CHY 46.

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Experiment 1: Calibration of 50-mL Buret and 10-mL pipet
Objectives:

At the end of the activity, students should:

1. Learn the proper techniques in calibrating volumetric glassware.
2. Learn the importance of accurate volume readings in analysis.
3. Understand the effect of temperature and buoyancy in weighing.
4. Apply the rules of retaining significant figures in calculations.
5. Properly apply the calibration information of volumetric glassware in reporting volume measurements.

Introduction

Many experiments in this laboratory class involve volumetric measurements and titrations. In order to achieve the best
possible results on those experiments, you need to be confident in the accuracy of your volumetric glassware. Calibration
of volumetric glassware provides information on the actual volumes delivered by the glassware and thus avoiding
volume errors in analysis. Calibration involves the weighing of water delivered by the volumetric glassware (pipet or
buret). Since the density, ρ, of water is known accurately at certain temperatures, we can calculate for the actual volume
delivered;

𝑉 = Eq. 1
Density of objects being weighed affects the mass reported/displayed by the balances especially if the density of the
objects were relatively different from the standard brass weights used to calibrate the balances. This is called the
Buoyancy error and can be corrected using Equation 2. In calibrating volumetric glassware, corrected mass of water,
should be calculated using Equation 2, in order to calculate the true volume delivered by the buret or pipet.

𝑀 =𝑀 + 𝑀 − Eq. 2

Where; MT= corrected or true mass of the water

Md= uncorrected mass of water
ρair= density of air @ a particular temperature, g/cm3
ρH2O= density of water @ a particular temperature, g/cm3
ρweights= density of standard brass weights @ a particular temperature, g/cm 3

The calculated MT can then be substituted to Equation 1 to compute for the corresponding volume of water.

Procedure

A. Cleaning of Buret and Pipet

A brief soaking in a warm detergent solution is usually sufficient to remove the grease and dirt responsible for water
breaks. Prolonged soaking should be avoided because a rough area or ring is likely to develop at a detergent/air
interface. This ring cannot be removed and causes a film break that destroys the usefulness of the equipment. After
being cleaned, the apparatus must be thoroughly rinsed with tap water and then with three or four portions of distilled
water. It is seldom necessary to dry volumetric ware.

B. Room Temperature Monitoring

As the calibration progresses, monitor the room temperature using a digital or alcohol thermometer. Make sure
to acclimatize the thermometer in the room for 10 minutes before recording. Consult online databases for the
corresponding density of water at a particular temperature.

C. Calibrating a 50-mL Buret

Many experiments in this laboratory class involve volumetric measurements and titrations. To achieve the best
possible results on those experiments, you need to be confident in the accuracy of your buret. In this experiment, you
will calibrate your buret so that you may correct its measured volumes in subsequent experiments.

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1. Choose a buret and note any markings so that you will be able to use the same for future experiments (or label your
buret). Wash the buret. Rinse the buret with tap water and then distilled water. Check the buret for possible leaks.
Refer to part A.

2. Fill the buret, slightly above the zero mark, with distilled water. Force any air bubbles out the tip by leaning the buret
to nearly horizontal with the stopcock open. Once the air bubbles are removed, mount the buret on the iron stand
using a buret holder. Set the initial volume of the buret to 0.00 mL, by slowly opening the stopcock to dispense the
excess water. Touch the buret tip to the inside wall of the beaker to remove any suspended drop of water.

3. Allow the buret to stand for 5 min while you weigh the clean, dry 125-mL Erlenmeyer flask fitted with a rubber stopper
in an analytical balance. While weighing, avoid holding the flasks with bare hands. Record the mass as initial mass
(Mi) in your notebook. Record the buret initial volume reading (Vi). Note: Read the volume with your eye level with
the meniscus. Read from the bottom of the meniscus and remember that the buret reads downward (0.00 mL mark
is on top while the 50.00 ml mark is at the bottom). Record the correct number of significant digits (the final
significant digit is the first one that you “approximate” on the buret). Refer to Figure 1 for proper volume readings in
burets.

(a) (b)

Figure 1. Guide on how to properly read volumes on a buret. (a) The meniscus lies between 12.20
and 12.30 mL. (b) Try to read the volume at position 2 or 3, just be consistent all throughout the
experiment. In this case, the volume reading should be 12.23 mL if read at position 2.

4. Slowly drain approximately 10 mL of water into the weighed flask. If a drop remains on the buret tip, transfer it to
the flask by touching the tip to the inside wall of the flask. Cap the flask with the same stopper to prevent
evaporation. Allow 30 s for the film of liquid on the walls to descend before you read the final volume (Vf) on the
buret. Weigh the stoppered flask again to determine its final mass (Mf). Record the Vf and Mf to the row
corresponding to 10.00 ml volume.

5. To the same flask, dispense another ≈ 10 mL from the buret, noting the same precautions in step 4. Cap the flask
with the same stopper and weigh. On the table, record the mass (Mf) and Vf corresponding to the 20.00 ml volume
increment. Continue dispensing approximately 10 mL of water to the same flask, with weighing, and recording of
masses and volume for each volume increment, until a total of around 50.00 mL of water has been delivered. Note:
DO NOT go below the 50 mL mark on the buret. Your last measurement may be 49.50 mL or less.

6. Refill the buret with water and repeat Steps 3-5 using another dry flask and stopper. Perform three (3) trials.

C. Calibration of 10-mL Pipet

1. Clean the 10-ml pipet and wash thoroughly with tap water, then lastly with distilled water.

2. Weigh a clean and dry 50-mL erlenmeyer flask with stopper. Record the mass on Table 1C.

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 3. Using an aspirator, fill the pipet up above the 0-mark. Slowly dispense the excess water into a waste container
until the lower the meniscus is within the zero mark.

4. Dispense the water from the pipet unto the pre-weighed 50- mL Erlenmeyer flask. Cover the flask with stopper
and weigh the flask again in an analytical balance. Record the mass.

5. Perform three trials for this calibration.

Calculations

1. Complete the first six columns in your data Table 1-A. To calculate Vd or Md, the volume reading (Vf) and mass (Mf)
for a particular volume increment (V), must be subtracted with the volume and mass reading directly above it. You
can use Excel to tabulate and easily compute the needed data.

Note: Calculated Vd or Md should be near the 10.00 mL and 10.0000 g values, respectively.

2. Determine the true mass (MT) of your dispensed water by adjusting the delivered mass (Md) to account for the
buoyancy of water in the air using Equation 2.

10. Calculate the true volume (VT) of water delivered by your buret for each volume increment by dividing MT by the
density of water. Refer to Equation 1.

11. Calculate the Correction Factor (CF) for each true volume as follows:
CF=VT −Vd Eq. 3
12. You can calculate Cumulative Correction Factor (CCF) for the corresponding volume increment, V, by adding up
mean CF values as you go down the summarized correction factor table (Refer to Table 1-B). Note: The final CCF
must be within the tolerance value of your buret. If NOT, the calibration must be repeated or replace your buret.

13. Prepare a plot (in Excel) of V (X-axis) versus the CCF (Y axis). Have Excel connect the points with straight line
segments. Be sure that the axes are properly labeled and units are included. Set your plot/graph to have grid lines.
When you perform titrations in subsequent experiments, you can use this plot to calculate true volumes delivered
by the same buret you calibrated. See example below.

Figure 2. Sample calibration plot.

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Sample applications of the Calibration Plot in Figure 2:

Initial volume : 0.01 mL Initial volume : 18.00 mL

Final volume : 18.00 mL Final volume : 30.00 mL
Apparent volume :18.00 -0.01= 18.99 mL Apparent :30.00-18.00= 12.00 mL
Example delivered Example volume
1 2 delivered
True volume :18.99+( +0.01) =18.00 True volume :12.00+(-0.008)- (0.01)
delivered mL delivered =11.98 mL
Alternative : 18.00 + (+0.01)- Alternative :30.00 +(-.008)-
Calculation [0.01]= 18.00 mL Calculation [18.00+(+0.01)=11.98 mL

Initial volume : 30.00 mL

Final volume : 45.00 mL
Apparent :45.00-30.00= 15.00mL
Example volume
3 delivered
True volume :15.00+(+0.01)- (-0.0058) =
delivered 15.02 mL
Alternative 45.00+ (0.01)-[30.00+
Calculation (0.008) = 15.02 mL

14. For the pipet calibration, calculate the corrected mass using equation 2, then compute for the correction factor.
Video links:

http://youtube.com/watch?v=0NmbYqERfoo
http://youtube.com/watch?v=xOGQsZul4P0

References:

Hamilton, L. et al. Quantitative Chemical Analysis, 12th edition. 1971.

Skoog, et.al (2014). Fundamentals of Analytical Chemistry. 9th ed. USA: Brooks/Cole- Cengage Learning
McLaren, R. Chem 2080 Course Notes. York Univeristy.
http://www.yorku.ca/rmclaren/CHEM2080/2080%20notes_B&W.pdf. Date accesed: 26 January 2024.

Prepared by:

Armenia C. Opog
CHY 46.1 Instructor

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 CHY 46.1
Experiment 1: Calibration of 50-mL Buret and 10-mL pipet
A. Supplementary Data
Temperature of water:_____________ oC
Density of brass weights: __________
Density of water at ____ oC :__________

B. Calibration of 50-mL buret

Buret Brand:__________ Class:__________ Tolerance:___mL

Table 1-A. Raw data for the calibration of 50- mL buret.

Volume Buret Apparent Mass of flask + Mass of H2O True Mass True Correction
Trial Increment Reading, Volume, H2O, g (Mf) (Md), g of H2O Volume Factor
(V) mL (Vf) mL (Vd) (MT), g (VT), mL (CF), mL
(Vi): *(Mi): 0.00
0.00 ------- --- --- ---

10.00

20.00
1
30.00

40.00

50.00

(Vi): *(Mi):
0.00 ------ ---- ---- ---- 0.00

10.00

20.00
2
30.00

40.00

50.00

(Vi): *(Mi):
0.00 ------ ---- ---- ---- 0.00

10.00

20.00
3
30.00

40.00

50.00

* Mass of flask and stopper only

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Table 1-B. Summary of Buret Correction Factor
Volume Correction Factor (CF),
Increment mL Cumulative CF, mL
(V) Trial 1 Trial 2 Trial 3 Mean s
0.00 0.00 0.00 0.00 0.00

10.00

20.00

30.00

40.00

50.00

Interpretation of data:

a. Review the CF for each increment and CCF. Is the buret fit for use in analytical work? Should the calibration be
repeated? Explain

C. Graph

Prepare a plot (in Excel) of V (axis) versus the Cumulative Correction Factor (Y axis) from Table 1-B.

D. Calibration of 10-mL pipet

Pipet Brand:______ Tolerance:_______mL

Table 1 -C. Raw data for the calibration of 10- mL pipet.

Mass of Mass of flask
Apparent Mass of water True Correction
empty flask (with True mass of
Trial Volume (Vd), delivered volume factor (CF),
and stopper, stopper)+ water, g (MT)
mL (Md), g (VT), mL mL
g water, g
1

Mean

a. Based on the data, is the pipet fit for use in analytical work? Should the calibration be repeated. Explain.

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