Handling Volumetric Glassware

Please review these practical techniques BEFORE coming to the Ontario Preparation Weekend!

1.

Obtaining Accurate Weights

Modern analytical balances allow weights to be obtained to the nearest 0.1 mg fairly easily. Proper technique is essential, however, if accuracy and precision are required. Most importantly, materials should be pure, dry, at room temperature, and both chemically and physically stable. Analytical balances are generally reliable, but can be prone to drifting or erratic readings if not used correctly. In general:

Procedure:

Do not move the balance Avoid touching weighing bottles with your bare hands Avoid creating static charge on weighing bottles Keep the balance pan free of chemicals Always close the balance doors when weighing Do not lean or tap on the bench while weighing Always determine the mass transferred by difference

1. Calculate the mass required for your experiment. 2. Dispense approximately the mass required into a clean, dry weighing bottle using a 2- or 3-decimal place top-loading balance. 3. Close the doors on an analytical balance, and set it to zero using the tare button. 4. Use crucible tongs or a folded slip of paper to place the weighing bottle on the balance pan. * Do not handle weighing bottles with your bare hands or rubber gloves!

5. Close the balance doors, and record the reading once stable. 6. Use crucible tongs or a folded slip of paper to remove the weighing bottle, and empty the contents into a suitable vessel. 7. Using crucible tongs or a folded slip of paper as before, re-weigh the weighing bottle, remembering to close the balance doors before taking the reading. 8. Remove the weighing bottle and close the balance doors; leave the balance clean and tidy for the next person.
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2.

Quantitative Transfer

The goal of quantitative transfer is to make sure that all of a solution is transferred from one vessel to another. It is typically used when preparing standard solutions from solids, as it is often undesirable to transfer and dissolve solids directly into volumetric flasks. In general:

Avoid spills and splashes Keep glassware positioned where it wont get knocked or fall over Make sure you have everything you need before you start
Procedure: 1. Take note of the size of the volumetric flask; you do not want to use more than about half this volume of solvent to dissolve the solid. 2. Dispense accurately the mass of solid required into a suitable size beaker. * You do not need to dispense exactly the right amount, as long as you know the actual mass transferred as accurately as possible (i.e. by difference to 0.1 mg) 3. Add about a quarter to a half of the required volume of distilled water to the solid in the beaker, and stir until the solid is fully dissolved. Funnel Clamp Volumetric flask

Decant down glass rod

Push last drop back into beaker 4. Position a funnel in the neck of the volumetric flask using a ring clamp, leaving an air gap between the stem of the funnel and the sides of the flask. 5. Decant the contents of the beaker down a glass rod into the funnel; use the glass rod to push the final drop in the beakers spout back into the beaker. * Keep the glass rod in the beaker! 6. Use a wash bottle to rinse the walls of the beaker; decant the washings into the flask as in step 5. Do this at least twice, making sure that you do not over-fill the flask (i.e. the solution should remain below the calibration mark on the neck.) 7. Rinse the glass rod into the funnel, then remove the flask from under the funnel. 8. Use a Pasteur pipette and rubber bulb to fill the flask to the calibration mark with distilled water. Stopper the flask, and mix the contents by repeated inversion.

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3.

Using a Transfer Pipette

Transfer pipettes allow specific volumes of solution to be dispensed precisely and accurately. They come in two basic types: ones marked TD (to deliver) and ones marked TC (to contain). The former are commonly used with aqueous solutions, and are calibrated to deliver the specified volume a small uncertainty when drained without forcing the final small volume of solution out. In general:

Procedure:

Always rinse pipettes with a small volume of the solution to be dispensed Never pipette by mouth always use a pipette filler Use a small beaker to hold the solution when filling the pipette Keep the tip of the pipette in the solution when filling Never shake a pipette to remove residual liquid after cleaning Keep a clean paper towel or KimWipe handy to dry the pipette tip

1. Pour a small excess of the solution to be dispensed into a small clean, dry beaker. 2. To operate a three-valve pipette filler: use the top valve (1) to evacuate the filler; place the filler on the end of the pipette without forcing it; use the middle valve (2) to draw solution into the pipette; use the lower valve (3) to drain it.

3. To rinse a pipette, draw a small volume of solution into the pipette (usually just up to the lower part of the wide middle section.) Tip the pipette horizontally, slide the filler off the end, and let the solution run past the calibration mark while rotating the pipette. Drain the solution into a waste container. Rinse two or three times in total. 4. Fill the pipette by drawing the solution up past the calibration mark on the stem, but not so far that the solution enters the pipette filler. 5. Remove the pipette from the solution, and wipe any excess liquid from the outside of the pipette at the tip. 6. Holding the pipette over the beaker of solution, carefully drain the pipette until the bottom of the liquid meniscus just touches the calibration mark; if you drain to far, refill following steps 4 and 5, then try again. 7. Hold the pipette just inside the neck of the required volumetric flask, and drain the contents of the pipette into the flask under gravity. Lightly touch the tip of the pipette to the liquid surface in the flask to deliver the correct volume.

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4.

Using a Burette

Burettes allow controlled volumes of solution to be delivered precisely and accurately. When operating the burette, make sure it is clamped in the lower half (about a third of the way up from the valve) in order to avoid stressing the glass. You should always interpolate the meniscus between scale markings to achieve the greatest precision. In general:

Always rinse burettes with a small volume of the solution to be dispensed Never reach overhead to fill a burette; lower it within the clamp, place the
Procedure: 1. Pour the solution to be dispensed into a clean, dry beaker. 2. Make sure the valve on the burette is closed (tap at right-angles to the burette), and then pour a few millilitres of solution into the burette while rotating it. 3. Drain this solution into a waste beaker, and repeat step 2 one or two times more. 4. Fill the burette with solution up past the zero reading on the scale. Run a small volume of the solution out in order to expel the air. 5. Reading a burette: take the reading with the liquid meniscus at eye level (move the burette if necessary!). Interpolate the reading on a 50 mL burette between scale divisions to the nearest 0.01 mL: clamp stand on a stool, or remove the burette from the clamp to fill it Expel the air in the burette tip by opening the valve fully once filled; a full height of liquid is needed to expel the air Never shake a burette to remove residual liquid after cleaning Keep a clean paper towel or KimWipe handy to dry the burette tip Never waste time trying to get the initial reading to be exactly zero; this is actually less accurate than recording a reading within the scale.

To deliver

0.00 mL 0.10 mL 0.20 mL 0.30 mL 0.40 mL

1st scale division

0.50 mL

Reading is estimated as 0.18 mL

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