JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY AUGUST 1993 VOL. 8 35N Conference Report Chemistry and Applied PittCon ’93 44th Pittsburgh Conference and Exposition on Analytical Spectroscopy March 8-1 2 Atlanta GA USA At the opening ceremony of this year’s PittCon as it is fondly known by all who attend Georgia’s Governor Zell Miller declared Georgia ‘an up and coming place to be for science’ and he predicted that Georgia would be a world class scientific research centre in the future. He also invited exhibitors and visitors to take some time out and enjoy Atlanta and ‘spend money-we need it!’. He was possibly thinking of the Olympic Games which Atlanta is hosting in 1996 when he extended those hospitable words. He could not have known that seven days later he would be adding Georgia to the list of 11 US states requesting federal aid after being hit by a Winter storm that stranded many of PittCon’s visitors for days and left them no choice but to stay and spend! PittCon had just wound down when the ‘Blizzard of ’93’ as it was dubbed in the US headlines struck the East coast with up to 12 feet of snow and hurricane-force winds closing most airports from Atlanta to Boston and turning most interstate highways into parking lots.PittCon is the largest exhibition and technical programme of its kind in the world and this year it attracted over 1000 exhibitors displaying over 5 miles of exhibits over 1800 oral pre- sentations in the form of symposia poster-sessions mini-meetings award addresses and short courses and 30000 visitors. In short a blizzard of activity shoe-horned into five days leaving every visitor exhausted and with the feeling that never was so much ground covered on the tip of the iceberg. The sheer size of the exhibition and technical programme limits the num- ber of US cities in which it can be housed and for the immediate future Chicago New Orleans and Atlanta are the only three slated.This year’s facili- ties at the Georgia World Congress Center were excellent and accommo- dated the exhibition in three halls and the technical programme in meeting rooms above. Considering the number of visitors the halls were not uncom- fortably overcrowded and the meeting rooms were spacious. The technical programme this year lacked lustre in its scope. PittCon usually presents a programme that strikes a balance between leading edge research and commercially viable wis- dom which attempts to cover many subjects ranging from the nitty gritty of precise analytical measurements through to the more topical concerns of all chemists with conscience. Con- spicuous by their absence were the plenary lectures-always the most popular and best attended-but one is promised for next year.However there was content aplenty for those willing to sift through the symposia carefully and there was en- tertainment. Some of this year’s speak- ers made courageous efforts to leave the stiff and starchy presentation be- hind them and portray their work with an element of fun and humour. One of those speakers was Professor Robert Samuel Houk senior chemist at the Ames Laboratory US Depart- ment of Energy who was presented with this year’s Maurice F.Hasler award for his work in the fundamental studies and applications of plasma ion sources for mass spectrometry. His research paid particular attention to ICPs time-of-flight and ion-trap mass spectrometry. His award address en- titled ‘Now for Something Completely Different The Scientific Impact of ICP-MS’ was particularly humorous as he likened his career to that of Napo- leon Bonaparte during the Napoleonic wars! For example with the aid of slides Houk was able to show that he like Napoleon started his career with long hair! Environmental science geo- chemistry and the nuclear and semi- conductor materials industries now make widespread use of the high sensi- tivity and selectivity of ICP-MS but Houk feels that there are several areas in which ICP-MS is underutilized; for example stable isotope tracing of min- erals in nutrition particularly zinc and elemental speciation by ICP-MS using a nebulizer.The symposium entitled ‘Promising Analytical Techniques on the Horizon’ was dedicated to the memory of Professor R. Sam Houk recipient of the I993 Maurice Hasler A ward36N JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY AUGUST 1993 VOL. 8 Professor L. B. (Buck) Rogers who pioneered developments in a wide range of analytical techniques includ- ing electrochemistry separations tech- niques and spectroscopy. Of particular interest was Gary Hieftje’s (Indiana University) talk on ‘Spectrometric Measurements and Instrumentation on the Horizon’ in which he sug- gested future paths that spectrometric measurements and inst rumen t at ion might follow.Particularly that they will be more biologically oriented use a greater range of dimensions make better use of spatial resolution have increased signal processing capa- bilities and use diode lasers. The importance of data visualization and imaging technology will progress for example with ICP imaging to show three spatial dimensions for true 3-D imaging using two spatial axes. The impact of nanotechnology will mean greater development of molecular- level instrumentation and advances now being made in semiconductor lasers suggest that in the not too distant future techniques like these may become routine and practical. Furthermore Hieftje deduced that spectrometric developments coupled with the advancement of new techno- logies would mean that such instru- ments will be capable of examining a sample as it is being analysed of tuning their own operating character- istics in order to optimize the sample characterization and therefore pro- duce accurate analytical results during the initial sample examination.Again H ieftj e’s present at ion was both humorous and enlightening. For example he showed a slide of a natural polarizing spectrometer-a goldfish! The Special Symposium celebrating the ‘10th Anniversary of the First Commercial ICP-MS Instrumenta- tion’ again featured entertaining pre- sentations from Sam Houk (Strategy and Tactics for ICP-MS for the Third Millenia A.D.) and Gary Hieftje (Atomic Mass Spectrometry-Current Status and Future Prospects).The opening remarks to the Symposium were given by Professor Velmer Fassel another early pioneer of ICP-MS and of course Sam’s supervisor. The ses- sion included presentations from other leading exponents of the subject Dr Don Douglas (SCIEX) ‘ICP-MS in 1993 Looking Back Looking Forward’; Professor Joe Caruso (University of Cincinnati) ‘Sample Introduction for ICP-MS’; Dr Jim McLaren (NRC Canada) ‘From Lith- ium to Uranium Picograms to Per Cent’. As can be seen simply from the titles of these presentations this excellent symposium was a fitting cele- bration of the last 10 years work on ICP-MS. It covered the history of the development of ICP-MS practical ex- periences and applications through the exciting future of the technique. A full report of this symposium can be found on page 37N. Meanwhile back down in the exhi- bition halls a technological showcase of the newest fastest best and bright- est that instrument manufacturers have to offer was on display.The continuing impact of developments in electronics and computer technology was evident in terms of faster analysis times improved sensitivity greater flexibility in technique usage and improved data handling and inter- pretation. Commercial viability of all analytical techniques is also greatly influenced by instrument component developments especially when those components have been around long enough to produce significant data. However it would appear that the battle of the arrays is on and diode array detection systems were the talk of spectroscopists at PittCon.Particu- larly Perkin-Elmer with its segmented- array charge coupled device (SCD) which permits operation in the UV region between 160 and 200 nm Baird Corporation with its megapixel charge coupled device (CCD) and Thermo Jarrell Ash which is marketing a charge injection device (CID) spectrometer. The Optima 3000 ICP-OES spectro- meter from Perkin-Elmer consists of an Cchelle based polychromator with an SCD a 40 MHz free running r.f. generator with true power control and temperature-controlled plasma pneu- matics. The user can measure the spectral background and each analyte simultaneously allowing 60 elements to be measured in less than 1 min. The optical system and SCD provide access to over 5000 atomic emission lines including over 200 prominent ICP lines.Inductively coupled plasma mass spectrometry would appear to be to- day’s technique for elemental determi- nations and if the new instruments (and lecture sessions) are anything to go by has a very promising commercial future. Wherever there is an increase in demand an increase in supply is not far behind and so it is not surprising that more companies are now market- ing ICP-MS instruments and new play- ers in the field include Varian Spectro Analytical Thermo ,Jarre1 Ash and Finnigan who are now marketing the previous Turner instrument. Spectro has introduced its Spectro- flame ICP-MS which it is claimed allows the determination of nearly all elements in the ultra-trace range with exceptional precision in approximately 20 s. Leeman Labs and Thermo Jarrell Ash have both introduced dedicated multi-element AA systems.Leeman Labs launched its simultaneous diffi- cult element analyser for the determi- nation of As Se Sb Pb and T1. The PS5000 is a graphite furnace AA sys- tem which is able to measure these elemental wavelengths at very high efficiency and is designed to increase productivity and analytical quality for contract laboratories. The AA-Scan series of AA spectrophotometers from Thermo Jarrell Ash has Smith-Hieftje background correction is run by an external PC and can be configured with either single-beam or double-beam op- tics. Furnace flame or automated flame atomizers are optional. The AA- Scan 4 includes a four lamp arrange- ment and a galvanometer controlled section mirror which provides for the simultaneous determination of up to four elements.The AA-Scan 8 is also a multi-element system which includes a motorized elevator to switch between two four lamp arrays. It is capable of measuring by flame or furnace AA up to four elements at a time and up to eight elements in an unattended run. Also from Thermo Jarrell Ash is the QS-1 mercury analyser which incor- porates a continuous flow mercury cold vapour module detection and readout system and a random access autosampler. The system has im- proved detection limits high sensitiv- ity and an automatic detection system which prevents contamination from high mercury samples. Away from the hustle and bustle of the exhibition halls The Royal Society of Chemistry hosted an evening recep- tion as it has done in past years as part of its role at PittCon.Almost 300 guests including some of PittCon’s organizers and some of the technical programme’s keynote speakers relaxed with friends and colleagues. The recep- tion is hosted each year at PittCon to provide an opportunity to meet all the US chemists who contribute to referee for and purchase the RSC‘s publica- The RSC standJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY AUGUST 1993 VOL. 8 37N tions. The RSC’s role at PittCon is vital for the continuing promotion of Infor- mation Services abroad. To that end the RSC’s staff manned an exhibition booth displaying the Society’s books journals and databases while some of the editorial and advertising staff scouted around for new ideas authors articles and book titles and new con- tacts for advertising.Next year PittCon will be held in Chicago Illinois in February-a Northern US city much more likely to Andrea Bedson be snowbound at that time of year KA YMICH INC. than this year’s Southern host city. 3387 Anderson Highway However Atlanta will be remembered Powhatan VA 23139 USA for a long time to come by all PittCon participants as the blizzard city! PittCon Symposium. ICP-MS The 10th Anniversary of the First Commercial Instrumentation (1983-1993) When attending a conference there is usually at least one symposium which one feels simply cannot be missed. For those conferees at the 1993 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy interested in inductively coupled plasma mass spectrometry that session was ‘ICP- MS The 10th Anniversary of the First Commercial Instrumentation (1983-1993)’.The symposium was arranged and presided over by V. B. Conrad (Consol Inc.) Several of the current leaders in the field expressed their views on a number of topics. The symposium began with a few opening remarks by the presider and then the surprise introduction of Vel- mer A. Fassel who gave some delight- ful memories of one of his former students and a co-inventor of ICP-MS Professor Sam Houk who was this year’s recipient of the Maurice F. Hasler Award. Professor Fassel stated there was little research activity on ICP-MS in other laboratories at the time the first paper was published in 1980 by Houk Fassel Gerald D. Flesch Harry J. Svec Alan L. Gray and Charles E. Taylor.This changed of course after the first commercial instrument was introduced in 1983 by SCIEX. In closing Professor Fassel quoted David W. Koppenaal as saying that ‘the technique appears poised for destiny and longevity in the trace analysis field’. These introductory remarks pro- vided an excellent lead into the first speaker’s talk. Donald Douglas of SCIEX discussed ‘ICP-MS in 1993 Looking Back Looking Forward‘. He spoke of the technical developments leading up to the first commercial instrument and the early challenges met by ICP-MS users including clogg- ing of the sampling orifice and very high continuum backgrounds. Rapid progress however ensued and today there are several ICP-MS instrumental manufacturers and roughly 800 ICP- MS systems installed in the world.The technique certainly seems poised for the future which will likely include developments in ion spray MS com- monly used in organic MS. Professor Joseph A. Caruso of the University of Cincinnati presented the second talk of the symposium enti- tled ‘Sample Introduction for ICP- MS’. Professor Caruso discussed work in his research laboratory utilizing novel sample introduction techniques such as electrothermal vaporization hydride generation liquid chromato- graphy (LC) gas chromatography (GC) and supercritical fluid chromato- grapy (SFC). These techniques provide alternatives to solution nebulization which is the most common method of sample introduction for plasma MS. Additionally coupling such chromato- graphic techniques as LC GC and SFC to ICP-MS allows one to obtain speciation information at the ultra- trace level.Finally a few slides in yellow and black were dedicated to Professor Houk who is a big fan of Pittsburgh athletic teams! After a brief recess Professor Gary M. Hieftje from Indiana University spoke on the current status and future prospects of atomic mass spectrome- try. A review of the strengths and weaknesses of modern plasma source (PS)-MS instruments was given. He stated that no other atmospheric pres- sure source is likely to be more effici- ent than the ICP. The most significant shortcomings however include ma- trix and spectral interferences. In addi- tion Professor Hieftje discussed ‘tan- dem’ atomic MS as a means to obtain greater flexibility and the advantages and disadvantages of time-of-flight mass spectrometry.His idea of the next generation of PS-MS instruments includes the simultaneous determina- tion of all isotopes. ‘From Lithium to Uranium Pico- grams to Per Cent’ was the title of the fourth presentation of the symposium. The overall theme of Dr Jim McLar- en’s talk (National Research Council of Canada) was the versatility of ICP- MS. There are numerous trace elemen- tal and environmental applications of the technique to a variety of samples such as sea-water freshwater and marine sediments. In particular Dr McLaren presented his work on the analysis of natural waters; HPLC-ICP- MS techniques were also addressed. The last (but certainly not least) speaker of the symposium was Professor Sam Houk of Iowa State University. Professor Houk discussed ‘Strategy and Tactics for ICP-MS’ for the future and in particular ‘the Third Millenium A.D.’ As with any analysis technique there are areas in ICP-MS which require future im- provements.These areas include the reduction of matrix interferences at- tenuation of polyatomic ion inter- ferences and LC-ICP-MS or capillary electrophoresis ICP-MS for speciation analyses. The future of ICP-MS may include according to Professor Houk ion deposition or ion implantation as well as floating interfaces. Much to the disappointment of his fans Professor Houk did not regale the crowd with detailed excerpts of the adventures of Napoleon and Columbus! For all who attended the ICP-MS symposium honoring the tenth anni- versary of the introduction of the first commercial instrument was an en- lightening and educational experience.It is always exciting to listen to experts in one’s field discuss the events lead- ing up to significant findings review their present work in the area and address directions for the future. In conclusion as David W. Koppenaal humorously put it in his review of atomic mass spectrometry in the 1992 fundamental reviews issue of Analytical Chemistry ICP-MS ‘has truly become a technique for the masses’. Francine A. Byrdy Department of Chemistry University of Cincinnati Cincinnati OH USA38N JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY AUGUST 1993 VOL. 8 Instrumental Technique Development March 24-25 1993 Fitzwilliam College Cambridge UK Each year the Atomic Spectrometry Updates (ASU) Editorial Board of the Journal of Analytical Atomic Spectro- metry hold a one day Editorial Meet- ing followed by an open one day Scientific Meeting.To all intents and purposes the Scientific Meeting is a celebration of recent developments in the field of Atomic Spectrometry. This years meeting was held in Fitzwilliam College Cambridge and was co-spon- sored by the Atomic Spectroscopy Group of the Analytical Division of the RSC. As has become customary two Editorial Board Members from overseas were invited to the meeting to present a lecture on the general theme of ‘Instrumental Technique Development’. In the evening prior to the meeting a Sherry Reception was held at the Salt- marsh Room of Kings College Cam- bridge. During the Board Dinner on the following evening presentations were made to the visiting overseas speakers Professor Bob Michel (University of Connecticut USA) and Dr Henryk Matusiewicz (University of Poznan Poland).The scientific meeting was opened by Doug Miles chairman of the ASU Editorial Board who introduced the first of the guest speakers Professor Robert Michel (Connecticut USA) who gave an excellent overview on Laser Excited Atomic Fluorescence Spectrometry (LEAFS) in a Graphite Furnace. With such a subject many presenters could easily be bogged down in the theoretical aspects how- ever Robert kept the subject alive with his wit his basic ‘down to earth’ philosophy (i.e. practical) his honesty and openness and simply his enthusi- asm for Atomic Spectrometry. With respect to honesty and openness Robert explained that lasers to say the least are awkward to work with re- quiring at present a few days to change dyes in the tuneable laser in order to change analytical wave- lengths. Once the system is up and running detection limits obtained are at the femtogram level and the concept of ‘single atom detection’ becomes more than a theoretical discussion.Further the graphite furnace LEAFS technique has a dynamic range of 5-7 orders of magnitude. Here lies the root of yet another ‘practical’ problem -the method is so sensitive that the single most likely reason for poor analytical results is solution con- tamination. In order to increase the Doug Miles (L) making a presentation to Bob Michel dynamic range to a more ‘practical’ range of concentration an idea first proposed by L’vov for electrothermal AAS is being investigated.This idea involves the measurement of stray light in the spectrometer and the point of calibration curve ‘rollover’ and then extension of the dynamic range by applying a mathematical correc- tion. This work is on-going as is the development of a more practical laser system based upon solid state lasers with a hydrogen Raman cell to enable final wavelength tuneability. The second guest speaker was Dr Henryk Matusiewicz (Poznan Poland) who presented a lecture on ‘Novel Approaches to Microwave Sample Preparation and Sample Introduction to Microwave Plasma Atomic Emis- sion Spectrometry’. This lecture re- viewed some of the older methods of sample preparatiori and then con- tinued into the area of microwave Doug Miles (L) thanking Henryk Matusiewicz digestion procedures.Henryk showed a high pressure digestion bomb which used a microwave wave-generator in- stead of a magnetron to focus the microwaves inside a water-cooled stainless-steel jacket containing a sealed ceramic sample container. This enabled the complete digestion of organic samples with the main advan- tage of zero cool-time which is the time often ignored by workers report- ing the advantage of speed in micro- wave digestion procedures. The disad- vantages of the method were stated as the ‘batch’ nature of the procedure and that it was labour intensive. Of more current interest was the discussion of ‘on-line’ microwave digestion proce- dures involving ‘stopped-flow’ flow injection (FI) apparatus. It was con- cluded that this procedure is still at the preliminary stages of development and that no high pressure FI microwave digestion systems have as yet been described.Surely this is an idea worthy of commercial investment and development! The morning session was concluded with a lecture by Dr A. McMahon (AEA Technology UK) on ‘Recent Develop- ments in Resonance Ionization Mass Spectrometry (RIMS)’ and a lecture by Dr J. Bacon (Macaulay Land Use Research Institute) on ‘Thermal Ioniza- tion Mass Spectrometry (TIMS) for Measurement of Stable Isotopes in Environmental Studies’. On a lighter note it seems that Adam McMahon had to travel the world just to get a bit of research done on his chosen research interest. Adam suggested that after 20 years of development RIMS is just beginning to find its niche amongst an array of other instrumental techniques in analytical science.The applications discussed included the imaging of trace elements in biological samples and the measurement of Sr isotope ratios. The lecture by Jeffrey Bacon on TIMS in- cluded some excellent precision studies on isotope ratio measurements for Nd Pb and Sr. For Nd and Sr precision figures of one part in 1 O6 were presented for isotope ratio measurements. From the practical point ofview the technique involved extensive sample clean-up/ preparation and the sample throughput is low. However it is probably the most precise method for measuring isotope ratios and when combined with iso- tope dilution analysis the technique can also offer the highest quality accu- racy. One application discussed was the measurement of Sr isotope ratiosJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY AUGUST 1993 VOL.8 39N ASU Board Members at the Board Dinner. From leji Jim Crighton Adam McMahon Simon Sparkes and John Dawson in surface waters. The Sr isotope ratio in surface waters reflects the minimum age of the rocks over which the water flows and is of importance to isotope geologists. Further applications were presented including Cu:Zn isotope ratios in human nutrition studies and Pb isotope ratios in field experiments. The afternoon session included lec- tures by Dr Simon Sparkes (University of Plymouth) on ‘Measurement of Radionuclides by ICP-MS’ Dr Ian Shuttler (Perkin-Elmer Germany) on ‘The Development of AAS Instrument Control Software’ and Alan Batho (Thermo-Electron) on ‘Every Picture Tells a Story-ICP Signals Captured’.The lecture by Simon Sparkes outlined the use of ICP-MS to determine low levels of long-lived radionuclides e.g. 238U 235U 232Th 237Np 99Tc and 1291. One of the interesting points raised by Simon was that the ion-extraction ca- pability of the ICP-MS interface used was only 1 part in lo5 and that a small increase in this efficiency could lead to a large sensitivity increase of the tech- nique. The advantages of the tech- nique for these elements were isotope specificity simplicity speed few inter- ferences and high sensitivity. The presentation by Ian Shuttler changed the emphasis of the day’s proceedings from instrument hard- ware to software. This was a well presented lecture that took the audi- ence back to the days when atomic absorption instruments were com- pletely manual and comprised of knobs switches things that occasion- ally went bang and the requirement of a ‘Buck Rogers’ look-alike to give the results credibility.This reviewer is of course too young to remember such instruments. Ian then proceeded through the years reviewing the intro- duction of automation in analytical instruments and explained the ad- vances in software development up to the present day. The future develop- ment in software was forecast to be focussed upon one computer to con- trol many different instruments; more interactive screen software; intelli- gent/knowledge based systems; im- proved Windows based software; and advanced quality control and self- testing software.This lecture differed from the usual ‘instrument manufac- turer’ type lecture in that it addressed the philosophy of the type of software required by analytical chemists and that can only be praised. It seems that Perkin-Elmer now have an analytical chemist specifying software and that might explain why the newer instru- ments are becoming more user friendly (compare the PE-4100 to the The final lecture of the day from Alan Batho Thermo Electron also started by taking the audience back to the beginnings of optical emission spectroscopy namely with arc and spark sources when the emission spec- tra were recorded on photographic plates. In the intervening years the photographic plate has been super- ceded by the photomultiplier tube (PMT) as detector and while the PMT has many advantages its adoption meant that the complete elemental picture of a sample i.e. all the ele- ments was lost. Alan discussed how with the use of a solid-state detector such as the charge-injection device (CID) array as employed in the IRIS emission spectrometer that this situa- tion has been recovered. Thankfully Alan provided a useful and slow step- by-step approach to how CID arrays work. The CID array provides a com- plete picture of every emission line of every element in the sample which brings us back to the same situation as in the early days with photographic plates. Naturally in the 1990s the information is presented on a com- puter screen and the views of the software images produced and the use of the MS Windows package illus- trated some of the points raised by the previous lecturer. Overall an excellent day was had by all and thanks must go to all the speakers and the organizing commit- tee. My ‘lecturer of the day’ award must go to Professor Robert Michel who told stories of being covered in red dye whilst trying to change analytical wave- lengths in his laser system. My guess is there aren’t many Professors of analyti- cal chemistry worldwide who still get their hands dirty. My thanks must also go to the ASU Editorial Board who asked me to review this meeting. P E-30 30). Alistair A. Brown [Jniversity of Plymouth Drake Circus Plymouth UK PL4 8AA