ISL MINGGU 13

MICROSCALE CHEMISTRY

Microscale Chemistry (often referred to as Small-Scale Chemistry, in German:Chemie im Mikromastabde:Chemie im Mikromastab) is not only an analytical method, but also a teaching method widely used at school and at university levels, working with small quantities ofchemical substances. While much of traditional chemistry teaching centers on multi-gramme preparations, milligrammes of substances are sufficient for Microscale Chemistry. In Universities modern and expensive lab glass ware is used and modern methods for detection and characterization of the produced substances are very common. In schools and in many countries of the Southern hemisphere small-scale working takes place with low-cost and even no-cost material. There has always been a place for small-scale working in qualitative analysis, but the new developments can encompass much of chemistry a student is likely to meet.

History

There are two main strands of the modern approach. One is based on the idea that many of the experiments associated with General Chemistry (acids and bases, oxidation and reduction, electrochemistry, etc.) can be carried out in equipment much simpler (injection bottles, dropper bottles, syringes, wellplates, plastic pipettes) and therefore cheaper than the traditional glassware in a laboratory, thus enabling the expansion of the laboratory experiences of students in large classes and to introduce laboratory work into institutions too poorly equipped for standard-type work. Pioneering development in this area was carried out by Egerton C. Grey (1928),[1] Mahmoud K. ElMarsafy (1989)[2] in Egypt, Stephen Thompson in the US[3] and others. A further application of these ideas was the devising by Bradley of the Radmaste kits[4] in South Africa, designed to make effective chemical experiments possible in developing countries in schools that lack the technical services (electricity, running water) taken for granted in many places. The other strand is the introduction of this approach into synthetic work, mainly in organic chemistry. Here the crucial breakthrough was

achieved by Mayo, Pike and Butcher[5] and by Williamson[6] who demonstrated that inexperienced students were able to carry out organic syntheses on a few tens of milligrams, a skill previously thought to require years of training and experience. These approaches were accompanied by the introduction of some specialised equipment, which was subsequently simplified by Breuer without great loss of versatility.[7] There is a great deal of published material available to help in the introduction of such a scheme, providing advice on choice of equipment, techniques and preparative experiments and the flow of such material is continuing through a column in the Journal of Chemical education called The Microscale Laboratory that has been running for many years. Scaling down experiments, when combined with modern projection technology, opened up the possibility of carrying out lecture demonstrations of the most hazardous kind in total safety.[8] The approach has been adopted world wide. It has become a major presence on the educational scene in the US, it is used to a lesser extent in the UK and it is used in many countries in institutions with staff who are enthusiastic about it.

Advantages of Microscale Chemistry

Saves time for preparation and clear away Reduces waste at the source More safety Lower costs for chemical substances and equipment Smaller storage area Reduced reliance on intensive ventilation systems Pleasant working atmosphere[9] Shorter reaction times More time for evaluation and communication.

ISL MINGGU 13

MICROSCALE CHEMISTRY IN UNDERGRADUATE TEACHING LABORATORIES

Applicable Regulations Overview of Procedure Waste Minimization Procedure Known Limitations Safety & Health Precautions/Personal Protective Equipment Benefits Disadvantages Project Related Costs

Summary: Beginning in 1989, the University of Michigan (U-M) Department of Chemistry began implementing microscale chemistry techniques in the undergraduate teaching laboratories. Microscale laboratory experiments reduce the amount of chemicals necessary to perform undergraduate chemistry experiments to a fraction of what was historically used. In addition to decreasing the quantities of chemicals purchased and amount of chemical waste generated, microscale techniques have proven to be safer and more cost effective than traditional experiments.

Applicable Regulations 40 CFR Parts 260-268. State of Michigan Act 451 Part 111. Overview of Procedure Microscale chemistry is a pollution prevention method that decreases the amount of chemical waste generated during laboratory experiments. This concept was first introduced by chemistry professors at Bowdoin College in Brunswick, Maine. Standard chemistry procedures are re-written for individual experiments and specialized microscale equipment is utilized to perform the work. In some cases, the amount of a particular chemical needed for an experiment has been decreased by as much as 99 percent. The U-M has implemented microscale chemistry in its undergraduate inorganic and organic teaching laboratories.

Waste Minimization Procedure Due to the number of laboratory experiments that have been converted to microscale, it is not practical to detail the individual procedures. However, the following table presents a before and after comparison of the amounts of chemicals used, as well as the cost of those chemicals, for an Aldol Condensation experiment. These quantities represent the per student amounts. Micro Micro Traditional Traditional Quantity Quantity Quantity Chemical (gm or Chemical (gm or ml) Cost ml) Cost 5 $0.03 0.073 <$0.01 60 $0.60 4.1 $0.04 5.3 $0.81 0.212 $0.03 5 $0.19 0.24 $0.01 5 $0.71 0.2 $0.03 5 $0.36 0.2 $0.01 5 5 5 Total Cost* $0.77 $0.47 $1.27 $5.21 0.2 0.2 0.2 Total Cost* $0.03 $0.02 $0.05 $0.23

Chemical Acetone Ethanol Benzaldehyde Sodium Hydroxide p-Anisaldehyde p-Chlorobenzaldehyde 3,4Dimethoxybenzaldehyde 2-Furaldehyde 1-Naphthaldehyde

*All costs were obtained from the 1994/95 Aldrich catalogue. Known Limitations Due to the small quantities of materials used, it may not be possible to have enough "product" left at the end of an experiment to run a series of experiments. For example, experiment #1 might have generated a product that was used to run experiment #2, etc. However, in the typical teaching laboratory, the "products" typically have no value and are disposed of as waste. Safety & Health Precautions/Personal Protective Equipment Follow all applicable safety and health protocols and regulations as established by your institution.

Benefits Microscale techniques in the laboratory:

Reduce chemical waste produced at the source; Improve laboratory safety by decreasing the potential for exposure to chemicals and reducing the potential for fire/explosion hazards; Improve air quality due to the greatly reduced volumes of solvents and other volatile substances used; Reduce laboratory costs for chemical purchase and disposal; Reduce the time required to perform experiments due to shorter chemical reaction times; Decrease the amount of storage space necessary for chemicals; and Encourage students to think about waste minimization.

Disadvantages To begin teaching microscale techniques in the laboratory, the institution must purchase microscale equipment and textbooks. However, the costs can be recovered in a relatively short period of time due to savings realized on purchase and disposal costs of reduced quantities of chemicals. Project Related Costs The table below presents a per student comparison of traditional vs. micro chemical purchasing costs for the Chemistry 216 course at the U-M. The experiments were performed during the 1996 spring semester. All costs were taken from the 1994/95 Aldrich catalogue. Experiment Acetanilide Adol Condensation Sodium Borohydride Reduction Electrophilic Aromatic Substitution Diphenylacetylene Tetrapheynlcyclopentadienone Total Traditional Cost 0.46 $5.20 $0.16 $1.01 $0.99 $2.11 $9.93 Micro Cost $0.05 $0.23 $0.02 $0.02 $0.10 $0.08 $0.50

The purchasing cost of chemicals for performing microscale

experiments is 99.5 percent less than for traditional experiments. Disposal costs for the individual experiments were not calculated. However, the quantities of chemicals used for microscale experiments are typically less than one tenth the amount used in traditional macroscale experiments. Disposal costs should be reflective of this significant decrease.

Sumber link:
http://www.scienceinschool.org/2010/issue16/microscale http://www.p2000.umich.edu/chemical_waste/cw7.htm