NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab EXPERIMENT: Calibration of Volumetric Glassware

DATE LAB WAS CONDUCTED: 28th January 2013

INTRODUCTION The objective of this lab is to produce data for future experiments that is as precise and accurate as possible by way of calibrating volumetric glassware. Calibration is an important method that introduces students to their glassware, ensuring that the glassware work effectively thereby reducing the risk of error in measurements. Specifically in this lab, students were required to calibrate 3 different types of volumetric glassware, namely, 100mL volumetric flask, 25mL transfer pipet and 50mL buret MATERIALS 1. 2. 3. 4. 5. 6. 7. 100mL volumetric flask (1) 25mL transfer pipet (1) 50mL buret (1) 125mL flask w/ stopper (1) analytical balance beaker(s) stand 8. buret clamps 9. wash bottle 10. parafilm 11. acetone for drying glassware 12. deionized/distilled water 13. thermometer

PROCEDURE I) Calibrating a 100mL volumetric flask a. All volumetric glassware used for calibration were cleaned, rinsed and dried before any further steps. The glassware were cleaned with soap and water and rinsed three or four times with distilled water. OPTIONAL: student used acetone and pressurized air available in the lab to help dry glassware. b. Analytical balance was calibrated and the measurements were recorded. c. The temperature of distilled water was recorded by filling up a beaker with it and leaving a thermometer in the beaker. d. Once the 100mL vol. flask was dried, it was marked to ensure that it will not get mixed up with other 100mL vol. flasks that were not calibrated. e. The empty flask was placed on analytical balance and the mass was recorded. f. The flask was then filled with distilled water to the 100mL point. A disposable micropipet was used to get the meniscus to the 100mL

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab point. Student ensured that the meniscus was at eye-level when reading the flask. g. The now filled flask was weighed and the mass was recorded. h. Steps d. through g. were repeated three more times, ensuring that the flask was dry each time before weighing it. II) Calibrating a 25mL transfer pipet a. The 125mL flask with stopper was weighed on the analytical balance. b. A cleaned 250mL beaker containing distilled water was prepared (the amount of distilled water in beaker was irrelevant). c. Using a bulb, 25mL of distilled water from the beaker was drawn into the pipet . TECHNIQUE: the water was drawn until it passed the 25mL point. The bulb was quickly replaced with a thumb to ensure that the water did not leave the pipet. The water slowly displaced from the pipet by moving the thumb slightly. d. Once 25mL of water was collected in the pipet, the water was transferred into the 125mL flask and capped using its stopped before weighing it. The mass of flask was recorded. e. The procedure was repeated three more times. III) Calibrating a 50mL buret (repeated lab on 2/5/2013) a. The buret was filled with distilled water and air bubbles were forced out of the tip. Student ensured that the buret drained out without leaving any drops on its walls. b. The meniscus was adjusted to be at or slightly below 0.00mL, and any suspended drop of water was removed by touching the tip of buret to a beaker. c. The buret was left to stand for 5 min to make sure that it was not leaking. d. While waiting on the buret, a 125mL flask with a stopper was weighed. e. The level of water in the buret was recorded again. f. 10mL of water was drained at a rate <20mL/min into the weighed flask and the flask was capped to prevent evaporation. g. The buret was left to stand again for 30secs to allow film of water to descend before the buret was read. Readings were estimated to the nearest 0.01mL. h. The flask was weighed again to determine the mass of water. i. The procedure was repeated for 20, 30, 40 and 50mL. The whole procedure was repeated twice.

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab RESULTS Room Temperature on 28th Jan: 22.9C Room Temperature on 2nd Feb: 24C Correction Factor: 1.0035mL/g Correction Factor 1.0038mL/g * Trial 1 exemplifies all calculations shown in this section

I. 100mL Volumetric Flask

i) ii) Tr ia l 1 2 3 4 iii) Tolerance of Class A 100mL volumetric flask: 0.08mL Data: TABLE A Mass of empty vol. flask (g) 59.66 59.7 59.67 59.64 Mass of filled vol. flask (g) 159.22 159.18 159.18 159.21 Apparent mass of water (g) 99.56 99.48 99.51 99.57 True vol. of water (mL) 99.91 99.83 99.86 99.92 True mass of 100mL water 99.65 99.57 99.60 99.66

Bar Graph 1.1: a comparison between the apparent mass to the true mass of the measured 100mL water using a volumetric flask Please refer to Appendix I for the bar graph Calculations for Trial 1, 2, 3, & 4: a. True vol. delivered: eg. Trial 1 Apparent mass of water: 159.22g - 59.66g = 99.56g True vol. of water: 99.56g x 1.0035mL/g = 99.91mL b. True mass of 100mL water delivered eg. Trial 1 True mass delivered = apparent mass x buoyancy equation = 99.56g x buoyancy equation* = 99.65g *Please refer to Appendix IV for buoyancy equation

iv)

v)

Average and Standard Deviation: Mean: 99.88mL Standard Deviation: 0.04mL

II. 25mL Transfer Pipet

i) ii) Tolerance of Class A transfer pipets: 0.03mL Data: TABLE B

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab T ri al 1 2 3 4 Mass of empty 125mL flask (g) 89.58 89.58 89.59 89.59 iii) Mass of filled 125mL flask (g) 114.42 114.44 114.46 114.44 Apparent mass of water (g) 24.84 24.86 24.87 24.85 True vol. of water (mL) 24.93 24.95 24.96 24.94 True mass of 100mL water 24.86 24.88 24.89 24.87

Bar Graph 1.2: a comparison between the apparent mass to the true mass of the measured 25mL water using a transfer pipet Please refer to Appendix I for the bar graph Calculations for Trial 1, 2, 3 & 4: Eg. Trial 1 Apparent mass of water: 114.42g 89.58g= 24.84g True vol. of water: 24.84g x 1.0035 mL/g = 24.93mL

iv)

v)

Average and Standard Deviation: Mean: 24.95mL Standard Deviation: 0.01mL

III. 50mL Buret Trial 1, 2, and 3

a) b) Tolerance of Class A 25mL buret = 0.03mL Calculations to find true vol. and mass delivered and buret correction for all three trials i) true vol. delivered eg. Trial 1 (Refer to Appendix II, shaded row in Tables 1.1) Buret Reading: 0.01mL-10.01mL Apparent mass of water = mass of filled flask mass of empty flask = 99.5231g - 89.5849g = 9.9382g True vol. delivered = apparent mass of water x correction factor @24C = 9.9382g x 1.0038mL/g = 9.9760mL ii) true mass delivered eg. Trial 1 True mass delivered = apparent mass x buoyancy equation = 9.9382g x buoyancy equation = 9.9469g

IV. Constructing a calibration curve

a) Data for constructing the calibration curve: TABLE C

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab

Buret correction (mL) Amount of water (mL) T1 T2 T3 0 0 0 0 -0.01 -0.05 10 -0.02 -0.02 -0.05 20 -0.03 -0.05 -0.05 -0.025 30 0.03 40 -0.06 -0.03 -0.04 -0.06 50 -0.02 Average Standard Deviation 0 0 -0.02667 0.020817 -0.03333 0.015275 -0.04167 0.014434 -0.02 0.045826 -0.04 0.02

b)

Calculation to find the buret correction eg. Trial 1 (shaded) Buret correction = true vol. delivered apparent vol. delivered = 9.9760mL (10.01mL - 0.01mL) = 9.9760mL 9.99mL = -0.01mL

Refer to Appendix II for the calibration curve

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab DISCUSSION This experiment, basically, allows student to understand the glassware that they will be working with for the rest of the semester. Calibrating volumetric glassware yields results that demonstrate the efficiency of the glassware to measure the amount needed by analytical chemists. In addition, students are taught to understand the theory of density and buoyancy when taking measurements and doing their calculations. This lab report discusses the concepts of glassware tolerance, buoyancy equation, the average and standard deviations for each calibration, and determining the true mass and true volume of water that was measured in the procedure. The average and standard deviations were calculated and were compared to the tolerances of each glassware provided in chapter 2 of Exploring Chemical Analysis 5th Ed. textbook by Daniel Harris. The tolerances are also provided in Appendix V of this lab report. The average and standard deviation for the calibration of the 100mL volumetric flask are 99.88mL and 0.04mL respectively, while the tolerance for this glassware is 0.08mL. This means that the 100mL volumetric flask works well within the tolerance that is set by the manufacturer. The same conclusion can be made for the 25mL transfer pipet as the average, 24.95mL, and standard deviation, 0.01mL, are within the tolerance that is set by the manufacturer, which is 0.03mL. As for the buret, its calibration had to be repeated to yield a better result and after the repetition, the burets corrections were well below the tolerance set by the manufacturer. A comparison between the apparent mass and the true mass of water that was measured using the 100mL volumetric flask and 25mL transfer pipet is depicted in the bar graphs provided in Appendix I. As evident in the graphs, the true masses of the water measured are higher towards 100mL and 25mL, than the apparent mass. This is due to the fact that the calculations to find the true masses incorporate density and buoyancy equation. These incorporations demonstrated that the density of anything is highly affected by its surroundings i.e. temperature, humidity, elevation and time of day the experiment was conducted. Thus, what was invisible to the students when measuring the masses of water was caught by the incorporations of these important factors. As for the calibration curve, students will be referring to this curve in their future experiments and know that they have to make corrections in their measurements. An example is when a student measured a volume of a solution as 20.05mL. By looking at the calibration curve (Appendix III) at point 20mL, the correction is about 0.03mL, so the student should subtract 0.03mL from the 20.05mL to get the true volume of the solution i.e. 20.02mL. At the same time, student must keep in mind of the temperature of the lab, as the density of the solution is highly dependent on that. Some of the limitations to this experiment were time management issue and knowing how to use the glassware effectively to yield a good result. Lack of skills could result in

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab APPENDIX I Bar Graph 1.1
Apparent Mass vs. True Mass of 100mL Water Using Volumetric Flask

Mass of 100mL water (g)

Apparent mass of 100mL water (g) True mass of 100mL water (g)

Trials

Bar Graph 1.2

Apparent Mass vs. True Mass of 25mL Water Using 25mL Transfer Pipet

Mass of 25mL water (g)

Apparent mass of 25mL water (g) True mass of 25mL water

Trials

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab APPENDIX II TABLES 1.1 Raw data for buret calibration
Trial 1 Buret Readin g (mL) 0.0110.01 10.0120.00 20.0029.98 29.9840.01 40.0149.99 Mass of empty 125mL flask (g) 89.5849 89.7056 89.8229 89.8051 89.7534 Mass of filled 125mL flask (g) 99.5231 99.6480 99.7414 99.7836 99.7217 Apparent mass of water (g) 9.9382 9.9424 9.9185 9.9785 9.9683 Trial 2 Buret Readin g (mL) 0.0210.00 10.0020.00 20.0029.99 29.9939.99 39.9950.00 Mass of empty 125mL flask (g) 89.5927 89.6865 89.6846 89.6968 89.6903 Mass of filled 125mL flask (g) 99.4860 99.6463 99.6352 99.6567 99.6534 Apparent mass of water (g) 9.8933 9.9598 9.9506 9.9599 9.9631 Trial 3 Buret Readin g (mL) 0.0110.00 10.0020.00 20.0030.01 30.0140.00 40.0050.01 Mass of empty 125mL flask (g) 89.5878 89.6517 89.6742 89.7054 89.7170 Mass of filled 125mL flask (g) 99.5244 99.597 99.6538 99.6526 99.6947 Apparent mass of water (g) 9.9366 9.9453 9.9796 9.9472 9.9777 True vol. of water (mL) 9.9744 9.9831 10.0175 9.985 10.0156 Buret correcti on (mL) -0.016 -0.017 0.008 -0.005 0.006 True mass of water (g) 9.9453 9.9541 9.9884 9.9560 9.9865 True vol. of water (mL) 9.9309 9.9976 9.9884 9.9977 10.001 Buret correcti on (mL) -0.049 -0.002 -0.002 -0.0023 -0.009 True mass of water (g) 9.9020 9.9686 9.9593 9.9687 9.9719 True vol. of water (mL) 9.9760 9.9802 9.9910 10.0164 10.0062 Buret correcti on (mL) -0.024 -0.0098 0.011 -0.0136 0.026 True mass of water (g) 9.9469 9.9511 9.9272 9.9873 9.9771

TABLES 1.2 Data to construct calibration curve

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab

Trial 1 Vol. of water (mL) 10 20 30 40 50 Vol. delivered 9.99 19.98 29.96 39.99 49.97
Mass delivered Actual vol Buret correction (mL) -0.01 -0.02 -0.05 0.03 -0.04

9.9382
19.8806 29.7991 39.7776 49.7459

9.9760
19.9561 29.9123 39.9288 49.9349

Trial 2 Vol. of water (mL) 10 20 30 40 50 Vol. delivered 9.98 19.98 29.97 39.97 49.98
Mass delivered Actual vol Buret correction (mL)

9.8933 19.8531 29.8037 39.7636 49.7267

9.9309 19.9285 29.9170 39.9147 49.9157

-0.05 -0.05 -0.05 -0.06 -0.06

Trial 3 Vol. of water (mL) 10 20 30 40 50 Vol. delivered 9.99 19.99 30.00 39.99 50.00
Mass delivered Actual vol Buret correction (mL)

9.9366 19.8819 29.8615 39.8087 49.7864

9.9744 19.9575 29.9750 39.9600 49.9756

-0.02 -0.03 -0.025 -0.03 -0.02

APPENDIX III

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab Calibration curve of 25mL buret
Chart Title

Correction

Volume delivered (mL)

APPENDIX IV

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab Correction factor of water at 23C and 24C

Buoyancy Equation, m :

i) Date & Time: January 28th, 2013 at 3.00pm. m

dw dH2O da

= m (1 - da/dw)/(1 da/d)
= 8.0 g/mL (Harris, 2013, p. 40) = 1g/1.0035mL = 0.0655 lbm/ft3 = 1.02 x 10-3 g/mL

ii) Date & Time : February 5th, 2013, at 2.00pm. m

dw dH2O da

= m (1 - da/dw)/(1 da/d)
= 8.0 g/mL (Harris, 2013, p. 40) = 1g/1.0038mL = 0.0657 lbm/ft3 = 1.01 x 10-3 g/mL

APPENDIX V

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab Tolerances for Class A volumetric glassware

NAME: SONIA NAJIB COURSE: CHEM 371, M/W Lab SOURCES Harris, D.C. (2013). Exploring Chemical Analysis 5th Edition. New York: W. H. Freeman and company