Analysis of Commercial Bleach

Many commercial products are effective because they contain oxidizing agents. Some products which contain oxidizing agents are bleaches, hair coloring agents, scouring powders, and toilet bowl cleaners. The most common oxidizing agent used in bleaches is sodium hypochlorite, NaClO (or NaOCl).________________________________________________ 1) Commercial bleaches are made by bubbling chlorine gas into a sodium hydroxide solution. Some of the chlorine oxidizes to the hypochlorite ion, ClO-, and some is reduced to the chloride ion. The solution remains strongly basic.___________________________________ 2) The amount of hypochlorite ion present in a solution of bleach can be determined by an oxidation-reduction titration. One of the best methods is the iodine-thiosulfate titration procedure. Iodide ions are easily oxidized by almost any oxidizing agent. In an acidic solution, hypochlorite ions will oxidize iodine ions to the diatomic iodine molecule. Chloride ions and water will also form.___________________________________________________ 3) Diatomic iodine molecules are only slightly soluble in water, unless there are other iodine ions present in the solution. Then the triiodide complex is formed (I3-), which is very soluble. The color of the triiodide complex is yellow in dilute solutions and dark red to brown in concentrated solutions.________________________________________________________ 4) The triiodide is titrated with a standard of thiosulfate ions, which reduces the triiodide ions back to iodine ions. This reaction also forms S4O62- ions.____________________________ During this last reaction the red-brown color of the triiodide ion fades to yellow and then to the clear color of the iodide ion. It is possible to use the disappearance of the color of the triiodide ion to determine the endpoint, but this is not a very sensitive procedure. Addition of a starch solution to any solution containing iodine or triiodide ions will form a reversible blue complex. That is, if the iodine, or triiodide ions are converted into iodine ions, the starch complex will turn clear. The disappearance of the blue colored complex is a much more sensitive method of determining the end point. However, if the starch solution is added to a solution, which contains a great deal of iodine ions, the complex which forms may not be reversible. Therefore, the starch solution is added just before the end point is reached. The quantity of thiosulfate used in equation 4 is directly related to the amount of hypochlorite that was initially present in the bleach. Prelab Questions 1) Write the four net ionic equations for the above numbered paragraphs. 2) What is the ratio of thiosulfate ions used in relation to the hypochlorite ion in the bleach? 3) Calculate the molarity of the diluted bleach if, in this lab, 11.3 mL of the sodium thiosulfate

solution is used. 4) Calculate the molarity of the commercial bleach. 5) Assume the density of commercial bleach is 1.08 g/ml. Using the molarity in question 4, determine the % (by mass) of NaClO in the bleach. Chemicals Bleach, NaClO Starch solution

Hydrochloric acid, HCl 3 M Sodium thiosulfate, Na2S2O3 0.100 M

Potassium iodide, KI (s) Baking Soda NaHCO3 (s)

Equipment Transfer pipets, 5 and 25 mL Erlenmeyer flask, 125 or 250 mL

Ring stand Buret and clamp

Pipet bulbs Volumetric flask, 100 mL

Precautions Bleach is damaging to the skin, eyes and clothing, as well as hydrochloric acid. Both also give of strong vapors. Adding hydrochloric acid to bleach may cause chlorine gas to be given off! Carry out this procedure in the fume hood!

Procedure
1. Dilute the concentrated bleach: Use a pipet bulb and a 5-mL transfer pipet to measure 5.00 mL of a commercial bleach solution into a 100-mL volumetric flask. Dilute to the mark with distilled water, stopper and mix well. 2. Measure the potassium iodide: Weigh out approximately 2 g solid KI. This is a large excess over that which is needed.
Reminder for using burets: Rinse them with distilled water (never assume anything is clean), then be sure to rinse the buret with about 5 ml of the solution you are going to put into the buret, then drain out the solution into the sink. This assures any droplets inside the buret are the solution you are going to be putting inside. If they were pure water droplets, that would dilute the solution you are putting in the buret. So there ya go.

3. Oxidize the iodide ion with hypochlorite ion: Put the diluted bleach solution in a buret and use the buret to measure 25 mL of the dilute bleach into an Erlenmeyer flask. Add the solid KI and about 25 mL of distilled water. Swirl to dissolve the KI. Work in a fume hood and slowly, with swirling, add approximately 2 mL of 3 M HCl. The solution should be dark yellow to red-brown from the presence of the I3- complex ions. 4. Titrate the iodine: Use a second buret for the Na2S2O3 solution. Record the initial buret reading. Titrate with a standard 0.10 M sodium thiosulfate solution until the iodine color becomes light yellow. MAKE SURE YOU SWIRL! Add one dropper of starch solution. The blue color of the starch-iodine complex should appear. Continue the titration until one drop of Na2S2O3 solution causes the blue color to disappear. Record the final buret reading. 5. Repeat: Repeat the titration beginning with step 2 two more times.

6. Disposal: The solutions may be safely flushed down the drain with a large excess of water.

Data and Calculations

1. Use the equations given to determine the number of moles of sodium thiosulfate that are equivalent to one mole of sodium hypochlorite. 2. Calculate the average volume of Na2S2O3 needed for the titration of 25.00 mL of the diluted bleach. 3. Use the average volume and molarity of Na2S2O3to determine the molarity of the diluted bleach. 4. Calculate the molarity of the commercial bleach. 5. Assume that the density of the commercial bleach is 1.08 g/mL. Calculate the percent by mass of NaClO in the commercial bleach. 6. Read the label of the commercial bleach to find the percent by mass NaClO that is reported. Calculate the percent error of your value, assuming the label is correct.

Discussion

Include answers to the following in your laboratory report:

1. Define oxidation and reduction. 2. Write balanced oxidation and reduction half-reactions for the equations (2) and (4). For each half-reaction, identify which substance is oxidized or reduced. Identify the oxidizing and reducing agents. 3. In this analysis, an "aliquot", or a diluted fraction of the initial solution is used for the titration. What advantage is there in diluting the original solution for the analysis? 4. How many 25 mL aliquots can be measured from a 100 mL volumetric flask? Explain. 5. The reaction with thiosulfate ions produces the dithionate ion, S4O62-. Calculate the oxidation number for the sulfur in this ion. Do you think that the sulfur atoms in the ion will all have the same oxidation number? What might the oxidation numbers be? 6. How would each of the following laboratory mistakes affect the calculated value of the percent NaClO in the commercial bleach (too high, too low, no change)? Explain. a) Passing the endpoint b) The Na2S2O3 is slightly diluted c) The volume of diluted bleach used in the titration was more than you thought 7. What is the major source of error in this experiment?