* The information on this page is based on an original manuscript by Dr M. Wassall, with the permission of the author. Copyright © M Wassall

The quantitation of metallic and semi-metallic elements of the Periodic Table has been performed by many and varied techniques. Only three techniques however have ever reached the status of enjoying worldwide market value of between $100M and $200M per annum, and this remains true to this day.

The earliest of these techniques was Atomic Absorption Spectrometry (AAS), invented in the late 1950s, and enabled the part per million (ppm) level of detection of some seventy or so elements. A major additional improvement in the technique whereby the flame atomisation of the sample was replaced by a resistively heated graphite tube into which small samples (>5 microlitres) could be pipetted was invented by Dr Boris L’vov in the mid 1960s. This enabled detection down to parts per billion (ppb) level and the use of very limited sample.

The late 1970s saw the use, initially for research purposes and later for commercial exploitation, of an improvement of the emission spectrometry technique. This was the second technique and was christened ICP-OES or Inductively Coupled Plasma Optical Emission Spectrometry. By replacing the relatively cool flame as the source of excitation with an argon plasma running at temperatures up to 10,0000C a far more efficient and intense spectral output was achieved. By combining this with a very high resolution optical monochromator many elements could be determined at the same time and at levels slightly better than flame AAS. The relatively higher cost of the equipment could often be rationalised by the improvement in analysis time and hence sample throughput.

The third important technique was developed during the mid-1980s as researchers began to question the efficiency of the optical detection system. By capturing the ion species of the sample emitted from the argon plasma in a mass spectrometer detector this efficiency was greatly improved. The technique of ICP Mass Spectrometry (ICP-MS) had arrived. The technicalities of interfacing the flow of many litres a minute of argon gas with a very high vacuum detector were soon overcome and the technique moved into commercial realisation. This provided fast, simultaneous sample quantitation at levels down to part per trillion (ppt), again at yet greater cost to the user. Very quickly this field of instrumentation divided into two distinct sub-groups dependent on the mass spectrometer technology. These were quadrupole mass spectrometers and magnetic sector mass spectrometers, the latter offering the very lowest levels of detection but by far the highest costs and real estate space requirements!

All these techniques were to play a part in the development of the Pye Unicam and subsequent businesses as we will discover.

 

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Not unlike the identification of Furnace AAS as an increasingly important analytical technique, the York Street site of Pye Unicam/Philips was equally poor in identifying ICP-OES in the same way. This was curious and very difficult to explain since one of its greatest proponents, Dr PWJM Boumans, was employed by Philips at the Nat Lab research facility in Eindhoven. Not for the want of trying had Paul Boumans enthusiastically made the case for the technique, but it also requires a receptive audience to turn this into a viable commercial product. Throughout the late 1970s Dr Boumans visited York Street in order to demonstrate to a sceptical audience the benefits of emission spectrometry performed with high temperature sample excitation and high resolution optical detection.

In the end it was the sister Philips factory in Wavre, Belgium who introduced the company’s first commercial product, the Philips PV8050 ICP followed in turn by the PV8055, PV8060 and PV8065 systems. These were simultaneous multielement systems, produced by placing a number of detectors around what essentially was the Rowland circle of the polychromator. The user would then define the elements of interest and Philips would deliver an instrument with anything up to 56 detectors placed at the relevant wavelengths required.

As can readily be discerned from the advertising, the instruments were large, floor standing products requiring considerable laboratory space. This was necessitated by the optical resolution of the polychromator and the physical requirements of fitting the multiple detectors around the optical layout. Nevertheless the products in the right, experienced hands were capable of achieving fast and accurate analyses.

At a meeting of the Colloquium Spectroscopicum Internationale (CSI) in Cambridge during mid 1979 it became obvious that the market leader in elemental analysis, Perkin Elmer, was considering adapting its top of the range AA spectrometer - the PE5000 - by replacing the lamp and atomiser items with a plasma generator and torch. It was difficult to give the product much credibility owing to the small size of the monochromator, but nevertheless PE went ahead and subsequently launched such a product. Sure enough, the instrument was a bit of a flop, but in a sense it achieved its aim of providing them with a presence in this market.

At this time there were companies such as ARL, Jarrell-Ash, Philips, Baird and Leeman Labs who were effectively dedicated to this emission technology but had little or no presence in the AAS market. On the other hand there were companies such as Perkin Elmer, Varian, Instrumentation Laboratories and, of course, Pye Unicam who were heavily into the AAS market but had little or no presence in the ICP market. Since ICP was the new emerging technique there was a great deal of pressure for the AAS companies, with their relatively large market shares to protect, to become conversant with, and significant players in, the ICP marketplace. The race was on for all these latter companies to catch up with the dedicated suppliers and, where possible, overtake them in technology and market share terms. This indeed was the reasoning behind the Perkin Elmer move with the variant of the PE5000 product.

The other point to note was that the existing ICP companies had to date largely produced large simultaneous detection systems, often dedicated to specific market application segments. It’s clear that the AAS companies felt they could perhaps bring some more sophisticated, value for money, more universal product design to play once a market entry had been achieved.

By the early 1980s the penny was beginning to drop at Pye Unicam that this was a technology that could not be ignored and that we were a little late to the party once more!

 

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Given that we had neither the time or the resources, or for that matter the knowhow, to develop a product from scratch, it was clearly necessary to find a suitable partner. The company that stood out as by far the best fit was Leeman Labs in Boston, Mass, USA. They were a relatively small company, owned by a single person - John Leeman - and whose ICP offering was interesting to us in several ways. First of all the product was quite unique and employed technology that had a significantly advanced optical basis. Secondly Leeman Labs would definitely welcome the Philips distribution outside North America. And finally the product was of a type that would appeal to a user moving from AAS to ICP, in that it was benchtop, small, simple to operate and completely flexible in its application. Consequently we entered discussions with John Leeman, and under an appropriate non-disclosure agreement began to learn much more about the product and the potential ICP market

The Leeman Labs product being marketed around 1982 was known as the Plasma-Spec and consisted of an RF argon plasma, powered from a large Varian vacuum tube, as the means of excitation and an Echelle polychromator and a rapidly scanning photomultiplier as the detection system. The optics were quite unique. The Echelle polychromator used an echelle grating viewed in very high order and illuminated at a large angle of incidence. This is possible as the grating has relatively coarse rulings in the shape of steps - hence the name echelle. By using a prism to sort these high resulting spectral orders it is possible to form a two dimensional array of spectrum segments, thus covering the whole spectrum by adjacent "ribbons" of spectrum. The photomultiplier then had to scan rapidly from line to line at the exit slits in this plane in order to measure the intensity of the lines of interest, relating to the elements of interest. Thus the instrument was a very fast scanning sequential element ICP.

Leeman Labs had been marketing the product in North America for a few years and it had a reasonably good reputation.

The next step was to ship an example to Pye Unicam/Philips so we could properly evaluate it and move to the next steps in the negotiations. An instrument arrived just as the company was breaking for the Christmas holiday. Undeterred, the evaluation began despite the holiday, however this didn’t get far.

The torch of an ICP generally consists of three concentric glass tubes surrounded by the RF coil. A coolant gas, the plasma gas and the injector gas carrying the sample are all fed into these respective parts of the glass tubes. When the field is switched on and the plasma seeded the temperature inside this torch can reach as high as almost 10,000°C and only the careful balancing of the coolant, plasma and sample gas flows prevent the quartz glass tubes from melting.

There was little in the way of today’s interlocking of flows and the knowledge level of the operators was sadly lacking, so that within the period of a couple of hours we’d melted every torch sent with the instrument. We turned off the power and went home for Christmas - greatly disappointed and with a telex for more torches winging its way to Boston!

Following a complete evaluation of the product, preparation of application notes and user documentation, service training and manual preparations and all the rest of the product preparation, a full marketing plan was put in place and contracts signed with Leeman for us to handle the product worldwide with the exception of North America, from which we were barred from competing. This latter point was a big disappointment, since the territory was by far the biggest potential market, however from Leeman’s perspective it was quite understandable.

During this process the product was given a Philips makeover. The product became the PU7450 ICP and the casework given a change into the standard Philips colours and branding. John Leeman commented that the industrial designers at Philips were worse than, and even more demanding than, his wife’s home design consultant! Nevertheless the product looked a great deal more appealing in the new, lighter colours than in the rather depressing blacks and dark greys of the Leeman version.

This exercise was indeed of great value in rapidly learning much about the technique, the technology and the ICP market. Because of having no access to the North American market the sales volume remained firmly and consistently just below the 100 units per annum mark. This was something of a disappointment to ourselves and indeed to Leeman Labs. Despite that the partnership continued and when Leeman upgraded his product to the PS-1000 with an improved 40 MHz RF system we also had access to this technology. By the latter part of the 1980s we were ready to accommodate the new Leeman improvements and also change the whole appearance of the product to provide a more modern, sleek and improved product.

This was the PU7000 ICP, again making its initial appearance in the new Philips colours. For this product we were increasingly adding our own components and Leeman shipping internal modules upon which we could build. This enabled the product to visually depart even more from the Leeman version and for the York Street site to gain an even greater insight into the technologies. In addition to the more integrated nature of the product casework, a great deal of work was being put into the development of the PC based control and data processing software. Post processing of data and data storage and retrieval were becoming more and more important, especially with a technique like ICP which could produce relatively vast amounts of data.

Despite these improvements, we remained a relatively small player in the ICP market and without access to the North American market this was proving an uphill struggle.

 

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In early 1991 ATI (Analytical Technologies Inc) became the new owners of what had originally been Pye Unicam. Based in Boston, Mass, USA, ATI was essentially a venture capital company which was in the process of buying relatively struggling, mid-sized companies, putting them together and improving their financial performance with a view to finally floating the conglomerate on the New York Stock Exchange. We joined companies such as Mattson (a USA FT-IR manufacturer), Orion Research (pH systems) and Cahn (balances) and quickly became influenced by the new American management.

Although it might have done so, this new acquisition did not really affect our relationship with Leemen Labs and the ICP business continued in its previous fashion. Neither was there any internal competition within ATI as we were really the only one of their companies with these Elemental technologies.

However it was becoming more and more obvious that we should be contributing far more to the ICP development than in previous years. Because of our close relationship with the University of Strathclyde in Glasgow where we supported several students, much equipment and even a chair in Analytical Chemistry, it became possible to initiate a collaborative project in the development of ICP software. Major problems in ICP-OES analysis are caused by spectral interferences and incorrect analytical line choice. To overcome these problems, especially for relatively inexperienced analysts, a software package employing advanced chemometric techniques was developed within this project, to predict and quantify such issues and provide solutions to the user. This additional software package was given the acronym SLIM or Spectral Line Interference Modelling and, marketed with the latest version of the ICP product, provided significant differentiation from the Leeman ICP.

Together with a large number of other software improvements in the PC based software, the new package was launched in 1992/3 as the ATI Unicam 701 ICP. With the dropping of the Philips ownership and name, it had been agreed to resurrect the Unicam brand for our catalogue of ATI products. The new software provided very high levels of automation of hardware functions and considerable improvements in data processing and storage. Externally however the product remained relatively unchanged except for the branding and colour change.

The change in ownership, changes in sales-force and what seemed like a new start certainly helped support and even enhance the ICP sales volume somewhat, but it was difficult to accept this part of the business as highly successful - either from our own perspective or indeed from Leeman Labs perspective. Nevertheless we continued building our in-house expertise in the subject, which as circumstances proved was just as well.

It was decided that the relationship with Leeman would not last for ever. There was no access for us to the world’s largest market, there was simply insufficient margin available for both companies and Leeman Labs had technology strategies that were in conflict with our own thoughts. As a consequence we set about defining some projects that we would like to both investigate and start as soon as possible. In outline these were a "traditional" basic sequential ICP-OES based on conventional optics, detector and torch technologies, an advanced echelle based fast sequential, or even simultaneous ICP-OES utilising a CCD chip as detector rather than photomultiplier technology and finally a "blue sky" project to look at the feasibility of an ICP coupled with a mass detector - either a mass spectrometer or a time of flight spectrometer.

This latter project really was "blue skies". We had almost no resource to support it, but felt that since ICP coupled with a mass spectrometer was by now a commercial reality, then we should become both knowledgeable about the technologies and perhaps identify a disruptive technology that could be employed at some time in the future when resources were free from the ICP-OES projects.

The real focus was upon the first two proposed ICP-OES projects and in particular in the second of these employing a solid state detector. By this time digital cameras were well under development and the CCD imager business was in top gear trying to develop better and better chips for the purpose. Although the ICP instrument would requirement quite different chips to those in digital cameras, in fact more like the type used in astronomical telescopes, the activity in the industry in general was bringing such devices into an economically viable area for our purposes. When employed with an echelle polychromator that imaged the final spectra directly onto the chip, it meant that all moving parts disappeared and both fast sequential, or even simultaneous measurements could be made. This would provide the ultimately flexible analytical tool, with the entire spectrum saved for any future re-visit to obtain more data.

The "blue sky" project was out-sourced to a relevant local company for a paper study and the two ICP-OES projects started with some urgency.

Although we were dealing with new technology to us, the years working with Leeman proved invaluable in kick starting the projects. Experimental models were built following considerable paper feasibility investigations. At some point it was agreed to put the majority of resource behind the CCD based project, since it produced an instrument that would certainly be at least beyond the "state of the art" by the time of its launch. The basic instrument became more of a fall-back option should we ever have additional resource - in other words, unlikely to ever see the light of day!

This enabled the CCD instrument to make exceptionally rapid progress, given the issues to overcome and with great excitement the Marketing department set about planning brochures and launch events. Some of these items still exist in draft form, but sadly were never to see the light of day in a more general sense. Once more events were to overtake our plans!

In 1995 the world at the York Street site was again shaken up with the acquisition of ATI businesses by Thermo Electron Inc of Waltham, Mass, USA. As documented elsewhere, an early move by Thermo was to split the various Cambridge businesses up into independent entities, each with their own business team. So the IR business was effectively absorbed by another, bigger Thermo IR company - Nicolet. This effectively left three remaining Cambridge businesses, Chromatography, under Bob Bates, which eventually went off to a factory at Bar Hill outside Cambridge and the UV business, under Maurice Shorter, eventually converted a vacant factory unit in Mercers Row, Cambridge. The Elemental business, now consisting of AA and ICP-OES and under John Hemming, at the same time moved to an ex-Philips factory in St Andrews Road, Cambridge. This really proved to be a time of great upheaval, with a large reduction in workforce, however for the present we continued to work together in what remained of the York Street site.

The immediate impact as far as the ICP part of the business was concerned was that John Leeman, and hence Leeman Labs, refused to either co-operate with us as a Thermo company or in the relatively near term conduct any further business. There was much past history to which we were not privy and neither were we able to overcome the situation. Consequently we began to discuss an amicable separation of the ways.

 

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At first this problem with Leeman simply accentuated our need to accelerate the development of the CCD project which now had the Marketing name of QUASAR.

However times were indeed a-changing at York Street. An American, Clancy Schupert, had been drafted in as General Manager with the three remaining business teams reporting through him.

Some-time before the ATI acquisition Thermo had acquired the Jarrell-Ash Corporation, a distinguished optical and analytical instrument manufacturer in Franklin, Mass, USA. Although primarily an ICP manufacturer, Thermo Jarrell-Ash(TJA) had acquired another Massachusetts AAS manufacturer by the name of Instrumentation Laboratories - a company we in Cambridge knew very well as a strong competitor. This of course meant that Thermo had a surfeit of AAS and ICP manufacturers, together with other companies they possessed, such as ARL in Switzerland who also provided similar product.

Since TJA had been part of Thermo for some time, and were USA based, it fell to them to help resolve this issue. Engineers and marketeers were dispatched to Cambridge to review our products, our technologies and any products still "in the kitchen". Finally a showdown meeting was called in Clancy’s office in York Street. After much discussion, argument and hand-waving it was agreed that TJA would become the centre for ICP-OES and Unicam the same for AAS. In other words the significant ICP projects at York Street would immediately stop and similarly the AAS products at Franklin would be wound down. Any technologies from either would be available for the general good.

This was indeed a blow for the York Street site who saw their growth salvation very much in the ICP product. Having starved the AAS product line of development resource to get this far with ICP it was indeed a double blow for our future.

Despite all that had gone before, it became ever obvious that Thermo required a slimming of resources to better match our not so healthy business figures. In addition the York Street site was to be sold by Philips (who still owned the site) for housing development. Auctions were held on site for all the machine shop and other equipment and before long the Elemental business was searching for a new home. An ex-Philips building in St Andrews Road was available and so, with extensive refurbishment, this became the Thermo Unicam Elemental business home for the next few years.

Given the decisions described above, the Unicam business had no option but to throw all the available resource at developing new AAS products. As it turned out this was very successful and we were even able to use some of the knowledge gained during the later ICP developments to enhance our new AAS designs. The detail of this is described elsewhere, however the first major new development was the M Series AA System launched in May 1999 to be followed by a launch of the S Series AAS System in October 2001.

During this period another upheaval was underway. The lease of the St Andrews Road factory was coming to an end and the land was required for further housing development. A new home had to be found. The various Cambridge science parks could provide some very attractive alternatives but at a cost that Thermo was not prepared to pay. Finally an almost suitable unit was found in Mercers Row - just down the road from our UV-Vis business colleagues who had been there for some time now. The premises were cleared out and re-furbished and our move was completed. In the years to come Thermo surprisingly purchased the premises for around £1M and further refurbished and expanded the building with an additional £0.5M, adding an internal mezzanine floor and additional factory space.

 

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This date in 2001 was indeed a significant one for the ICP business in Thermo. During the S Series launch in Amsterdam we were confidentially told that ICP-OES activity would return to the Cambridge facility and the TJA facility in Franklin, Mass, USA would be gradually wound up. This indeed was surprising news but based on the following reasoning and conditions.

Thermo management were impressed by the design and manufacture of the new AAS products and wished to embrace this within the new ICP development. Cambridge would be given two years to develop a totally new ICP product with which to open a newly constructed area within our new factory for its manufacture. The savings in Franklin were immense and a relatively small proportion of this saving would be passed on to Cambridge to fund this total activity. Any technology from Franklin would be available to us. The marketing activity would also transfer to Cambridge.

For a week or two, especially being in the middle of an important AA launch, it was difficult to respond to this opportunity. The first and most pressing issue was that two years was quite inadequate to build a whole new team, come up to speed with the new ICP technologies, recruit new staff, refurbish our premises with suitable infrastructure, wind up the Franklin activity and take over the support of products with which we were not familiar, and then finally design a market leading new product. We suggested a minimum of three years, but the response fell on deaf ears - the potential Franklin savings were just too attractive to senior management. We simply had to get on with the job.

We discovered that some of the newly developing technologies within the Franklin activity could indeed be used within our own early concept of what a new ICP should be. These thoughts, some Franklin technology and our approach to the development of AA products formed the basis of our initial proposals.

We believed that a ridiculously small bench footprint combined with an echelle polychromator and solid state detector, and a solid state on-board RF power supply feeding a conventional torch would form the main components of the product. The project acquired a code name - Clipper - based on the next project name that was going to be used by Franklin.

Up until the launch of the new ICP product this part of the Thermo offering had mainly come from the Franklin factory. They had had a long line of successful products and had more or less invented the breakthrough of viewing the plasma along its axis - the so-called "axial" mode. The traditional torch viewing had always been at right angles to the gas flows, and hence termed "radial". An instrument capable of both viewing conditions became known as a "duo" instrument. The "axial" view systems in general offered better detection capability, whereas the "radial" systems could cope with interference effects somewhat better. Since 1994 the IRIS range of ICP from Franklin had been market leading products, and in total more than 3000 IRIS had been sold.

However the annual market share by the early 2000s was falling and barely achieving 300 units per annum. The last product in the series - the IRIS Intrepid - was launched in 2003, at the same time that the Clipper project in Cambridge was beginning to gain some momentum. The Intrepid was a very large, floor mounted system with average performance.

The detector in the new Clipper product was chosen to be the same as the Intrepid - a CID chip (Charge Injection Device) rather than the universally employed CCD (or Charge Coupled Device) chip. The CID chip was unique to Thermo and manufactured in the Thermo facility at Syracuse, New York State, USA. It had some unique advantages over the CCD chip, but also some disadvantages. The echelle optics were designed by Charles Perkins in Cambridge and the RF power supply for the plasma, chosen to be a solid state rather than valve system, was developed in Cambridge, and manufactured by AWS in Newcastle under Lyme.

Much effort was put into the casework design. The instrument would be breathtakingly small and by using injection moulded covers, we were determined to make the product both beautiful and jaw-dropping at first glance. Our industrial design consultants, Creative Design in Cambridge - mocked up many alternatives before alighting on the one chosen.

As with most new developments, there were many issue and problems to solve but just over 3½ years after the actual project start (and almost $10M investment) we went into production in the completely re-furbished Mercers Row facility. With little more than 20% to 30% of individual parts, assembly time, volume and weight of its predecessor, the IRIS Intrepid, and out-performing it on all performance parameters, the new product had met virtually all the original targets. As a gesture to the distinguished traditions of the Franklin factory, in January 2006 we launched the product at an international ICP conference in Arizona under the product brand of iCAP. This was a modern variation on the ICAP (Inductively Coupled Argon Plasma) brand adopted many years earlier by TJA and which had been defunct for many years. There were two major variants - the iCAP 6300 and iCAP 6500 - both available in either Radial or Duo views, but varying in RF power, gas control and sample peristaltic pump capabilities.

Within a year of launch we were shipping in excess of 500 units per annum and this number continued to steadily rise. Today it approaches almost twice that level and individual system rarely cost less than $50,000 and sometimes almost twice that figure. The success and return on investment would arguably make the iCAP the most successful product to come from the "Pye Unicam" Cambridge operation.

In addition to the warm, and often astonished, initial reaction of potential customers, recognition of the achievement arrived from many quarters. We were awarded the Instrument Business Outlook Journal’s 2006 IBO Industrial Design Award, which made a pleasing pairing since our S Series AA instrument had won the equivalent award in 2002.

In recognition of development of the iCAP product Charles Perkins and Mike Wassall, as representatives of the entire Cambridge team were wined and dined in Boston, USA in order to be presented with the 2009 Thermo Fisher Scientific Hatsopoulos Award for Technical Innovation. Named after the original founder of the Thermo company, this is the most prestigious award of the Thermo Fisher company and is only awarded once each year to an individual from the 50,000 employees of the company.

At this very moment the Cambridge site as a whole were awarded The Queen’s Award for Enterprise: Innovation 2009. This was primarily for work and business resulting from the new iCAP product. Since much of this work owed its roots to our AA heritage, the award was shared by the whole site. A party was held in a marquee erected in the car park at Mercers Row and the Lord Lieutenant of Cambridge, as the Queen’s representative presented the award, and enjoyed the party!

The iCAP product continued to break company records in terms of units shipped and market share achievement, finally returning Thermo to a market leadership position in the technique. As with most products, the inevitable face-lift and general improvement occurred some six or seven years after the initial launch. Rebranded as the iCAP 7000 Series and consisting of three basic products - the iCAP 7200, 7400 and 7600 - the all new Qtegra software is just one additional reason why the product continues to go from strength to strength in terms of unit volumes. Well in excess of 5000 iCAP units have now been shipped to customers and total revenues must significantly exceed $250M.

With the transfer of all the AAS product manufacture to the Thermo factory in Shanghai, China it was almost inevitable that the iCAP, with its relatively simple assembly and totally automated test regimes should become the next candidate for transfer to Shanghai. The process adopted was, like the AA transfer process, a gradual one with kitted sub-assemblies shipped to Cambridge for final assembly and test. A great deal of staff temporarily transferred and training for the Chinese staff was completed, and after a period of around two years the transfer was complete and all manufacture of both AAS and ICP-OES was now in China. A final irony was that due to the large order backlog, the Cambridge factory stayed open a month longer than planned but in April 2014 it finally closed and the building was put up for sale.

Throughout this period the technique of ICP-MS had largely been ignored by the Cambridge site following the completion of the earlier paper studies mentioned above. This was largely due to the fact that once acquired by Thermo we joined sister companies such as VG Elemental and Thermo in Bremen, Germany who both supplied quadrupole and magnetic sector versions of the ICP-MS product. Consequently there was little point in trying to provide even more internal competition. Ironically the Winsford, Cheshire, UK site of VG Elemental, whom we had had close relations with over the years was the first to be closed and all ICP-MS activity transferred to Thermo in Bremen. And it was to this site that all AAS and ICP-OES Development, Marketing and Product Support were transferred from the Cambridge site, concurrent with the Shanghai manufacture transfer completion.

So finally the lights were turned out in Mercers Row and all Thermo Fisher Elemental activity departed Cambridge. At least the company closed following arguably the most successfully designed, marketed and manufactured product in its history!

 

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Sources: 1. Original manuscript Dr M. Wassall