In the Laboratory

edited by

Cost-Effective Teacher

Harold H. Harris
University of MissouriSt. Louis St. Louis, MO 63121

A Small-Scale and Low-Cost Apparatus for the Electrolysis of Water

Per-Odd Eggen School Laboratory for Science and Technology, Norwegian University of Science and Technology, 7491 Trondheim, Norway Lise Kvittingen* Department of Chemistry, Norwegian University of Science and Technology, 7491 Trondheim, Norway; *Lise.Kvittingen@chembio.ntnu.no

The construction of two simple, inexpensive apparatuses that clearly show the electrolysis of water are described. Both apparatuses can be made by all students in any laboratory or classroom. The apparatuses were developed for a course in oxidationreduction chemistry aimed at secondary school instructors. Electrolysis of water is traditionally conducted in a Hofmann apparatus, which is expensive and fragile. Simpler and less expensive apparatuses have been reported (13) as well as changes to improve the demonstration (47). The apparatuses described here are appropriate for various grades and curricula. The two apparatuses are shown in Figures 1 and 2. The chemistry involved is not included, as this can be found in any general chemistry book, as well as in the references cited above. The components used to construct these apparatuses are disposable polyethene transfer pipets (also called Beral pipets) and floral wire (25 cm length, 1.1-mm diameter) from a local florist. The volume of the pipet bulbs is 3.5 mL, but the sizes of the stems vary. In these experiments 1-mL and 3-mL stem pipets have been used, but this is not critical and similar ones will work equally well. Both the pipets and the wire are chemically stable for the use intended here. Remember to use safety goggles during the experiment even though the risk of injury is very low. Apparatus for Electrolysis of Water with Hydrogen and Oxygen Collected Together The complete apparatus is shown in Figure 1. It allows electrolysis of water with collection of hydrogen and oxygen together. It is made as follows:
1. Cut the stem of a pipet (1mL-stem type) so that about 0.5 cm of the stem remains. 2. Push (while twisting) the floral wires through the top of the bulb and out again as shown in Figure 1B (the further down the wires protrude from the bulb the more water will be electrolyzed). Make the holes as small as possible as the pipet should remain water and gas tight. If the floral wire has blunt ends, cut a diagonal at one end of the wire with a wire cutter before pushing it through the pipet. The pipet should not be sealed as water is forced out when the gases are produced. The wires must not be in contact with each other.

Figure 1. Apparatus for the electrolysis of water with collection of oxygen and hydrogen together (bromothymol blue was added to the solution). (A) How to hold the apparatus: reaction starts when the wires are touched to the battery. (B) A close-up showing the gas development and changes of indicator color (solution color changes from green in A to blue and yellow in B; photo Roar hlander). A B

Figure 2. Apparatus for the electrolysis of water with separate collection of oxygen and hydrogen (bromothymol blue was added to the solution). (A) Shows one-hand grip of the apparatus (two hands are more stable) before the electrolysis has started. (B) A close-up illustrating the gas volumes, changes of indicator color, and a stand of floral wire (color changes from green in A to blue at the negative electrode and yellow at the positive electrode; photo Roar hlander).

www.JCE.DivCHED.org

Vol. 81 No. 9 September 2004

Journal of Chemical Education

1337

In the Laboratory 3. Bend the wires 90 degrees above the bulb (see Figure 1A). 4. Turn the pipet upside down and fill it with saturated Na2SO4 solution (it works well and is safe) and possibly an indicator (e.g., bromothymol blue) by using another pipet. Do not try to suck up the solution. Put a petri dish or another container under the open end of the pipet, into which the Na2SO4 solution can run when the gases produced force the liquid out. 5. Connect the floral wires to a battery, preferably 9 V. The electrolysis starts immediately, the color changes (as a result of the pH changes at the electrodes) and gas production can be observed. The electrolysis will continue until the water is at the level where the floral wires exit the pipet. Thus a drop of the solution remains in the bulb conveniently sealing the gas inside. 6. Move the pipet near a flame and squeeze the bulb gently. A surprisingly sharp pop will be heard. (You have probably never made a more favorable ratio of hydrogen and oxygen!) This actually surprises the students considering the tiny quantity of gas mixture collected. This experiment is an immediate winner and is promptly adopted for use in schools. In our experience even the least handy instructor will succeed immediately. The apparatus described next should, for pedagogical reasons, be made first as no student is inclined to listen after the first pop is heard. 4. Turn the pipets, so that the open ends are immersed into a solution of similar composition and hold them next to each other (Figure 2). 5. Connect the floral wires directly to a battery, preferably 9 V (Figure 2A). In the classroom let the students work in pairs, one holding the two pipets in the solution, the other keeping the wires in contact with the battery poles. The electrolysis starts immediately and gas bubbles and color changes (if indicator has been added) can be observed. 6. Verify the gases produced, if desired.

The stand of floral wire (as shown in Figure 2B) is made by bending (i) one end of the floral wire around two pens (items of similar diameter) to allow for two pipets to be held and (ii) the other end around an appropriately sized cylinder, for example, a vitamin jar. It is easier to make these two bends in one plane before finally bending the stand into the shape shown in Figure 2B. Alternatively hold the pipets in one hand and the wires onto the battery with the other hand (Figure 2A shows a one-handed grip). In the classroom let the students work in pairs as described above. Discussion The hydrogen ions and oxygen that develop during the electrolysis at the positive electrode result in a slight reaction with the iron in the wire. This is a minor problem for the gas production and can be ignored. However, some students will spot this, which advantageously allows a comment on conditions favoring the corrosion of iron. Information on this can be found in a standard general chemistry book (for example ref 8 ). To avoid corrosion a dilute solution of NaOH can be used as a means of ion transport, but this demands safety precautions and excludes the use of an acidbase indicator, which is very instructive. Even electrodes of copper, welding steel, and graphite from a normal school pencil are attacked at the positive electrode when a neutral salt (e.g., Na2SO4) is used, thus we prefer the use of cheap floral wire. Acknowledgment POE is grateful for financial support from the County of Nord-Trndelag enabling him to work at the School Laboratory for Mathematics, Science, and Technology, Norwegian University of Science and Technology. Literature Cited
1. Suzuki, C. J. Chem. Educ. 1995, 72, 912. 2. Skinner, J. Microscale Chemistry, Experiments in Miniature; The Royal Society of Chemistry: London, 1997; pp 1213. 3. Ciardullo, C. V., C. M. Micro Action Chemistry, 2 ed.; Flinn Scientific: Batavia, IL, 1992; Vol.1, pp 6768. 4. Heideman, S. J. Chem. Educ. 1986, 63, 809. 5. Skinner, J. F. J. Chem. Educ. 1981, 58, 1017 6. Zhou, R. E. J. Chem. Educ. 1996, 73, 786. 7. Kelsh, D. J. J. Chem. Educ. 1981, 62, 154. 8. Zumdahl, S. S.; Zumdahl, S. A. Chemistry, 5th ed.; Houghton Mifflin: Boston, MA, 2000; pp 862866.

Apparatus for Electrolysis of Water with Separate Collection of Hydrogen and Oxygen The complete apparatus for the electrolysis of water with reasonably controlled separate collection of hydrogen and oxygen is shown in Figure 2. The apparatus is made as follows:
1. Cut off the stem of two pipets (3-mL stem) so that about 0.5 cm of each stem remains. 2. Push (while twisting) floral wires through the bulbs of the pipets so that they protrude slightly from the stem (1/21 cm) and bend the wires 90 degrees just above the bulb (Figure 2A). Try to make the holes small so that the pipets remain water and gas tight. If the floral wire is blunt, cut a diagonal at one end of the wire with a wire cutter before pushing it through the pipet. The gases will be produced at the protruding ends of the wires, therefore keep the wires in the center of the stems, so that the gases bubble into the bulbs and not outside. This can be adjusted when the electrolysis is started. It is also possible to form a spiral in the wire where it passes through the pipet stem, thus aligning it better, but this is not necessary. 3. Turn the pipets independently upside down and fill each with saturated Na2SO4 solution (it works well and is safe) and an indicator such as bromothymol blue. Adjusting the pH of the Na2SO4 solution until the bromothymol blue indicator turns green will help the students to understand the half-reaction at each electrode, because the pH changes can be observed. If you want to have the apparatus in the stand when doing the electrolysis, put the pipets (with the floral wires pushed in) into the stand before filling with saturated Na2SO4 solution.

1338

Journal of Chemical Education

Vol. 81 No. 9 September 2004

www.JCE.DivCHED.org