Skill-Building Exercise:

Using Burets and Performing Titrations

We have used a many different pieces of equipment thus far in lab. You should feel comfortable with various filtering methods, volume measurements, mass measurements, and solution preparations, to name just a few. One of the last techniques that will be presented is titrations, requiring the use of a buret. It is the purpose of this skill builder to introduce you to the buret, teach its proper use, and give you a change to practice using it. A buret is a long tube calibrated to deliver variable volumes of liquid (usually with 0.02 mL accuracy). This is accomplished with a stopcock at one end that allows the user to control the flow of liquid. To use a buret: 1. Make sure it is clean. There are long brushes at the sinks that are designed for burets, and the stopcock can be removed for easier cleaning. 2. Before filling the buret, double check that the stopcock is in the CLOSED position (dont worry, it happens to the best of us ). You should also make sure the stopcock fits tightly and that there are no leaks present. 3. Next, rinse the buret two or three times with the solution that you will be using. This is called conditioning and insures that the concentration of your solution is uniform and not diluted by any remaining water. 4. Set up a ring stand with a buret clamp. Each clamp can hold up to two burets, but there are enough for everyone to use their own as well. 5. To fill the buret, remove it from the clamp, bring it down to eye level, place a funnel in the top, and add your solution slowly. You should never pour liquids above your head for safety reasons. Be careful not to overflow the buret. You can always use a disposable pipet near the end to avoid an overflow. 6. Fill the buret above the zero calibration mark. This allows you to drain it slightly to remove any air bubbles that may be in the tip. 7. You are now ready to begin your titrations. A few notes: You do not need to have the solution exactly at zero to begin. There are times when it is easier (for example, collecting a titration curve with LoggerPro), but most of the time, you can just read the initial volume and then the final volume.

There should never be drops remaining on the tip of the buret. This liquid has been measured, but not added. You can either touch the tip of the buret to the side of your beaker or flask, or simply rise the tip with DI water from a pipet or washbottle. You should always operate the stopcock slowly. Dont flip it around 360, but rather rotate it forward to open and backwards to close. Reading a Buret: To clearly see the meniscus, it is best to use a small piece of paper with a heavy black line, as shown. Hold the line behind the buret just under the meniscus. This will highlight the meniscus and allow for an accurate reading. The burets are calibrated to units of 0.1 mL, so you should be able to estimate to 0.02 mL Example:

TITRATIONS A titration is a method of analysis that will allow you to determine the precise endpoint of a reaction and therefore the precise quantity of reactant in the titration flask. Often, you add a solution of a known concentration to one of an unknown concentration in order to determine the unknown. A buret is used to deliver the second reactant to the flask and an indicator or pH Meter is used to detect the endpoint of the reaction.

There are many types of titrations. This semester, you will do a complexometric titration and an acid/base titration, but there are also redox titrations and several other common ones. The simple procedure involves measuring one reactant into a flask, adding the second to the buret, adding an indicator (or using a pH meter), and then titirating. Depending on the titration, you can often go quickly until just close to the endpoint, and then proceed very slowly. Make sure you know what the endpoint should look like. For phenolphthalein, the endpoint is the first permanent pale pink. The pale pink fades in 10 to 20 minutes. If you think you might have reached the endpoint, you can record the volume reading and add another partial drop. Sometimes it is easier to tell when you have gone past the endpoint. The photo on the left is correct, the flask on the right has gone past the endpoint.

Solutions of sodium hydroxide are virtually impossible to prepare to a precise molar concentration because the substance is hygroscopic. In fact, solid NaOH absorbs so much moisture from the air that a measured sample of the compound is never 100% NaOH. On the other hand, the acid salt potassium hydrogen phthalate, KHC8H4O4, can be measured out in precise mass amounts. It reacts with NaOH in a simple 1:1 stoichiometric ratio, thus making it an ideal substance to use to standardize a solution of NaOH. During this SBE, you will make and standardize a solution of NaOH. You should have at least three trials that agree within 1%.

OBJECTIVES
By preparing for and performing this exercise, you will:

Be introduced to a buret; Learn the proper technique for using a buret to add a variable volume of solution; Prepare an aqueous solution of sodium hydroxide to a target molar concentration; Determine the concentration of your NaOH solution by titrating it with a solution of potassium hydrogen phthalate, abbreviated KHP, with an exact molar concentration.

MATERIALS
Chemicals (hood/balance bench): Potassium hydrogen phthalate, KHP(s) Sodium hydroxide, NaOH(s) Prepare NaOH solution: 1. Measure out the mass of NaOH needed to prepare 250 mL of a 0.100 M solution and add it to some distilled water. Swirl the flask to dissolve the solid. CAUTION: Sodium hydroxide solution is caustic. Avoid spilling it on your skin or clothing. Next, add your solution to a volumetric flask and dilute to 250 mL. 2. Measure out the mass of KHP that will completely neutralize about 15 mL of 0.100M NaOH solution. Dissolve the KHP in about 50 mL of distilled water in an Erlenmeyer flask (this may take some time). Why does the amount of water not matter? 3. Set up a ring stand, hotplate/stirrer, buret clamp, and buret to conduct a titration. Rinse and fill the buret with your NaOH solution. Note: Burets are expensive, so please handle with care. The white stopcock can be removed for easier rinsing and cleaning. You should always fill the buret using a funnel at or below eye level. 4. Put the stir bar in your flask and begin to stir the acid solution. 5. After adding indicator (phenolphthalein), you are ready to begin your titration. The equivalence point is reached when the indicator remains a light pink color. Any pink is pink enough so avoid going too quickly once you observe the pink color taking longer to fade. When titrating, it is common to add liquid more quickly at the beginning and then slow down once the pink color begins to fade less quickly. 6. Make sure to dispose of all waste in the aqueous waste containers. Repeat the titration with additional KHP trials until you have a 1% agreement between your calculated concentration values. YOU NEED TO SAVE YOUR NaOH SOLUTION IN YOUR STORAGE BOTTLE FOR LATER. Equipment, (dispensing room): 250 mL Volumetric Flask Buret Stir bar Equipment, (common): Buret clamps Ring Stand Hotplate/Stirrer

Turn you notebook pages into your TA, questions and data for this week will be combined with the Acid/base experiment next week.