Techniques in Chemistry: Using A Burette: Initial Comments

TECHNIQUES IN CHEMISTRY: USING A BURETTE
INITIAL COMMENTS The burette is a rather delicate piece of equipment which costs in the neighbourhood of $70 to $80, so that considerable care is required in order to avoid breakage. The purpose of performing a titration is to get a precise and accurate measurement of the volume of solution in a burette needed to react with a specific volume of another solution. Therefore, all equipment must be properly cleaned, solutions must be well mixed, beakers used to store standardized solutions must be clean and dry, and all readings must be as precise and accurate as possible. Note: If you have made up any of the solutions to be used during the titration, it is extremely important that the solutions be very well mixed. The biggest sources of inaccuracy in a titration are poorly mixed solutions and equipment which is wet. Any water present in burettes and pipettes will dilute any solutions used, and lead to poor results.
INSPECTING THE BURETTE The first thing to do when you get a burette is to check for a broken lower tip. If the tip is chipped the burette will still function well, but a badly broken tip should be reported to your instructor. Next, check that the adjustable valve ("stopcock") just above the tip can be turned easily, but is not "sloppy". If the stopcock has an adjustable nut on the small end of the turnable piece (the "barrel"), make sure the stopcock is not too loose or liquid will seep out and spoil your titrations. When the little handle on the stopcock is perpendicular to the glass tube, the stopcock is closed; when the handle is parallel to the tube, the stopcock is open and liquid can flow out of the burette.
CLEANING THE BURETTE Close the stopcock, half fill the tube with distilled water, open the stopcock to allow some water to drain through the tip, then close the stopcock, and invert the burette to drain the remaining water. NEVER HOLD A BURETTE BY ITS MIDDLE AND WAVE IT; YOU WILL SNAP IT IN HALF! (If the tip is clogged, see your instructor, who will clean the tip with a fine wire.) Rinse with water a second time. Then, close the stopcock, pour in about 5 mL of the solution with which you intend to fill the burette, tip the burette on its side and roll the solution around the inside of the burette. The idea here is to coat the inside of the burette with the solution to be used. Drain some of the solution through the tip, and discard the rest. Note: if no liquid drains from the tip, hold the burette over the sink, tip down and stopcock open, and give the burette tube a sharp little downward shake; the liquid should start to flow at this point. Repeat with a second 5 mL portion of the solution. By this time the burette should be "prepared" to receive the solution you intend to use.
FILLING THE BURETTE Set up a stand and double-sided burette clamp (NOT a test tube clamp!), and clamp the burette in place. Fill the burette with solution. Next, you must fill the tip of the burette with solution. This is most easily done by putting a waste beaker under the tip and quickly turning the stopcock to "full on" for a second. The rush of liquid should fill up the tip and carry any air bubbles out of the tip. If an air bubble persists, take the burette out of the clamp, hold the burette tip over the sink, quickly open the stopcock and give a sharp downward jerk to the burette (NOT TOO SHARP - you'll break the burette or tip!) If necessary, refill the burette close to the zero mark if a great deal of solution has been lost. You CANNOT get accurate results if there is an air bubble in the tip.
Page 2 READING THE BURETTE When reading the volume of the burette note the following: a) the burette volumes INCREASE as we go down the tube. b) the volume reading is taken from the bottom of the meniscus. c) the readings MUST be read with a precision of +/- 0.01 mL. That is, estimate the volume to +/- 1/10 of the smallest (0.1 mL) division. eadings which are only estimated to the nearest !." mL are useless.
PERFORMING THE TITRATION Using a burette is a one-person job. If two people attempt to use it ("You work the stopcock and I'll swirl the flask.") the task is made unnecessarily complicated and too many hands get in the way. One hand should grasp the stopcock with the main part of the barrel in the palm of the hand, and the other hand should swirl the receiving flask and make sure it is under the tip. The tip should be inside the flask, below the lip. #$%& T'(T: put some white paper under the flask to help make any colour changes evident. The solution to be titrated will contain some sort of indicator which will change colour at the exact endpoint of the titration. As you add the solution from the stopcock, there will be no change seen at first; don't swirl the flask until some colour change is seen. After swirling the flask, the colour should change back to the original colour. After several add solution/swirl flask cycles, you should notice that the colour change takes longer to disappear, so that less solution should be added from the burette. By the end of the titration you will be adding a drop of solution at a time, or even a "half drop". (A half drop is obtained by carefully opening the stopcock until a partial drop forms at the tip. This drop is put into the flask by touching the burette tip to the lower inside surface of the flask.) When the colour change )ust barely occurs and stays after swirling, you are at end point. Record the final volume and calculate the total volume added: total volume = final volume - original volume .
Now, refill the burette (you don't have to start from scratch, just add more solution), set up another flask containing the solution to be titrated, and repeat the titration. The volumes used must agree to within +/- 0.1 mL (+/- 0.02 mL is expected with college level courses). If the total volumes do not agree, repeat the titration a third time (or more) until you get good agreement between total volumes. If values are wildly out (more than +/- 0.5 mL) consult your instructor. When you have finished your titrations, wash out the burette with water TWICE, including water through the tip. If solution is left inside a burette, corrosion of the stopcock or clogging of the tip can occur. TROUBLE-SHOOTING Problem: The titration readings decrease slightly from one titration to the next in a continuous manner. Reason: The burette was not properly washed out with the solution eventually placed in the burette. Hence, leftover water in the burette diluted the solution in the burette, so that as more solution is added for repeat titrations the solution became slightly more concentrated and required less of the solution to react with the pipetted solution below the burette How to correct: Usually, the readings will settle down to a constant value as the number of repeats increases. In the future, be careful to rinse out the wash water 2-3 times with the solution to be added to the burette. Problem: The titration readings increase slightly from one titration to the next in a continuous manner. Reason: The pipette was not properly rinsed out 2-3 times with the solution to be used in the pipette. Hence the first pipette-full was slightly diluted, requiring less solution to be added from the burette. Subsequent pipette-fulls contain less contaminating water and require more solution from the burette. How to correct: Usually, the readings will settle down to a constant value as the number of repeats increases. In the future, be careful to rinse out the wash water 2-3 times with the solution to be added to the pipette.

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TECHNIQUES IN CHEMISTRY: USING A BURETTE

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