A STUDY OF THE IMPACT OF MICROSCALE/ SMALL SCALE CHEMISTRY .
A STUDY OF THE IMPACT OF MICROSCALE/SMALL SCALE CHEMISTRY EXPERIMENTS ONTHE ATTITUDES AND ACHIEVEMENTS OFTHE FIRST YEAR STUDENTS IN GLASGOWUNIVERSITYBYMOHAMMAD IQBAL KHANA thesis submitted in part fulfilm ent of therequirements for the degree of M.Sc. in ScienceEducation (Chemistry) of the University of GlasgowScotland U.K.CENTRE FOR SCIENCE EDUCATION JANUARY 1996
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CONTENTSABSTRACTCHAPTER ONEIntroduction to MicroscaleChemistry LaboratoriesCHAPTER TWOA Review of the History of ChemistryLaboratory Work2.1Practical work in the early eighteenth century2.2Practical work in the late eighteenthand early nineteenth century2.3H istory o f practical laboratories inthe UK2.4Practical work in the firs t h a lf o f thetwentieth century2.5Practical work in the second h alf o f thetwentieth century2.5.1 1950’s and 1960’s2.5.2 1970’s and 1980’s
2.6Aims and objectives of practical work162.7Scientific enquiry182.8Learning through practical work23CHAPTER THREEConversion of a Chemistry Laboratoryto Small Scale263.1Introduction263.2Advantages o f a small scale laboratory273.2.1 Small scale impact on wastegeneration273.2.2 Laboratory safety283.2.3 Use of wider variety of reagents293.2.4 Laboratory efficiency293.2.5 Reduction in storage space293.2.6 Students performance in the laboratory303.3Small scale organic laboratory323.4Small scale organic equipmentand techniques333.5Small scale general inorganic chemistry333.6Equipment in small scale general inorganicchem istry equipment and techniques34
CHAPTER FOURSmall Scale Organic Chemistry as a newelement in the Laboratory for FirstYear Chemistry University Students354.1The aims o f the m odification o f chemistry-Iorganic experiments into small scale354.2Small scale equipment354.2.1 Equipment364.2.2 Small scale techniques44Procedure used in the small scale organiclaboratory544.3.1 The sample selected544.3.2 Experiments selected544.3.3 Small scale manual55Measurement o f the attitudes o f studentstowards small scale organic experiments554.4.1 The design of the questionnaire554.4.2 Student responses584.5The researcher's views aboutstudents' responses594.6Opinion o f demonstrators aboutsmall scale experiments604.7The researcher's views aboutdemonstrators' responses624.34.4
4.8Summary62CHAPTER FIVEModification of General Chemistry-1Inorganic Experiments to Small Scale645.1Introduction645.2Aims of the m odification o f generalchem istry-1 inorganic experimentsinto small scale645.3Apparatus used655.45.3.1 Transparent polythene sheet655.3.2 Pasteur pipette665.3.3 Beral pipettes675.3.4 Small test tubes675.3.5 Well -plate67Practical procedures used in theinorganic small scale laboratory' 5.4.1 Experiments selected68685.4.2 Modification of the manual685.4.3 The sample of the students selected72for the study5.4.4 The empirical work735.4.5 Points for discussion745.4.6 Results obtained from all75general chemistry students5.4.7 Summary of the findings79
5.5Student attitudes towards small scaleexperiments805.5.1 The questionnaire design805.5.2 The students attitudes towards82small scale experiments5.5.3 Student attitudes related to their previous84qualifications5.6Summary85CHAPTER SIXConclusions and Discussions866.1Problems confronted by the research866.2The findings obtained from this study876.2.1 The organic microscale findings886.2.2 The general inorganic microscale findings906.2.3 Findings obtained from students’92achievements in general inorganic microscaleexperiments6.3Suggestions fo r fu rth e r researchREFERENCESAPPENDICES9395
ACKNOWLEDGEMENTSI w o u ld lik e to express m y sincere g ra titu d e to Prof. A. H.Jo h n sto n e fo r h is s u p e rv is io n , a dvice , g u id a n ce andencouragem ent d uring m y studies. It was his help, and kindnessw hich helped me in the com pletion o f m y study.I w ou ld also lik e to thank Dr. Fakhir Al-Naeme fo r his help,guidance, encouragement, suggestions, participation the laboratoryand discussion o f the m aterial that has been introduced.I am g ra te fu l to the M in istry o f Education, G overnm ent o f theIslam ic Republic o f Pakistan fo r th e ir fin a n cia l support w ith o u tw hich this study w ould have been impossible.I am also gra te ful to m y parents, m y w ife and m y ch ild re n whoshowed great patience during the period o f this study when I wasaway from them.F in a lly I w ould lik e to thank m y colleagues at the Centre fo rScience Education, Glasgow U niversity fo r th e ir frie n d sh ip andsupport during m y stay at the Centre.
1ABSTRACTThis study is in te n d e d to measure the a ttitu d e s o f F irst YearChem istry Students and Demonstrators at Glasgow U niversity, andalso the im pact o f microscale experiments on the achievements o fstudents.In 1993-94, tw o experim ents fro m the F irs t Year O rganicC hem istry Course were selected fo r m o d ifica tio n to Small Scale.Small Scale apparatus and techniques were used by the students.Q uestionnaires were devised fo r the students and dem onstratorsfo r the measurement o f th e ir attitudes tow ard d iffe re n t aspects o fSmall Scale Experiments.In 1994-95 three experim ents (p a rtia lly o r fu lly ) fro m the F irstYear Inorganic General Chem istry were selected fo r m o d ifica tio nto Small Scale. This year students used the Small Scale apparatusand techniques w ith m odified w ritte n in stru ctio n s in w hich theprocedures o f experim ents were fu lly explained.A questionnaire to measure the a ttitu de s o f students tow ardInorganic Small Scale Experiments was designed in the same year.M oreover, the achievem ents o f students in the Sm all ScaleExperiments and Norm al Scale Experiments were also studied.This study revealed th a t students lik e d Small Scale experim entsand w ould p re fe r them to the N orm al Scale, p ro vid e d th a t thefo llo w in g two opportunities are given to them:a.the students are fu lly briefed about the usefulness o f theSmall Scale experiments;b.the d iffe re n t techniques used in these experim ents arefu lly explained to students before starting any experim ents.
2CHAPTER ONEIntroduction to Microscale/Small ScaleLaboratoriesP ractical w o rk in a science subject plays im p o rta n t roles byconfirm ing the theory w hich had already been taught in lecturesand as the core o f the learning processes o f in ve stig a tio n andin q u iry .In recent years the subject o f chemical waste has become a m ajorconcern everyw here. Disposal o f th is waste is n o t o n ly ve ryexpensive, b u t it is becoming increasingly m ore d iffic u lt to fin dplaces w illin g to accept it. In an a ttem pt to help alle via te thisp ro ble m , a tre n d is increasing to downscale the am ount o fchem icals used in c h e m is try la b o ra to rie s b y in s titu tin gm icroscale/sm all scale operations. This conversion has educationaladvantages as w ell. It teaches the students to be precise in th e irm easurem ents and v e ry ca re fu l w ith th e ir e q u ip m e n t andproducts.A significant change is taking place in today’s chem istry lab. Thisis the steady increase in a doption o f the m icro chem ical labconcept at secondary and post secondary levels. The m icroscaleapproach is being adopted to help solve a num ber o f problem s.Cheronis and Stein in 1935 p oin ted o ut the techniques such asfiltra tio n , d is tilla tio n and evaporation are general ones, w hichwere recommended on semi-microscale fo r teaching(l).In 1945 Cheronis and his co-workers published parts V I and V IIo f th e ir series "the use o f Sem i-m icro Techniques in organicc h e m is try "(2»3) w ith a lite ra tu re survey going back to 1919.There is n o t a little doubt th a t Cheronis was larg ely responsible
3fo r the in itia l g ro w th o f in te re st in the teaching o f organicch em istry b y sm all scale m ethods. A p a rt fro m his papers, hisbooks(4) inspired others to try sm all scale techniques.One w ho was in sp ire d was K line, Professor E m eritus a t theU nive rsity o f Connecticut. Kline s till professionally active, makesthe follow ing statem ent in the preface o f his book(5).“ In September, 1941, D r. N icholas D. C heronis described hisexperience w ith sem i-m icro procedures a t the A tla n tic C itym eeting o f the Am erican Chemical Society. He e xhibited some o fthe apparatus used and asked fo r in stru c to rs to vo lu n te e r totesting some o f the procedures w hich he had devised and w hichwere described in m im eographed m anual w hich he had prepared” .Kline (an expert glass maker) constructed apparatus and assignedit to 8 students. By the summer 1942, a ll firs t year students wereequipped w ith sm all scale glass ware. A ccording to K line therewas a dram atic rise in student intake a fte r the end o f the war.Supplies and bench space was lim ite d (6).In 1951, G riffin and George introduced the M acroid Sem i-m icroO rganic Set. Soon a fte r, another su p p lie r m arketed a s lig h tlyd iffe re n t set.Teaching loads were horrendous, b u t tim e was fo u n d to w ork onthe m anuscript o f a sm all, precollege organic text. The e ffo rt ,naive by m odem standards, attem pted to show th a t the pra cticalcu rricu lu m is best served by a com bination o f m acro and semim icro techniques(7).In the educational lab o ra to ry setting, the re d u ctio n in scale (toapproxim ately 50-150 mg o f solids and 50-2000 nL o f liq u id s ) isknow n as microscale chem istry (IUPAC uses the term “ Small Scalechem istry” ).
4In the educational la b o ra to ry setting, the re d u ctio n in scale (toapproxim ately 50-150 mg o f solids and 50-2000 \iL o f liq u id s ) isknow n as m icroscale chem istry (IUPAC uses the term “ Small Scalechem istry” ).The a p p lic a tio n o f th is concept in in d u s tria l research anddevelopm ent laboratories o f today is also a viable option. Notably,pharm aceutical research laboratories have w orked at this level fo ryearsW .P rior to 1960, m icro-techniques were h ig h ly delicate, tedious andspecialised, and was used m ain ly in n atu ral p ro d u ct research andin graduate school studies. In was n o t u n til the 1980’s whene n viro n m e n ta l concerns had risen to the fo re fro n t and thee le c tro n ic m illig ra m balance became a va ila b le th a t usingm icroscale experim ents at the in tro d u c to ry level o f in s tru c tio nbecame a re a lity W .M icroscale ch e m is try was developed fo r the in tro d u c to ryla b o ra to ry b y M ayo and B utcher (fro m B ow doin C ollege,B runsw ick, M aine, USA) and Pike (M e rrim a ck College, N o rthAndover, Massachusetts, USA)( ).The necessary techniques and m aterials were developed fo r theorganic chem istry lab o ra to ry in 1982-3. The firs t teaching testsoccurred at Browdoin and M errim ack colleges in 1983. The testsproved to be h ig h ly successful w ith the sophomore level studentswho ra p id ly adapted to the new techniques. P re lim in a ry resultswere reported at the national meeting o f the Am erican ChemicalSociety in 1984(8) and were published in the Journal o f ChemicalE ducation ).In 1985 (9,10) a series o f articles appeared in the Journal o fChem ical Education. One o f the m ajor reasons fo r the in itia lin tro d u c tio n o f m icroscale e xp e rim e n ts ) was to decrease theq u a n tity o f p o te n tia lly hazardous organic solvents in the a ir in
5q u a n tity o f p o te n tia lly hazardous organic solvents in the a ir inorganic chem istry laboratories toward the levels recommended bythe O ccupational Safety and Health A d m in is tra tio n 11). This goalis m ore ce rta in ly attainable when reactions are ca rried o u t w ithm illilitre s o f solvents ra th e r than w ith hundreds o f m illilitre s asu s u a lly done p re vio u sly. C onversion to m icroscale has alsoprovided m any other benefits, both financial and educational.The m icroscale experim ents th a t have been developed in organicch e m istry are m a in ly synthetic in nature since m uch o f thela b o ra to ry w o rk in organic chem istry involves syntheses. Incontrast the d ive rsity required o f general chem istry experim entsis m uch greater, since this course m aterial ranges fro m descriptivech e m istry to physiochem ical p rin cip le s. A lth o u g h q u a lita tiv eexperim ents can be used to present the basis o f chem icalreactions, q uantitative activities are often needed to illu s tra te thep rin cip le s in h e re n t to such topics as stoichiom etry, e q u ilib ria ,therm odynam ics, kinetics and electrochem istry. F ortunately botho f these needs can be m et by m icroscale techniques. In fa ct theease and speed w ith w hich microscale experim ents can be done,besides sm all quantities o f m aterials required fo r them , make itpossible fo r students to ca rry o ut m ore tria ls u n d e r a greaterrange o f conditions.The real inn o vato r o f microscale techniques in general chem istrywas Thom pson (1990)(12) o f the U niversity o f Colorado. In 1977he m od ified general chem istry experim ents so th a t o n ly drop sizequantities were required. These were m ixed on a plastic sheet andthe reaction i f any, was observed by means o f a m agnifying glass.Thom pson also realised th a t plastic m edical science equipm entcould have a pote n tial fo r microscale experiments.A lth o u g h Thom pson's idio syn cra tic la b o ra to ry m anual gainedsome fo llo w in g , it was M ills and H am pton (1 9 9 1 )(13) whobro ad e ne d the appeal o f p la s tic w are fo r in tro d u c to ry
6co lle g e /u n ive rsity chem istry experim ents in the US. A t about thesame tim e the im petus fo r the use o f m icroscale techniques ath ig h school leve l came fro m a w orkshop h e ld a t P rincetonU n ive rsity (1 9 8 7 )(14). Since then the leaders in school a ctivitieshave been M aunch and Russo (1989, 1990 and 1 99 2)(15»16) inthe US, and Slater (1 9 9 4 )(l7) in Canada. A series o f m icroscaleexperim ents have appeared in the N orth Am erican H igh SchoolC hem istry Magazine, Chem. 13 News.The fir s t m icroscale ch em istry textbook, M icroscale O rganicL a b o ra to ry appeared in 1986(18)* M any others have fo llo w edsince then.This w o rk d ire c tly led to the grow th o f a m in i-in d u s try in thearea o f m icroscale chem istry, w ith at least seven glass companiesm anufacturing microscale kits and glassware.Szafran, Pike and Singh (at M errim ack College) investigated theim plem entation o f microscale techniques in inorganic chem istry.There had been an increasing tendency tow ard e lim in a tio n o fla b o ra to rie s in inorganic chem istry, due to excessive cost o fchemicals and equipm ent, the d iffic u lty o f perform ing interestingexperim ents in a safe and e fficie n t m anner, and the problem s o fwaste disposal. By converting the ino rga nic la b o ra to ry to them icroscale level, it became possible to expand the range o fe xp e rim e n ta l coverage to in clu d e such im p o rta n t areas aso rg anom etallic chem istry o f the heavy m etals, catalysis, andbioinorganic chem istry(19). The text book o f M icroscale InorganicC hem istry: A Comprehensive Laboratory Experience appeared in1 9 9 l(20). F urther w ork by Singh, Szafran, Pike, Foster and othershas expanded the role o f m icroscale chem istry to the general(in tro d u cto ry) chem istry laboratory(2 ).The use o f m icroscale techniques in general ch e m istry is n o tlim ite d to the laboratory, since microscale experim ents conductedon transparent acrylic spot plates are re a d ily visible, even in large
7lecture halls, when shown on an overhead p ro je cto r (reactions inw hich precipitates are form ed are less satisfactory than those th atinvolve colour changes o r evolution o f gases). This should help tob rin g lecture dem onstration w ith in the reach o f a ll teachers.A large num ber o f publications on m icroscale experim ents andtechniques have appeared in the Journal o f Chemical Educationd u rin g the last decade.
8CHAPTER TWOA Review of the History of Chemistry LaboratoryWork2.1 Practical work in the early eighteenthcenturyIn the early eighteenth ce ntu ry chem istry was ta ug h t o n ly bylectures. It was fe lt at la te r stages o f the same century th a t somepractical w ork should be introduced in the fo rm o f dem onstrationsin lectures. In 1748 at the U niversity o f Glasgow, W illia m C ullenand Joseph Black included some dem onstrations in th e ir lectures.O therwise the p ra ctica l w ork was done o n ly b y assistants anddem onstrators in the laboratories.A t the end o f the eighteenth century lab o ra to ry based m ethods o fteaching gained ra p id ly in im portance fo r research schools inchem istry. Therefore, in d iv id u a l practical w ork was accepted asan essential p a rt o f the u n ive rsity chem istry course. U n til thenla b o ra to ry w ork had been an isolated a c tiv ity w ith little support;some o f i t p riv a te instead o f in s titu tio n a l and o u tw ith thecu rricu lu m i.e. it was n ot com pulsory.A t th is tim e p ra ctica l w ork played a great su pp ortive ro le fo rco nfirm in g the theory w hich had already been taught in lectures.The experim ental procedures were p rin te d along w ith details inthe te xt book, and any help required during this period was givenb y w ell trained s t a f f ( 2 1 » 2 2 ) #
92.2Practical work in the late eighteenth and earlynineteenth centurySystem atic la b o ra to ry w ork by students began a t the end o feighteenth century. In 1795(21), the Ecole Polytechnique o f Paris(France) introduced laboratory w ork. In 1806(23) p ra ctical w orkwas o ffe re d at G ottingen U nive rsity in G erm any b y F rie d ric hStrom eyer who believed th a t chem istry could o n ly be learnedth ro u gh la b o ra to ry practice and th a t students m ust be given ano p p o rtu n ity to carry o u t analysis on th e ir own.In S tockholm (Sweden) a t the C ollegium M edium , Berzeliusopened his own private teaching lab o ra to ry fo r a few students in1 8 0 8 (21), fir s t situated in H isinger's house and then in theSwedish Academ y o f Sciences, attended b y his m ore fam ouspupils.In the beginning o f nineteenth century, in D u b lin U niversity, Dr.Perceval included practical w ork in his lectures. D uring the periodo f 1810 u n til 1826 the firs t lab o ra to ry course in chem istry waso ffe re d in the U.S.A by W illia m James MacNeven, professor o fchem istry in the College o f Physicians and Surgeons o f New York,where students had an o p p o rtu n ity to practise the techniques,processes and procedures o f chem istry(24).2.3 History of practical laboratories in the UKThe fir s t teaching la b o ra to ry in a B ritis h u n iv e rs ity wasestablished by Thomas Thomson in the U nive rsity o f E dinburghin 1807. In 1819 he in tro d u c e d i t to the U n iv e rs ity o fG lasgow 3). Thomson took up a teaching post in the U niversity o fGlasgow, where he trie d to establish a research school based onhis teaching la b o ra to ry(2 1 ). In d u s tria l pressure fo r tra in e dchem ists had grow n substantially, p a rtic u la rly fo r analysts tom a in ta in q u a lity c o n tro l in in d u s try as w e ll as fo r research
10chem ists. P ra ctica l tra in in g b
Chemistry Students and Demonstrators at Glasgow University, and also the impact of microscale experiments on the achievements of students. In 1993-94, two experiments from the First Year Organic Chemistry Course were selected for modification to Small Scale. Small Scale apparatus and techniques were used by the students.
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