This document provides instructions for calibrating common volumetric laboratory glassware including volumetric flasks, pipettes, and burettes. The calibration process involves measuring the mass of water delivered by the glassware and using correction factors to determine the actual volume. Students will calibrate their personal glassware and create a calibration curve for their burette to account for any differences between the measured and actual volumes delivered.
This document provides instructions for calibrating common volumetric laboratory glassware including volumetric flasks, pipettes, and burettes. The calibration process involves measuring the mass of water delivered by the glassware and using correction factors to determine the actual volume. Students will calibrate their personal glassware and create a calibration curve for their burette to account for any differences between the measured and actual volumes delivered.
This document provides instructions for calibrating common volumetric laboratory glassware including volumetric flasks, pipettes, and burettes. The calibration process involves measuring the mass of water delivered by the glassware and using correction factors to determine the actual volume. Students will calibrate their personal glassware and create a calibration curve for their burette to account for any differences between the measured and actual volumes delivered.
This document provides instructions for calibrating common volumetric laboratory glassware including volumetric flasks, pipettes, and burettes. The calibration process involves measuring the mass of water delivered by the glassware and using correction factors to determine the actual volume. Students will calibrate their personal glassware and create a calibration curve for their burette to account for any differences between the measured and actual volumes delivered.
1 Introduction: Two basic types of equipment in an analytical laboratory are volume measuring devices and balances. Volumetric glassware used in analysis should be clean.
• Glassware that looks clean may or may not be clean.
• Surfaces, that have no visible dirt, are sometimes contaminated with invisible film of greasy materials. • Glassware into which a brush can be inserted such as beaker or Erlenmeyer flasks, are best cleaned with soap or synthetic reagent. ▪ Pipettes, burettes, and volumetric flasks, on the other hand, are ordinarily cleaned with cleaning solution, whose strong oxidizing properties ensure clean glass surfaces in most cases. • Afte cleaning, apparatus should be rinsed several times with tap water then with small portions of distilled water, and finally allowed to drain. Calibrations of volumetric glassware used in volumetric analysis is sometimes necessary. Tables (1) (2) (3) show some of the tolerance values established for volumetric glassware.
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2 Very often Low-priced glassware does not meet these tolerances. For this reason, it is often advisable for the student to calibrate his volumetric glassware. Volumetric glassware can be calibrated to measure the volume that is actually contained in or delivered by a particular piece of equipment. Calibration is done by measuring the mass of water contained or delivered and using Table 2-5 to convert mass into volume: True volume (actual volume) = (mass of water) x (correction factor in table 4) Objectives: • This lab will introduce the basic laboratory equipment and skills you will need for accurate and precise quantitative analysis. • To determine through the calibration process the actual volume delivered by volumetric tools, as opposed to the volume they say they deliver; this information will be contained in correction factors and a burette correction graph specific for your personal stash of glassware and you will use the data throughout semester. Laboratory Procedure: A. Volumetric flask calibration Figure 1 shows different kinds of volumetric flasks. 1. Select a clean dry volumetric flask to calibrate. 2. Record the mass of the empty, dry volumetric flask. 3. Fill the flask to the mark with deionized water and record the mass.
Because of the time constraints, we will not repeat this procedure-the flask would need to be dried between measurements.
3 B. Pipette Calibration Figure 2 shows different kinds of volumetric pipettes. Pipettes are made to deliver specific volumes. The following procedure will be used to calibrate your 10 mL pipette. 1. Determine the weight of an empty large weighing bottle or small beaker. 2. Fill the pipette to the mark with distilled water. 3. Empty the pipette into the weighing bottle or beaker. Be sure to touch off the pipette on the side of the weighing bottle. 4. Weigh the container and its contents. 5. Repeat this three times to obtain total of three measurements. (Report the mass of each individual addition- the net mass on the data sheet)
Figure 2 C. Calibrating a 50-mL Burette This procedure tells how to construct a graph such as the figure 3 below to convert the measured volume delivered by a burette to the true volume delivered at 20°C.
4 1. Fill the burette with distilled water and force any air bubbles out the tip (Figure 4). o See whether the burette drains without leaving drops on its walls. o If drops are left, clean the burette with soap and water soak it with cleaning solution. • Adjust the meniscus (Figure 4) to be at or slightly below 0.00 mL, a touch the burette tip to a beaker to remove the suspended drop of water. • Allow the burette to stand for 5 min while weigh a 100 mL flask (hold the flask with a paper towel to prevent fingerprints for changing its mass). • If the level of the liquid in the burette has changed, tighten the stopcock and rep the procedure. Record the level of the liquid. 2. Drain approximately 10 mL of water into weighed flask, and cap it tightly to prevent evaporation.
• Allow 30 s for the film of liquid on the walls to descend before you read the burette. Estimate all readings to the nearest 0.01 mL. • Weigh the flask again to determine the mass of water delivered. 3. Drain the burette from 10 to 20 mL, and measure the mass of water delivered.
• Repeat the procedure for 30, 40, and 50 mL
Calculations: ▪ Using the correction factor table, calculate the water volumes from the masses you recorded. ▪ For the burette, construct a calibration graph similar to that in figure 3. Questions: 1. How do your results for the volumetric flask and transfer pipette compare with the Class A standards listed in Tables 1 & 3? 2. How different were the burette readings from the actual volumes delivered? Is this error acceptable? Attach your burette calibration curve to this report sheet.
5 aBurette Volume= (burette reading for this aliquot)-(Initial burette reading) bMass of Water= (mass of this aliquot)-(initial mass) cActual Volume = (mass of water) × correction factor-see Table 4 in book) d Correction = (Actual volume) - (burette volume)
