15.1042)2+(15.188815.1042)2/ 3-1
=7.410610-3
s= 7.4106 103
= 0.08608
Average volume of water
transferred (mL) standard
deviation
20mL
15.10420.08608
Trial 1
16
Trial 2
Trial 3
20.00-0.00
=20.00
40.00-20.00
=20.00
30.00-10.00
=20.00
70.5177-50.3804
=20.1373
70.3230-50.3803
=19.9427
70.6755-50.3805
=20.2950
(0.001220.1373)
+ 20.1373
=20.1615
(0.001220.1373)
+ 20.1373
=19.9666
(0.001220.1373)
+ 20.1373
=20.3194
19.9666
0.996232
20.3194
0.996232
=20.2378
=20.0421
=20.3963
20.2378-20.00
=0.2378
20.0421-20.00
=0.0421
20.3963-20.00
=0.3963
mL
g/
Density of water at 28 C
True mass of water transfer( g)
x=
(20.2378+20.0421+20.3963)
3
17
= 20.2254
s2= (20.2378-20.2254)2+ (20.0421-20.2254)2+(20.396320.2254)2/ 3-1
=0.03148
s= 0.03148
= 0.1774
Average volume of water
transferred (mL) standard
deviation
25mL
Nominal volume of water
transferred (mL)
20.22540.1774
Trial 1
25.00-0.00
=25.00
Trial 2
50.00-25.00
=25.00
Trial 3
50.00-25.00
=25.00
75.4403-50.3795
=25.0608
75.5139-50.3796
=25.1343
75.5116-50.3795
=25.1321
(0.001225.0608)
+ 25.0608
=25.0909
(0.001225.0608)
+ 25.0608
=25.1645
(0.001225.0608)
+ 25.0608
=25.1623
25.0909
0.996232
=25.1858
25.1645
0.996232
=25.2597
18
25.1623
0.996232
=25.2575
mL
g/
Density of water at 28 C
True mass of water transfer( g)
25.1858-25.00
=0.1858
x=
25.2597-25.00
=0.2597
25.2575-25.00
=0.2575
(25.1858+25.2597+25.2575)
3
= 25.2343
s2= (25.1858-25.2343)2+ (25.2597-25.2343)2+(25.257525.2343)2/ 3-1
=1.767810-3
s= 1.7678 103
= 0.02405
Average volume of water
transferred (mL) standard
deviation
25.23430.04205
19
Trial 1
158.9380-59.8533
=99.0847
Trial 2
159.0762-59.8534
=99.2228
Trial 3
159.1699-59.8532
=99.3167
(0.001299.0847)
+ 99.0847
=99.2036
(0.001299.0847)
+ 99.0847
=99.3419
(0.001299.0847)
+ 99.0847
=99.4359
99.2036
0.996232
= 99.5788
99.3419
0.996232
= 99.7176
99.4359
0.996232
=99.8120
mL
g/
Density of water at 28 C
True mass of water transfer( g)
Standard deviation,s
x=
(99.5788+99.7176+ 99.8120)
3
= 99.7028
s2= (99.5788-99.7028)2+ (99.7176-99.7028)2+(99.812099.7028)2/ 3-1
=0.01376
s= 0.01376
= 0.1173
20
99.70280.1173
DISCUSSION
We are required to calibrate volumetric glassware namely volumetric pipette, burette and
volumetric flask in this experiment. Distilled water is the only reagent needed in conducting this
glassware calibration experiment.
First and foremost, the experiment is started with the calibration of volumetric pipette. A
small empty and dried beaker is placed on the analytical balanced and the balanced is tared to
ensure the readings obtained are accurate. The weight of the empty beaker is identified. This step
is very crucial as we have to calculate the apparent mass of distilled water drained into the empty
beaker from the pipette.
The mass of empty beaker is actually equivalent to the pure mass of beaker with the mass of air
inside the beaker. This is because when we are weighing the mass of beaker, there is also air
inside the beaker. As we are not weighing the empty beaker under vacuum condition, the beaker
must be filled with air.
Therefore, the apparent mass of water transferred can also be expressed in this way:
Apparent mass of water transferred (g) = Mass of water in the beaker (g) Mass
of air displaced (g)
21
The true mass of water transferred (g) could be determined from the apparent mass of water
transferred (g). The apparent mass of water transferred does not include the mass of air
displaced, however the true mass of water is the total of the apparent mass of water transferred
with the mass of air displaced. Therefore, the mass of air displaced must be determined. Given
density of air is 0.0012 g/mL, which means that the mass of air displaced is 0.0012 times of the
volume of water transferred into the beaker.
True mass of water transferred (g) = [0.0012 x apparent mass of water
transferred (g)] + apparent
mass of water transferred (g)
The density
of water is
varies with the temperature. Therefore, the temperature of water is observed in order to
determine the density of water. The temperature of water throughout this experiment is 28.0C.
Thus, the density of water is 0.996232 g/mL.
As
Density (g/mL) =
Mass( g)
Volume (mL)
From the equation above, the actual volume of water transferred could be calculated.
Rearranging the formula, the actual volume of water transferred can be obtained as below:
Actual volume of water transferred (mL) =
T 1+ T 2+T 3
=(
3
x x
The average volume of water transferred from the pipette is 19.9384 0.02783 mL.
In the calibration of burette, burettes of 5mL, 10mL, 15 mL, 20mL, and 25mL are calibrated.
First and foremost, the temperature of water is recorded in order to determine the density of
water. Temperature recorded is 28C , and the density of water at this temperature is 0.996232
g/mL. Erlenmeyer flask is weighed before 5mL of distilled water is drained into it. The
Erlenmeyer flask is weighed again and the apparent mass of water could be calculated using the
formula:
Apparent
in the Erlenmeyer
flask
Apparentmass
massof
ofwater
watertransferred
transferred(g)
(g)==Mass
Massof
ofwater
Erlenmeyer
flask with distilled
(g) Mass of air displaced
(g)
water (g) Mass of empty Erlenmeyer flask (g)
From the apparent mass of water transferred, true mass of water could be calculated using the
formula:
The actual volume of water transferred could also be calculated from the formula:
True mass of water transferred (g) = [0.0012 x apparent mass of water
transferred (g)] + apparent
mass of water transferred (g)
Nominal volume of water transferred is the difference of final reading of burette and the initial
True mass of water transferred (g)
g
Actual volume Correction
of water transferred
= (mL)
Density
of water
at 28of( water
) transferred (mL)
of nominal(mL)
volume
= Actual
volume
mL
reading
of
burette.
Formula to
calculate the
correction of
nominal
volume is as
follow:
23
In order to get accurate result of the calibration of burette, the average volume of water
transferred standard deviation must be calculated. The formula is:
=(
T 1+ T 2+T 3
)
3
x x
The same steps are repeated for calibration of burette of 10mL, 15mL, 20mL, and 25mL .
For the calibration of volumetric flask, the water temperature is recorded to determine the
density. The temperature of water is 28C and the density is 0.996232 g/mL . The volumetric
flask with stopper is weighed before water is added to the mark. The volumetric flask is weighed
again. Apparent mass of water is calculated using the formula:
Apparent mass of water transferred (g) = Mass of volumetric flask with distilled
water (g) Mass of empty volumetric flask (g)
Therefore, the true mass of water can be calculated using the formula:
24
In order to get accurate result of the calibration of volumetric flask, the average volume of water
transferred standard deviation must be calculated. The formula is:
=(
T 1+ T 2+T 3
3
x x
Throughout the experiment, there might be some factors which may affect the accuracy
of results. Parallax error may occurred when taking the reading on the burette and observing the
water level in the pipette and volumetric flask. To avoid the parallax error, the eyes must be
perpendicular to the scale on the volumetric glassware when taking the reading. Other than that,
the volumetric glassware might not be fully dried during weighing. This might causes the mass
of empty volumetric glassware to be inaccurate as there are some water droplets inside the
glassware. Furthermore, the burette is left for 5 minutes to make sure the volume of distilled
water inside remains constant. If not, the stopcock must be tighten and the procedure is repeated.
When weighing the mass of volumetric glassware using analytical balance, the enclosure of
balance must be close immediately to ensure accurate mass is obtained. Make sure the stopper of
volumetric flask is weighed together with it.
25
CONCLUSION
Throughout this experiment, the pipette, burette and volumetric flask are considered
accurate and precise. The pipette had a mean of 19.9384 and a standard deviation of 0.02783.
While for the burette, we had transferred 5mL, 10mL, 15mL, 20mL and 25mL distilled water
26
from the burette to the Erlenmeyer flask. The average volume and standard deviation are
5.17310.2260, 10.15350.1319, 15.10420.08608, 20.22540.1774 and 25.23430.04205
respectively. For the volumetric flask, it had a mean of 99.7028 and a standard deviation of
0.1173.
POST-LAB QUESTION
1. Pipettes are used to transfer liquid sample and they are rinsed with a small amount
of the sample after transfer. Calculate the % error that will be produced with
27
pipette of 1 mL, 5 mL and 10 mL if each pipette retains 5 drops of water after use.
Assuming the volume of one drop of water is 0.05 mL.
Volume of water retains in the pipette = 0.05mL 5
= 0.25mL
Therefore, the will be always less than 0.25mL of water not be transferred for every used.
% error =
Experimental value: Theoretical value - Volume of water retains in the pipette (0.25mL)
Volume of Pipette used (mL)
% error=
Experimental valuetheoretical value
100
Theoretical value
%
( 10.25 )1
100
1
= -25%
( 50.25 ) 5
100
5
= -5%
10
( 100.25 ) 10
100
10
28
= -2.5%
2. It is important to ensure that no air bubbles are captured at the stopcock of the
burette when the initial reading is recorded. If 0.5 mL of air bubbles is present in the
burette, what is the % error that will be generated in 10 mL, 20mL and 40 mL of
sample when the air bubbles are released?
When there is 0.5mL air bubble present in the burette, the actual volume titrated will be
always 0.5mL less than the theoretical volume
Experimental valuetheoretical value
100
% error =
Theoretical value
Experimental value: Theoretical value - Volume of air bubbles (0.5mL)
Volume of sample (mL)
% error=
Experimental valuetheoretical value
100
Theoretical value
%
10
( 100.5 ) 10
100
10
= -5%
20
( 200.5 ) 20
100
20
= -2.5%
40
( 400.5 )40
100
40
= -1.25%
29
REFERENCE
Macaulay, D. B., Bauer, J. M., & Bloomfield, M. M. (2011). General, organic, and
biological chemistry: An integrated approach (2nd ed.). New York, NY: John Wiley &
Sons, Inc.
30
APPENDIX
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