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Procedia - Social and Behavioral Sciences 59 (2012) 508 514

UKM Teaching and Learning Congress 2011

Organic chemistry practices for undergraduates using a small lab kit

Zuriati Zakariaa, Jalifah Latipa and Supawan Tantayanonb
b a School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia Department of Chemistry, Faculty of Science, Chulalongkorn University, Bangkok, Phayathai Road, 10330 Patumwan, Bangkok,, Thailand

Abstract The recent budget cuts in Universities in Malaysia affect the running of practical chemistry classes at undergraduate levels as purchase of equipment, glassware, chemicals and other consumables need to be reduced . The rising costs of chemicals also alleviate the problems in the acquisition of sufficient chemicals for the practical classes. Most lecturers give priority to equip their research laboratories as expected when Universiti Kebangsaan Malaysia was given the status of a research university by the Government of Malaysia. With such challenges, it is inevitable that the teaching of practical chemistry in the undergraduate are given less attention and the quality deteriorating since experiments are done by a group of 4 students as a measure to adjust to the availability of equipment and chemicals in the laboratory. Another necessary measure is to reduce the number of experiments conducted by the students. For organic chemistry practical classes, the small lab kit provided a solution for practices to run as usual and the learning of organic chemistry more effective. Students per group can be downsized to two per group to encourage everyone to be hands-on. The quality of learning can be enhanced and the quantity of chemicals can be reduced 10 times or even lower in some experiments. The students awareness to the conservation of environment can be manifested through the savings in the use of chemicals and water. Survey conducted among second year organic chemistry students showed that 80% of the students agreed that using the portable chemistry laboratory kit has enhanced their interest in learning chemistry. Among the reasons given is that the time taken to set up the experiments as well as conduct the experiments are short compared to the traditional methods. Experiments can be repeated easily. The types of experiments using common materials from daily life need to be developed to attract interest among students to learn chemistry. 2011 Published by Elsevier Ltd. Selection and/or peer reviewed under responsibility of the UKM Teaching and Learning 2011 Published by Elsevier Ltd. Selection and/or peer reviewed under responsibility of the UKM Teaching and Congress 2011. Learning Congress 2011
Keywords: Green chemistry; organic chemistry practices; small lab kit

1. Introduction Practical chemistry is essential in the learning of chemistry because chemistry is an experimental Science (Golinski, 1992). The teaching of first year Chemistry practicals at Universiti Kebangsaan Malaysia faces many

* Corresponding author. Tel.: +6-03-8921-3875; fax: +6-03-8921-5410 E-mail address: jali@ukm.my

1877-0428 2011 Published by Elsevier Ltd. Selection and/or peer reviewed under responsibility of the UKM Teaching and Learning Congress 2011 doi:10.1016/j.sbspro.2012.09.307

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problems due to the great number of students and the background of the students registered for the basic chemistry course at the Faculty of Science and Technology (FST). The students are from the Food Science, Chemistry, Biochemistry, and Microbiology programmes. In addition, students from Education Faculty (FE) as well as Allied Health Sciences Faculty (FAHS) also opt to take up the basic chemistry course. With an average of 300 students per semester, the limited number of laboratories further aggravates the problem of the running of chemistry practices. The variation in the fundamentals of basic chemistry among the students is another problem as many of them have never exposed to basic practical operations in the chemistry laboratory at schools. According to some students, practical chemistry is not a given priority in the upper secondary schools as it is not compulsory for students to take the practical exams. Some teachers use the allotted practical classes with normal chemistry classes as a measure to improve the overall grades of the examination results. There are cases where students are requested to copy notes on practices to familiarize themselves with laboratory methods. Other teachers demonstrate some experiments in front of the class with non-participatory students. The students interest in chemistry is diminished as they have the perception that the use of chemicals is dangerous and it is very difficult to conduct chemistry experiments. The learning environment for practical classes for chemistry is not attractive as the students conduct the experiments in groups and require a long time to complete the experiments. In some cases, it takes 3 hours and the students find it tiresome and boring. At the school levels, microscale chemistry has been introduced in many countries such as England, USA, China, India and Africa (Bradley 1999, Huang 2007, Sane et al. 1991, Singh 1999; 2000, Skinner 1999). The main concept is to use chemicals in droplets to observe a reaction. The experiments can be done hands-on by each individual which encourage the students to try as well as experience in chemistry. As only small amount is used, the chemicals are affordable and less dangerous to the students. The disposal of chemicals is less costly and less chemicals are released to the environment. The idea of microscale chemistry is popular and many countries set up microscale centres to encourage schools and universities to adopt the microscale practicals. Mashita et al. (2009) have transformed the chemistry practical experiments conducted at Form 4 and Form 5 levels in Malaysian schools from the traditional to microscale, but the Ministry of Education has yet to give approval before it can be implemented at all the schools in Malaysia. Microscale chemistry can potentially be developed at the undergraduate level. One of the driving factors would be the effect of budget cuts experienced by universities due to the world economic downturn and, as a result, the purchase of laboratory equipments and chemicals are also affected. Another challenge to the running of practicals in universities is that lecturers involved in proctoring the laboratories are not given the recognition as it is not considered in the key performance index in their career development. There is little effort to solve the budget issue by looking for alternative cheaper experiments to run. Instead, the easy solution is to increase the number of students per group from 4 to more and to reduce the number of experiments per semester. This practice will result in producing graduates who are less competent in laboratory techniques. With the status of Universiti Kebangsaan Malaysia as a research university, academic staff tends to give more attention to equip the research laboratories. Practical chemistry for undergraduates is essential as this is the stage where the chemistry students can improved their laboratory skills in order to be more prepared for their work as analytical chemists or as researchers in postgraduate studies. As such, the microscale approach can be used to solve the problem in improving the quality of organic chemistry at Universiti Kebangsaan Malaysia. In the microscale technique introduced by Bradley (1999), plastics well plates called the comboplates were used as the main tool because the materials are light, durable and cheap (Figure 1). Successful experiments using the comboplates were titration, qualitative analysis of inorganic compounds, reduction reactions, oxidation and electrolysis. However, the comboplate is not suitable for organic chemistry experiments at the university undergraduate level because plastics cannot withstand organic solvents used in many of the experiments. Futhermore, most basic organic chemistry operations such as distillation and reflux require heating, which is not possible for the comboplates. A good approach would be to use the small lab kit developed by one of the authors (ST) in Chulalongkorn University. All the glassware and apparatus are packed in a box and experiments can be carried out in an ordinary classroom provided that there is a power supply. The small lab kit (Figure 2) contains all important glassware including a heating tool, thermometer, filtration apparatus, a water pump and other required accessories, for examples, lab stand and clamps, joint clips,

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and water hoses. The small lab b kit is recomm mended by UN NESCO (Tanta ayanon 2009) where the ma anual which contains about 30 experiments ar re published on nline.

Figu ure 1. Apparatus fo or microscale chem mistry used for scho ools

Figu ure 2. Small lab kit completed with heating h tool and oth her required accessories.

T The objective of o this study is to assess the students s respo onses in whethe er the learning g of chemistry i is enhanced by u using the smal ll lab kit in the e second year organic chemistry experimen nts. Second ye ear students we ere selected beca ause more of the students will be major ring in chemis stry and there will be conti inuity in using g the basic proc cesses in organ nic chemistry when w they have e to conduct an n academic rese earch in the thi ird year.

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2. Method About 20 sets of the small lab kits were purchased from Thailand. Around 120 students who registered for the organic practical class: STKK2022, were selected to conduct 7 experiments in groups of two, in 3 sections, as follows:Experiment 1: Sublimation of naphthalene from mothballs Experiment 2: Purification of liquids by distillation Experiment 3: Preparation of salycilic acid from Kwan Loong Ointment Experiment 4: Reaction of Aldol condensation Experiment 5: Extraction and identification of the essential oil of cloves Experiment 6: Separation of trimyristin from Nutmeg Experiment 7: Nitration of phenol on solid surface After conducting all the experiments, a questionnaire was distributed to the students. 3. Results and Discussion The portable organic laboratory kit is equipped with flasks, sublimation tube, heating tool, filtrating apparatus, retort stand, clips as well as a thermometer. All the equipments are easily accessed and set up as they are all kept in a box, which minimize movement of the students in the laboratory when they select glassware and apparatus to perform the experiments. In the case of the normal laboratory, students have to walk to different sections of the laboratories as the glassware and apparatus are stored according to each type, e.g. flasks are stored separately from the condensers. The hot plate completed with an aluminium heating block accessory was a perfect fit for the flask, therefore providing efficient heat exchange without the hassle of using a sand bath or a water bath. Setting up a distillation set, for example, takes only a few minutes as all the glassware, retort stand and clips contained in the box which are within reach. In addition, the aluminium heating block can accommodate both round bottom and conical bottom flasks, 5, 10 and 25 mL size, to suit the requirement of the given experiment. The use of chemicals requires a small quantity, that is, one gram scale or lower compared to a 20 gram scale which is often used by a group of students. Thus a 20 gram chemical used by 4-6 students can be used by 20 individual students to illustrate the minimization of costs whilst providing similar results in the experiments as well as a better quality of learning. In each experiment where a melting point measurement is required, the students can measure the melting point using the aluminium heating block provided. This will cut down the students time in queuing up to use the only commercial melting point apparatus provided in the normal second year chemistry laboratory practical. In the synthesis of salicylic acid, a common ointment normally found in a sundry shop was used as a starting material. The ointment, used for the relief of headache and stomachache, contains a mixture of methyl salicylate, eugenol, menthol and paraffin. In terms of cost, a bottle of 15 mL medicine costs RM5 or around 1.5 USD, where 20 students are able to use to obtain the expected product. Not only do the students learn about the hydrolysis of an ester to an acid, but at the same time, they are able to learn how to separate the neutral compounds from the acidic compounds. Furthermore, they are fascinated that the chemicals that they are dealing with have normally been used in the medicinal application. In an organic laboratory, a water source is always important as a continuous supply is necessary for the distillation and refluxing processes. The practical classes often have to be postponed because there is a water cut due to repairs or to save water during the dry weather. The reflux process sometimes needs water to be continuously flowing for 30 minutes where more than 50 L of water will be wasted. The small lab kit provides a water pump to avoid such usage. As little as 500 mL of water is used as the water is recycled back to the condenser. If the water is warm due to the hot weather, a few lumps of ice can be added to effectively cool the condenser and thus prevent organic vapours to be released in the room (Figure 3). In the fitrating process, a filtrating funnel is provided with a vacuum flask. Although a vacuum pump or water aspirator can be applied, the solutions can be filtered using a three-way pipette filler bulb to generate a vacuum

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and save energy or o water. This process p was su uccessfully carr ried out in the experiments o on preparation of salycilic acid d, the Aldol con ndensation as well w as the separation of trim myristin from nu utmeg.

Water recyc cling

ure 3. The reflux pr rocess with cooling g using recycling cool c water Figu

T Table 1 shows the feedback from f students who w have used d the small lab kit and their v views on wheth her the tools help p them to bett ter understand the concepts in organic ch hemistry. The questionnaire have been dis stributed to stud dents from the e Faculty of Sc cience and Technology (FST T), Faculty of f Education (FE) and Faculty ty of Allied Hea alth Sciences (F FAHS). It was found that 80. .4% of the stud dents agreed, 1 17.6 % did not agree and 1.96 6 % leave it unan nswered that microscale m che emistry using the t small lab kit k helps them m in understand ding the chemi istry better. The e majority of th he students wh ho agreed are from fr the Facult ty of Science a and Technolog gy, followed by y Faculty of Alli ied Health Sciences and Fa aculty of Educ cation. Univer rsiti Kebangsa aan Malaysia is the first un niversity to imp plement the usa age of the smal ll lab kit which h is well receiv ved by the stud dents. Initial results also show wed that the lear rning of the pra acticals is mor re effective wit th more studen nts performing the experimen ntal handson and the use of th he small lab ki it should be con ntinued. O Open questions were also in ncluded in the questionnaire as to determin ne the preferen nce to use of t the portable labo oratory for the practical chem mistry classes. Among A the reasons they gave e were as follow ws:i i. ii i. iii i. iv v. v v. vi i. vii i. viii i. ix x. Fast, apparatus were sm maller, easier to o handle A box wi ith a complete set, ready to ru un the experim ments Low cost t for chemicals s More attr ractive Disadvan ntage because yield y is small, but b reaction oc ccurred, should d continue. Less chem micals used, le ess time taken. Small, ea asy to use, less space required d. It is more e interesting Students have to be more careful. If not, n unsatisfied result is obtain ned, but experi iment can be re epeated.

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Table 1. Results from survey among second year organic chemistry students

FST 54

Agree 82 (80.4%) FAHS 18

FE 10

FST 4

Do not agree 18 (17.6%) FAHS 9

FE 5

FST 2

No answer 2 (1.96%) FAHS -

FE -

Overall 102 (100%) FST FAHS 60 27

FE 15

From the comments received, it is found that most of the outcome expected from the use of the small lab kit has been achieved. However, the students did not aware the use of the small lab kit and microscale chemistry on the laboratory safety as well as conservation of the environment aspects. Thus, the students awareness towards environment has not been effective in a way that they could not relate their activities with the macro effect of their environment. Thus, it is important that a briefing about the effect of using less amount of chemicals, using less energy as well as using recycled water for lab safety and environment must be given to the students before they carry out the experiments. From the interview with the laboratory assistants, they are in the opinion that with the implementation of the small lab kit, responsibility is given for the students to clean and keep the glassware in each box and they are less burdened in keeping glassware clean and stored at various places in the labs. The boxes can also be stacked neatly in the laboratories. They also noticed that there is a saving in the use of solvents, where in previous years, they had to buy 4 bottles of dichloromethane instead of only one bottle during the current study. They also observed that there were less glassware breakages when using the small lab kit. There is a potential to develop the small lab kit in Universiti Kebangsaan Malaysia to first year chemistry laboratory and inorganic laboratory courses for the second year. New experiments need to be introduced and for instilling environmental consciousness among students, green chemistry need to be emphasized. For the design of new experiments in green chemistry, chemicals are used in a smaller amount, safer, and involved minimum steps in synthesising the target molecules. If possible, household chemicals can be used for the students to realize the connection of chemistry to daily living. 4. Conclusion The second year practical chemistry classes conducted at Universiti Kebangsaan Malaysia using the small lab kit has succeeded to stir interest of the students to learn chemistry. The small lab kit is safe and easy to carry. Savings in time, water and chemicals were found during the implementation of the small lab kit which at the same time makes learning organic chemistry fun for the students. This practice can be applied to other countries that face the similar problems as well. Experiments should be designed so that the small lab kit can be used at all levels of undergraduate studies. It is also a great challenge for schools and universities to protect their students and staffs from chemical risk as well as to save chemicals, energy, and environment by transforming their traditional laboratories to microscale or small scale ones. Acknowledgement We would like to thank Universiti Kebangsaan Malaysia for providing the research grant (UKM-PTS-013-2010.). References
Bradley, J. D. (1999). Hands-on practical chemistry for all. Pure Applied Chemistry, 71(5), 817 823. Golinski, J. (1999). Science as public culture: chemistry and enlightenment in Britain (pp. 1760-1820). USA: Cambridge University Press. Huang Z. (2007). Study on Micro-organic Chemistry Experiment Teaching. Journal of Guangxi University for Nationalities, 2-6. Mashita, A., Norita, M. & Zurida, I. (2009). The effect of an individualized laboratory approach through microscale chemistry experimentation on students understanding of chemistry concepts, motivation and attitudes. Chemistry Education Research and Practice, 10, 53 - 61. Sane K. V. & West D. C. (1991). Low Cost Chemical Instrumentation. Delhi:University of Delhi

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Singh, M. M., Szafran, Z. & Pike R. M. (1999). Microscale Chemistry and Green Chemistry: Complementary Pedagogies. Journal of Chemical Education, 76(12), 1684. Singh, M.M., McGowan C. B., Szafran Z. & Pike R. M. (2000). A Comparative Study of Microscale and Standard Burets. Journal of Chemical Education, 77 (5), 625 Skinner, J. (1999). Microscale Chemistry. London: The Royal Society of Chemistry. Tantayanon, S. (2009). Small Scale Laboratory: Organic Chemistry at University Level. http://www.unesco.org/science/doc/Organi_chem_220709_FINAL.pdf Retrieved December 1, 2010, from