Bleach Lab Activity of Bleach Lab Name: ___________________________________________ Page 1 of 4 Introduction The traditional commercial bleaches such as ChloroxTM and PurexTM are solutions of sodium hypochlorite, NaClO, in water. The hypochlorite ion, ClO-, is a fairly strong oxidizing agent. The bleach removes stains by their chemical oxidation. In this experiment we will perform a quantitative analysis on commercial bleach samples to determine the amount of the active ingredient hypochlorite ion they contain. To do this, we will dissolve weighed samples, add an excess of a reagent, I-, which reacts with the hypochlorite ions to form I3- with a standard solution of thiosulfate. The chemical reactions involved are called oxidation-reduction reactions. A whole series of quantitative analyses are based upon the quantitative reduction of a strong oxidizing agent by I- followed by titration of I3- with thiosulfate, S2O32-. Quantitative methods of this particular type are called iodometric determinations. The chemical reaction between hypochlorite and iodide ion can be written ClO- + 3I- + 2H+ ----> Cl- + H2O + I3and the reaction taking place during the titration can be written as I3- + 2S2O32- ----> 3I- + S4O62Thus two moles of thiosulfate ion are consumed by each mole of hypochlorite ion. (The product ion S4O62-, is called dithionate.) One takes a known quantity of bleach solution and finds the number of moles of thiosulfate it indirectly consumes through measuring the volume of a standard solution of thiosulfate required to titrate the I3- is formed. Then the concentration of hypochlorite in the bleach can be calculated. It is possible to prepare sodium thiosulfate solutions of accurately known concentration by weighing out the anhydrous salt, but the titer of the thiosulfate solutions tends to change slowly with time making it advisable to standardize the solution at the time it is used. Thus you will standardize your thiosulfate solution using potassium iodate as the primary standard. IO3- + 8I- + 6H+ ----> 3I3- + 3H2O The triiodide (I3-) produced is then titrated with thiosulfate using the reaction above to determine the concentration of the thiosulfate solution. You will prepare a 0.1 M Na2S2O3 solution and standardize it against an accurately known amount of KIO3, and then will be analyzed. The results for all the analyses for a given lab room and day (two sections) will be collected and provided to you. You will then perform some statistical analysis of the results and decide which of the two products provides the more bleach per buck. Properties of Sodium Thiosulfate Solution Sodium thiosulfate solutions properly prepared are quite stable, but there are two potential sources of instability. First, in acid solutions, thiosulfate slowly disproportionates to sulfite and elemental sulfur to the reaction S2O32- + H+ ----> HSO3- + S Since the deionized water coming out your tap is slightly acidic (as you will find out in the pH experiment) because of dissolved carbon dioxide, this is potentially a problem. To make the thiosulfate solution to be as stable as possible, one should boil the deionized water used to make the solution, thus driving out dissolved CO2, and also add a small amount of sodium carbonate to insure the solution is slightly basic. The concentration of your thiosulfate solution can change not only from the disproportionation reaction, but also because some bacteria actually eat sodium thiosulfate! Sterilization of the reagents and glassware can prevent this problem. Fortunately, because we’ll do all of our thiosulfate titrations in a short time we don’t have to go to the trouble of insuring a very stable solution. During the preceding lab period you should dry about 1 to 1.5 grams of KIO3 at 120˚ C for 1-2 hours. 1 The reaction produces more I3- by 6I- + O2 + 4H+u2I3- + 2H2O Bleach Lab Name: ___________________________________________ PREPARATION OF 0.1 M SODIUM THIOSULFATE Page 2 of 4 Weigh out approximately 7.9 g of Na2S2O3 on a watch glass or weighing paper using one of the rough balances in the main lab. Transfer into your clean 500 mL clear glass bottle and add approximately 500 mL of deionized water. Then insert the glass stopper and shake very thoroughly to obtain a solution of uniform concentration. STANDARDIZATION OF 0.1 SODIUM THIOSULFATE The solution should be standardized on the day you titrate the bleach samples. Calculate before coming to class the weight of KIO3 which will require 20 mL of 0.1 M Na2S2O3 solution to titrate the I3- that it produces. This will turn out to be less than 0.1g of KIO3. Therefore in order to improve your precision, weigh accurately a KIO3 sample that is within 15% of four times the weight for a single titration as calculated above into your 100 mL volumetric flask. Dissolve and make up to the mark. Don’t forget to mix thoroughly. You will titrate a 25.00 mL aliquot of this KIO3 solution withdrawn using your 25 mL volumetric pipet. You need to have at hand 1g of KI for each sample, about 10 mL of dilute (1:4) sulfuric acid, and about 5 mL of starch indicator solution. Make sure that your buret is clean and drains without forming droplets on the walls. Rinse it three times with small portions of your thiosulfate solution and then fill to a point on scale near the top. Read the initial volume to 0.01 mL. Put a 25.00 mL aliquot from your KIO3 solution into one of your 125 mL Erlenmeyer flasks and add 1g of KI to one of your KIO3 samples and swirl to dissolve. Then add 2-3 mL of the dilute sulfuric acid. The solution should immediately become dark red from the formation of I3-. Because I- (which is in excess) is readily air-oxidized1 in strongly acidic solution, titrate immediately with the thiosulfate. You may proceed with the addition of titrant very rapidly until the solution becomes a pale yellow. When the solution is a very pale yellow, add 1-2 mL of the starch indicator solution. The solution will immediately turn blue-black. Titrate to the disappearance of the blue color (probably about 1/2 mL more of titrant will be required). Repeat with the other sample. The calculated concentrations of the thiosulfate solution should agree within a few parts per thousand. We suggest that you verify that the ratio of the volume thiosulfate to weight of KIO3 agree within a few parts per thousand before continuing. If not, weigh out more KIO3, and do more standardization titrations. For the report, put a note in the standardization section and the results on the back page of the report PREPARATIONS OF THE BLEACH SAMPLES Bleach is sold by volume so that in order to calculate the cost per mole of ClO- we need to measure the sample by volume. Obtain about 30 mL of one of the two bleach solutions in the lab in a small beaker. (Be sure to write down the cost/bottle and the volume of the bottle!) Immediately, using your 10 mL volumetric pipet, pipet 10.00 mL of the bleach into a clean, but not necessarily dry 250 mL volumetric flask (BE SURE TO USE THE RUBBER BULB AND NOT MOUTH SUCTION!!). Fill the volumetric flask to mark with deionized water, put in the stopper, and mix thoroughly by inverting the flask at least 10 times. TITRATION OF THE BLEACH SAMPLES Using your 25 mL volumetric pipet, transfer 25.00 mL of the bleach solution to a 125 mL Erlenmeyer flask. Fill your buret with thiosulfate solution and read the buret. Add 5 mL of glacial acetic acid (WARNING: Glacial acetic acid burns the skin! If you get any on you wash it off with copious amounts of tap water.), mix and then add 1g of potassium iodide. The solution will again immediately turn dark reddish brown indicating the formation of I3-. Rapidly titrate (to minimize air oxidation) the solution as in the thiosulfate titration above. Repeat. If the same amount of thiosulfate is required for both titrations within 0.05 mL, go through the same procedure with the other bleach sample; otherwise repeat the titration again until satisfactory reproducibility is achieved. 1 The reaction produces more I3- by 6I- + O2 + 4H+u2I3- + 2H2O Bleach Lab Name: ___________________________________________ Page 3 of 4 CALCULATIONS From the standardization titrations calculate the concentration of thiosulfate in moles/1 for each standardization run. If your runs agree within a few parts per thousand use the average of the runs for the thiosulfate concentration in the rest of the calculations. Otherwise you will have to make a decision about which runs to keep and which to discard. Then calculate the number of moles of ClO- indirectly titrated for each run and from that result the concentration of ClO- in the original bleach solution taking the dilutions into account. Report your results on the computer in the lab your values obtained for the ClO- concentration for each run on each bleach solution. There will be a sheet for each bleach solution. If you know that there is good reason to believe that something went seriously wrong for a run, indicate that by putting an asterisk on the run. You will be given the results of your section and another section on the same samples for the statistical analysis asked for in the lab report. Bleach Lab Procedure (Short Version) Teacher Notes Note: I need a little more time with the students for this lab: Start at 6:15: Sorry kiddos Have them only draw a picture of the procedure (And some calcs) for their prelab) Standardization of the Thiosulfate 1. 2. 3. 4. 5. 6. 7. 8. Weigh out about 7.9 g of Na2S2O3 and dissolve in 500 mL of d.i. water. Shake thoroughly to get a solution of uniform concentration Calculate the weight of KIO3 which will require 20mL of 0.1 M Na2S2O3. [0.0713g] Weigh out 4 times the mass calculated in 2 above A: Place this in a 100 mL volumetric and dissolve Set up your burette rinsing it thoroughly with your thiosulfate solution. Put a 25.00 mL aliquot from the KIO3 solution into a 125 mL erlynmeyer flask: add 1 g of KI, 2-3 mL of dilute sulfuric acid Titrate immediately with the thiosulfate solution: When the solution is pale yellow add 1-2 mL of starch indicator solution. It will then turn blueblack. Titrate until the blue goes away (Probably 1/2 mL more) Repeat this and do it again. Bleach 1. 2. 3. 4. 5. 6. 7. Obtain 30 mL of the bleach and place this in a clean dry beaker Use a 10mL volumetric pipet and place in a clean 250 mL volumetric flask. This is to dilute the bleach so that it can be tested more easily. Transfer 25 mL of the dilute bleach into a 125 mL Erlenmeyer flask Add 5 mL of glacial acetic acid danger Add 1 g of KI. The solution will turn reddish brown. Rapidly titrate with the thiosulfate Repeat until satisfactory reproducibility is achieved. Bleach Lab Expectations Formal Lab write-up Procedure should have a series of pictures Data and Calculations 1. Data in neat data tables: 2. Show the following calculations Amount of KIO3 required 1 The reaction produces more I3- by 6I- + O2 + 4H+u2I3- + 2H2O Bleach Lab Name: ___________________________________________ Concentration of S2O32 Concentration of ClO- (Don't forget to multiply by the dilution factor) Page 4 of 4 Error Discussion List and discuss sources of error in a cause effect table Discussion Questions: 1. Why was it necessary to dilute the bleach in order to titrate it? 2. Explain why it was necessary to use the thiosulfate ion to determine the concentration of the hypochlorite ion. (Remember that the thiosulfate ion is not a part of the main reaction that involves the hypochlorite ion.) Conclusion Include the final answer which is both your answer and the class answer. 1 The reaction produces more I3- by 6I- + O2 + 4H+u2I3- + 2H2O