ISSN:0144-557X    

DOI:10.1039/AP98926FX009

出版商:RSC    

年代:1989

数据来源: RSC

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March 1989 ANPRDI 26(3) 85-120 (1989) Analytical Proceedings Proceedings of the Analytical Division of The Royal Society of Chemistry CONTENTS 'The Decline of British Analytical Chemistry: Fact or Artifact? by T. Braun, A. Schubert and S. Zsindely 92 Silver Medal Lecture 92 96 Ronald Belcher Memorial Lecture 96 85 New Members of Council 86 Award of Fourth Robert Boyle Gold Medal 86 Hilger Spectroscopy Prize 1988 86 Analytical Viewpoint 87 'Becoming Absorbed and Excited in Atomic Spectrometry' by David Littlejohn 'Membrane Design and Photocuring Encapsulation of Flatpack Based Ion-sensitive Field Effect Transistors' by Jonathan M. Slater 99 SUMMARIES OF PAPERS 99 Laboratory Information Management Systems 'Current and Future Impact of LlMS in Quality Control' by A. A. Wagland 'LIMS in the Pesticide Residue Laboratory' by P. J. Snowdon 'Justify a LlMS System' by G. Davison 'LIMS for the End User' by A. D. Henderson 'Hewlett-Packard's LABSAM in an Integrated System' by I. J. Smith 99 100 102 102 103 106 SAC 89: Scientific Programme 113 Equipment News 117 SAC Silver Medal (Rules) 118 Conferences and Meetings 118 Courses 119 Analytical Division Diary Typeset and printed by Black Bear Press Limited, Cambridge, Fngland

ISSN:0144-557X    

DOI:10.1039/AP98926BX011

出版商:RSC    

年代:1989

数据来源: RSC

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ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 85 New Members of Council Neil Crosby is currently head of Fertilisers and Feeding Stuffs at the Laboratory of the Government Chemist. He was born in Sutton, Surrey, in 1936 and was educated at Bolton School before studying at the University of Leeds, where he was awar- ded a BSc degree in 1959 and a PhD in 1962 for a thesis entitled ”Some Physical Properties of Solubilised Collagens .” He then joined the LGC and worked succes- sively on pesticide residues, water and sewage chemistry, nitrosamines, food additives and contaminants before start- ing his current job some 9 years ago. He was awarded the Fellowship of the Insti- tute of Food Science and Technology in 1977. Mr. Penketh had a long career with ICI, where at various times he was Chief Analyst of the Heavy Organic Chemicals and Petrochemicals Divisions, Chairman of the ICI Analytical Chemists Com- mittee, R & T Administration Group Manager of Petrochemicals and Plastics Division, and Head of Physics and Radio- isotopes Group.On retiring from ICI he became Principal Consultant of Penlee Services Ltd. and Managing Director of Sanderson Chemical Consultants Ltd. He is married with three children. He has travelled extensively for both business and pleasure, and his hobbies include collecting stamps, coins and miniature medals. He is interested in most sports and plays geriatric badminton and lousy golf. In his weaker moments he confesses to be a supporter of Middlesbrough Foot- ball Club. Dr. Crosby was first Honorary Assis- tant Secretary, then Honorary Secretary, of the Education and Training Group of Peter Stevens was born in London in the Analytical Division for 7 years.He is December, 1929. He attended a local also a member of the Analytical Methods grammar school at Wembley and, despite Committee and Chairman of its Medicinal frequent wartime excursions to the air- Additives Sub-committee as well as being raid shelters, qualified for university entry on the Editorial Boards of The Analysr in 1948. Like most of his contemporaries and Food Additives and Contaminants. he had first to complete National Service Dr. Crosby now lives in Watford with in RAF Signals, which he regards as an his wife Margaret, son and daughter. His important part of his education. The recreations include gardening, piano 2-year break made resumption of studies, music, chess, wine appreciation and at Bristol University, an effort but he marathon running.graduated in 1953, writing an undergradu- ate thesis on the attempted synthesis of a George Penketh is Chairman of the North septanose sugar. During this time he East Region of the Analytical Division spent two summer vacations at the Post and is serving on Council for the third Office Research Laboratories at Dollis time. He has served on several of the Hill, and prior to university did 6 months’ Division’s Committees and is currently a routine milk testing with the Express member of the Analytical Methods Com- Dairies at Cricklewood, both useful mittee. He was educated at Stockton experiences. Grammar School and obtained an exter- His first job was in the research labora- nal BSc (London) degree in Chemistry by tories of the Calico Printers Association in evening study at Constantine Technical Manchester, where terylene had recently College (now Teesside Polytechnic). been discovered.He worked on crease proofing of fabrics, and was also involved with the first automatic pleating machine to be used in Britain. He met his wife Ruth, as a fellow resident at the Man- Chester University Settlement, where she was involved in postgraduate social work training. Deciding to begin married life some- where new, he was the first graduate to join the newly created Process Investiga- tion Department at Montrose in January, 1956. Glaxo had established a factory in 1952 to make cortisone, the first synthetic steroid. During 4 years’ development work he took an interest in paper chro- matography. When Glaxo became one of the first British companies to investigate thin-layer chromatography, he applied the technique to the range of steroids then being manufactured at Montrose.His observations made such an impact on the control of production quality that he became a full-time analyst as a result, publishing several notes on the technique as well as a review, contributing to a book on chromatography and lecturing on ster- oid TLC. In 1964 he took over responsi- bility for infrared spectroscopy, another key technique for steroid analysis, and in 1969 began using gas chromatography for steroids. However, the introduction of liquid chromatography in 1974 was of much greater impact for main component assays.The factory had diversified to include the manufacture of cephalosporin antibiotics and a variety of fine chemicals, e.g., salbutamol, an anti-asthmatic drug. He devoted quite a lot of time to environmental analysis in the nineteen- seventies, both by infrared and GLC. In 1980 his Analytical Development Unit was translated to the Quality Assurance Department, and in 1985 he was trans- ferred to administer the Analytical Chemistry Unit, where shift teams and day staff run a wide variety of routine86 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 analyses on over 50 different chemical stages of more than a dozen syntheses. During his career the Montrose factory has expanded from 125 to over 750 employees. He became involved with the Scottish Region of the Analytical Division, RSC, in 1970, when he was invited by John Ottaway to join the Committee as an East Coast Representative. He served three spells, from 1970-72, 1981-83 and 1984- 87, when he became Chairman of the region somewhat unexpectedly, the Chairman designate having migrated to England. He attended his first SAC con- ference in 1971 and was pleased to serve as a member of the Edinburgh SAC 83 organising Committee. His two children are both Scottish graduates, son Howard training in South Wales to become a GP, and daughter Monica teaching at a mission school in Pakistan. His principal leisure enthusiasm is amateur drama and he has just completed 3 years as National Chairman of the Scottish Community Drama Association. He has maintained a lifelong interest in Scouting, is a reader in the Church of Scotland, and a keen gardener. He has just joined MENSA.

ISSN:0144-557X    

DOI:10.1039/AP9892600085

出版商:RSC    

年代:1989

数据来源: RSC

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86 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 Award of Fourth Robert Boyle Gold Medal The Analytical Division’s Fourth Robert Boyle Gold Medal was presented on Friday September 2nd, 1988, at the Town Hall, Eberback, West Germany. The medal was received on behalf of the late Professor Dr. Dr. Dr. h.c. mult. Egon Stahl by his widow, Liselotte Stahl, from the immediate Past President Mr. D. C. M. Squirrell, following addresses by Burgermeister H. Schlesinger and the President of the Division, Professor D. Thorburn Burns. Professor Burns out- lined Boyle’s links with Germany, know- ledge and interest in German chemical matters, and noted that both Stahl and Boyle had many common areas of study, including natural product chemistry and the study of gases. The large gathering included his son, Guests at the ceremony: (R-L) Professor D. Thorburn Burns, Frau Professor L. Stahl, Herr E. Stahl and Dr. P. Koepff many local citizens and representatives of Frau Professor receiving the award from Mr. D. C. M . Squirrel1 the University of Saarlandes, various Stoess Q. Co. Gmbtt, who dealt with the German chemical and pharmaceutical The Division is indebted to Dr. Peter local arrangements and liaison with the societies and industry. Koepff of Deutschen Gelatine-Fabriken Town Hall.

ISSN:0144-557X    

DOI:10.1039/AP989260086a

出版商:RSC    

年代:1989

数据来源: RSC

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ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 87 Analytical Viewpoint ~~ The following is a member of a continuing series of articles providing either a personal view of part of one discipline in analytical chemistry (its present state, where it may be leading, etc.), or a philosophical look at a topic of relevance to chemists in general or analytical chemists in particular. These contributions need not have been the subject of papers a t Analytical Division Meetings. Persons wishing to provide an article for publication in this series are invited to contact the editor of Analytical Proceedings, who will be pleased to receive manuscripts or to discuss outline ideas with prospective authors. The Decline of British Analytical Chemistry: Fact or Artifact? T. Braun,*t A. Schubertt and S.Zsindelyt Institute of Inorganic and Analytical Chemistry, L. Elitvos University, P.O. Box 723, 7443 Budapest, Hungary* and Information Science and Scientometric Research Unit (ISSRU), Library of the Hungarian Academy of Sciences, Budapest, Hungaryf Two recently published studies1.2 have reported a decline in British science, with a third paper bringing new data in favour of the same argument.3 At about the same time, some evidence was presented according to which “Britain is falling behind the major industrialised countries in its investment in academic and related research, which may explain the nation’s declining contribution to world science.”j Whereas reports on the underfunding of British academic research4 seem to be unchallenged, serious doubts have been expressed on the validity of the results on the decline of British science, on the methodologies used and on the supposed cause - effect short-term relationship between the funding of basic research, publication productivity and citation impact .5 Although new data and arguments have been presented,h scepticism seems not to have been removed7 and some newer results do not seem to prove the decline of the functional effectiveness of British academic research, at least for the 1981-198s period.8 In two of the above-mentioned papers,lJ the authors went beyond evaluating the British scientific landscape in general ~ dealing also with some specific fields and sub-fields.British analytical chemistry during the 1981-1984 period was men- tioned as an example of a weak area,l i.e., declining sub-field.2 In the same papers the authors also mentioned a series of sub-fields which they considered “growing” or “stronger” sub-fields, ecology, parasitology, marine biology, etc.As during the last few years we have been dedicating a considerable amount of effort to the scientometric evaluation of the literature of analytical chemistry,g11 we decided to examine whether our own data, databases and methods prove or refute the above-mentioned authors’ results and conclusions on the decline of British analytical chemistry. For the details of the bibliometric or scientometric proce- dures of measuring research performance the reader is referred to previous publications on the topic.1J.8.12 The data on the decline of British research in analytical chemistry1.2 in 1981-1984 were extracted from the National Science Foundation’s “Science Literature Indicators Data Base.” This is compiled by CHI Research (New Jersey) on behalf of NSF for use in the biennial “US Science Indicators’’ report, and is constructed according to a special CHI Research cleaning and unifying algorithm from the Science Citation Index database produced by the Institute for Scientific Infor- mation (Philadelphia).The statement that British analytical chemistry is a declining sub-field’,? is based on two sets of data extracted from the above mentioned database. Firstly, in Table 5 of reference 1, dealing with “Strengths and Weaknesses of British Science Share of World Publications, 1982,” analytical chemistry (with a value of 6.9) is listed as a weak area, i.e., <7% of the world share.Secondly, in Table 6 of reference 2, dealing with “Recent Trends in British World Publication and Citation Shares by Subfield, 1981-1984,” analytical chemistry is listed as a declining sub-field with a percentage change of -12 in the share of papers and -6 in the share of citations for the 1981-1984 period. With these data and the conclusion therefrom at hand, let us turn now to two questions we consider of paramount impor- tance: is such a strongly negative statement according to which the whole national research in a certain sub-field is in decline justified when based on differences of percentages of world publication shares only?; how does the “Science Literature Indicators Data Base” and the data extracted therefrom’ .2 compare with data extracted from our own version of the SCI database12 and from a database more specifically related to analytical chemistry? As to the first question, it is to be accentuated that British analytical chemistry’s decline or “weakness ,” as presented in Table 5 of reference 1 and Table 6 of reference 2, is relative and not absolute.That is why in the titles of references 1 and 2 it would have been by far more correct to write “relative decline. ” The authors would have had to add that in absolute terms (i.e., as related to its own previous publication productivity) British analytical chemistry is not declining. On the contrary, it is increasing (over all the 1981-1984 period). Moreover, judgements from percentage share (of world total) data on publications must avoid interpreting as decline what may have been the effect of diffusion of scientific work.An alternative conclusion from the decreasing percentage share data is that British analytical chemistry research is not sinking but the rest of the world analytical chemistry research is rising, which is considerably different. As a way of answering the second question we considered that a scientometric evaluation of the Analytical Abstracts database would be the most appropriate. As far as we know this is the most comprehensive specialised abstracts journal dealing with the sub-field of analytical chemistry. A manual counting has been performed on the 1981,1982,1984 and 1986 volumes of that journal for publications from the UK, Federal Republic of Germany, France, Japan and the Peoples RepublicANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 88 Table 1.National publication productivities, 1981-1986, based on data from Analytical Abstracts 1981 1982 1984 1986 1981-86. change Country No. O/" No. YO No. O/" No. Y" In 7'0 share A. "/" UK 885 6.78 847 6.79 856 7.56 1003 7.58 11.80 13.33 FRG 836 6.40 788 6.31 766 6.76 785 5.93 -7.34 -6.10 France 368 2.82 359 2.87 292 2.58 399 3.01 6.73 8.4 Japan 1247 9.55 1205 9.65 1063 9.39 1274 9.62 0.70 2.17 China 219 1.67 412 3.30 423 3.73 639 4.82 188.62 191.78 World total 13 045 12 477 11 317 13 230 of China. There are three possible ways of allocating papers to countries: based on first author's country of origin; based on the majority nationality of the different authors; and based on allocating a full authorship to each author from different countries.Our recent studies have shown14 that with productive countries there are practically no differences in adopting any of the first two ways of counting. That is why in the present case the counting was based on the country of origin of the first author. The results are shown in Table 1. It appears, according to our data, that far from the decrease of 12% in the share of British analytical chemistry publications mentioned in Table 6 of reference 2 for the 1981-1984 period, an increase of 11.8% in the relative percentage share and an increase of 13.33% in the absolute number of British analytical chemistry publica- tions has occurred. Compared with the publication productiv- ity of the other countries enumerated in Table 1 the position of British analytical chemistry is a highly respectable one and, with the exception of the change showed by the very substantial Chinese productivity, appears with the highest values of positive changes during the 1981-1986 period.The changes in the Chinese publications productivity in analytical chemistry seem to follow the trend already signalled for the growth of Chinese scientific research in general. 15 As is apparent from Table 1, there is a substantial increase in the publication productivity of British analytical chemistry also in absolute terms. We now turn to the question of whether the citation impact of British analytical chemistry research for the 1981-1985 period is falling behind that of its main competitors (the USA, the Federal Republic of Germany, France, Japan and Canada).Table 6 in reference 2 reports a change of -6% in the share of the citations to British analytical chemistry research during the 1981-1984 period. Instead of looking at percentage shares of citations we have used a recently devised scientometric indicator that we call "relative citation rate" (RCR).8 This is the ratio of observed to expected citations. The observed citations refer to the mean number of citations recorded in our own version of the SCI database12 of the Institute for Scientific Information (ISI, Philadelphia) between 1981 and 1985 to the analytical chem- istry papers published in the same period counted for each of the assessed countries. The expected citations is the mean citation rate per paper published in the 1981-1985 period and calculated for each analytical chemistry journal (see Appen- dix) recorded in our database.The product of the number of papers in analytical chemistry from a given country and the mean citation rate was then calculated for each journal, and the results were summed. Mean expected citation rate of analytical chemistry papers 1 0 1 2 3 4 5 6 Expected citation rate Fig. 1. Relational chart of relative citation rate (RCR) zoning The relative citation rate (RCR) assesses the relative contribution of scientists from a particular country to the average citation rate (citation impact) of the analytical chemistry journals in which they publish. The RCR has a value of unity if the publications in question are cited at the average rate, values between zero and one indicate a lower than average citation rate, and values greater than one indicate that the analytical chemistry articles of the given country have a greater citation impact than the average for the respective analytical chemistry journals. In other words, when applied to the assessment of national performance, this indicator measures each country's contribution relative to the mean citation impacts of the publication channels (journals) they use.As, however, countries may use publication channels (journals) of varying quality, comparisons based on the RCR values alone might be misleading. A two-dimensional rela- Table 2. National publication productivities and citation impact. 1981-1985.based on data from 30 analytical chemistry journals and the SCI database Country UK USA FR Germany France Canada Japan China No. of publications 2120 9846 2272 1669 1137 3783 179 "/a of total 5.74 26.66 6.15 4.52 3.08 10.24 0.48 Expected citation rate 2.98 3.56 1.79 2.85 3.13 2.45 2.35 Observed citation rate 3.38 3.87 1.96 3.00 3.19 2.29 0.89 Relative citation rate (RCR) 1.13 1.09 1.09 1.05 1.02 0.93 0.38ANALYTICAL PROCEEDINGS, MARCH 1989. VOL 26 89 tional chart displaying both observed and expected citation rates is usually more informative. These are orthogonal diagrams and display the “main diagonal” (the straight line x = y , i.e., RCR = 1 .00) and the vertical boundary between “low” and “high” impact analytical chemistry journals, marked by the mean citation impact of the journals considered for analysis (Fig.1). Points in this diagram may be considered to belong to a “higher class” or “lower class” depending on which zone (A-D) they are in. In this sense, the RCR can also be viewed as an indicator of the publication strategy of the country in question, giving information on the quality of the publication channels used by scientists in that country. The indicators computed are presented in Table 2. In addition to the UK and its five main competitors the table contains data for China. This was included mainly to show that although in Table 1 China shows a very high growth of publication productivity during the 1981-1985 period this is not yet accompanied by a similar effect in the comparative (relative) citation impact of the publications.As can be seen in Table 2, the UK appears with the highest relative citation rate of its analytical chemistry publications. Taking into account the RCR indicator alone the values for the UK overtake those of all the other countries in Table 2. However, if we also consider the relational chart in Fig. 2 the picture becomes more diversified. A s is apparent, three countries are situated in the “highest level” zone (A), the US, the UK and Canada, i.e., the analytical chemistry papers by authors from these countries in 1981-1985 were published in high impact journals (high expected citation rate) and were receiving also a high citation rate (high observed citation rate). The chart also reveals that analytical chemists from the UK, Canada, France and China publish their papers in journals of approximately identical average citation rate (impact factor around 3.0, which is higher than the average for the whole field of analytical chemistry, 2.64).The citation reward of these papers is, however, very different with only the UK and Canada situated above the diagonal ( i e . . above the value of RCR = 1.0). 6 I I I I / 4 2 4 I / I / I I I I I I 0 1 2 3 4 5 6 Expected citation rate Fig. 2. papers of seven countries Relational chart o f RCR values for analytical chemistry Although showing an RCR value lower than that for the UK, the relational chart shows that analytical chemistry papers by authors from the US are published in the analytical chemistry journals of highest average citation rate (impact factor: 3.87).On the other hand, although the Federal Republic of Germany shows an RCR value identical with that of the US, its position in the relational chart situates it in the “lower class” (C) zone, i.e., authors of analytical chemistry papers from FRG were rewarded by relatively high observed citation rates although this happened in analytical chemistry journals of low average impact. Based on the data given in Table 2 and Figs. 1 and 2 we can conclude that the relative citation impact of analytical chem- istry papers from the UK was not falling behind the impact of the papers from any of the six countries taken into account. On the contrary, they show up more or less on a par with those from the US, these countries having the leading positions in the comparative assessment for the 1981-1985 period.For assessing the relative impact of British analytical chemistry research during the 1981-1985 period we have also used our newly devised method of subject field characteristic citation scores and scales. 17 Citations to all analytical chemistry papers in the 30 journals of our database for 1981-1985, coded in the SCI as research articles, reviews, notes and letters, have been computed and the distribution of their citation frequency ( X ) has been recorded. The following characteristic scores of the distribution were then determined: Xo is zero; X I is the mean citation rate per paper; X , is the mean citation rate of papers cited above average; and X3 is the mean citation rate of papers cited above X2. These scores have been used to group all the analytical chemistry papers in the database into five categories of degree of citation: Category 0 (see Fig.3) X = x,, Category 1 (see Fig. 3) x E (X,,,Xl) Category 2 (see Fig. 3) uncited papers (papers not cited at all) poorly cited papers (papers cited lower than average) fairly well cited papers (papers cited at least average but below X,) very well cited papers (papers cited not lower than X2 but below X 3 ) outstandingly well cited papers (papers cited not lower than X,) A- E (XI ,x2> Category 3 (see Fig. 3) A- E (X2 3x3) Category 4 (see Fig. 3) XE(X3J Analytical chemistry 36 540 papers 0 2.64 7.51 14.75 (xo) ( x , ) ( X * ) ( x 3 ) W l l l I II I I I I I I1111 I111 111111 1111 1222222n2m21222tmn3m4~ I I I 1 1 I I I I 10 20 30 40 50 60 70 80 90 100% FIA 627 papers 0 1.93 5.58 9.44 1 I I (xo) ( X , 1 ( X 2 ) ( x 3 ) Fig.3. Citation scores and distribution scales for analytical chemistry and flow injection analysis (FIA) papers, 1981-1985: X,,, category (01, uncited; X,, category (1) , poorly cited; X,, category (2), fairly well cited; X,, category ( 3 ) . very well cited; category (4), outstandingly well cited On the basis of the scores defined above, two pairs of diagrams are presented in Fig. 3, the first pair for the whole sub-field of analytical chemistry, the second one for the topic of flow injection analysis (FIA), which is one of the most dynamically expanding areas of analytical chemistry. The first diagram of the pairs shows a linear scale featuring the Xo, X I , X,, X 3 scores characteristic of analytical chemistry and FIA, respectively. The second pair presents a horizontal bar chart indicating the percentage distribution of analytical chemistry, i.e., FIA papers between categories of citedness from 0 to 4.Table 3 presents the percentage participation of analytical chemistry papers from different countries in the first 100 of the group of outstandingly well cited papers (category 4). As can be seen in Fig. 3 this group contains those papers which were cited at least 15 times during the 1981-1985 period. In Table 4, the same data are presented for FIA papers19 which, as is apparent from Fig. 3, were cited at least 10 times during the same period (putting them in cateogory 4).90 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 Table 3.Distribution of the 100 analytical chemistry papers, cited 15 or more times during the 1981-1985 period (see also Fig. 3) Papers in the top category Country of citation, % USA 66 UK 7 France 6 Switzerland 6 The Netherlands 3 Japan 2 Sweden 2 Australia 2 Czechoslovakia 1 Poland 1 Italy 1 Belgium 1 Canada 1 FR Germany 1 In both tables British papers are placed on the top, being exceeded numerically only by papers from the US. Finally, based on the above mentioned measurements, we will try to answer the following two questions. Firstly, is the previously described1.2 decline of British analytical chemistry real, i.e., is the quantity and the impact (quality?) of the scientific output of British analytical chemists decreasing as compared with their previous position and with their main competitors? Secondly, where does the difference between the data in references 1 and 2 and our present results and conclusions come from? Table 4.Distribution of the 61 flow injection analysis (FIA) papers cited 10 or more times during the 1981-1985 period (see also Fig. 3) Papers in the top category Country of citation, O/O USA 22 UK 11 Denmark 8 Sweden 6 Brazil 4 The Netherlands 3 Canada 1 South Africa 1 Venezuela 1 Japan 4 assumption of a short-term, direct, cause - effect relationship between funding and publication productivity and impact4 is highly questionable. On the contrary, there is some evidence that by decreasing funding scientists increase their publication output,2(] and more publications attract, in general, more citations .21 1.2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. References Irvine, J., Martin, B., Peacock, T., and Turner, R . , Nature, 1985, 316, 587. Martin, B. R., Irvine, J . , Narin, F.. and Steritt. C., Nature, 1987, 330, 123. Irvine, J., and Martin, B. R . , Scientometrics, 1989, 15, in the press. Irvine, J . , and Martin, B. R . , Nature, 1986, 323, 591. Leydesdorff, L., Sci. Public Policy, 1988, 15, 149. Anderson, J . , Collins, P. M. D . , Irvinc, J . , Isard, P. A . , Martin, B. R., Narin, F., and Stevens. K . , Sci. Public Policy, 1988, 15, 153. Leydesdorff, L., Sci. Public Policy, 1988, submitted for publication. Braun, T., Glanzel, W., and Schubert, A.. “Proceedings of the Ciba Conference on Thc Evaluation of Scientific Research,” Wiley, Chichester, 1989.Braun, T., Bujdoso, E., and Schubert, A., “Literature of Analytical Chemistry: A Scientometric Evaluation,” CRC Press, Boca Raton, FL, USA, 1987. Braun, T., Fresenius Z. Anal. Chem., 1987, 328, 1. Braun, T., Radioisotopes, 1986. 35, 391. Braun, T., Fresenius 2. Anal. Chem., 1986, 323, 105. Braun, T . , Glanzel, W., and Schubert, A . , “Scientometric Indicators. A 32-Country Comparative Evaluation of Publish- ing Performance and Citation Impact.” World Scientific, Singapore and Philadelphia, 1985. Nye, M. J., ZSZS, 1984, 75, 697. Braun, T., Glanzel, W., and Schubert. A.. to be published. Davidson Frame, J., and Narin, F., Scientometrics, 1987. 12, 135. Schubert, A., Glanzel, W., and Braun, T., Scientometrics, 1987, 12, 267. Guralnik, D.B., Editor, “Webster’s New World Dictionary of the American Language,” Popular Library, New York. RGiiCka, J . , and Hansen, E . 0.. Anal. Chim. Acta, 1986, 179, 1. Whitley, R., and Frost, P. A . , Human Relations, 1971.24, 161. Chew, F. S . . A m . J. Roentgenol., 1988. 150. 227. APPENDIX The Analytical Chemistry Journals Set Used in the Assessment As to the first question, the conclusion from our own results is that the quantity and quality of British analytical chemistry research shows, in the 1981-1985 period, no signs of decline in the dictionary sense of that word18 (to decline = to deterio- rate). Its absolute amount, growth and impact places it at the top of the list of countries enumerated in Table 1 and 2, and at an approximately similar average level to the US.The data and conclusions of references 1 and 2 on the decline of British analytical chemistry, which differ substantially from our own results, can be attributed to the following: the kind and mode of use of the database; the question as to whether decisions on decline (in the dictionary sense) can be based solely on increases or decreases of percentage shares of the world total of items examined (publications and/or citations). As mentioned previously, such changes sometimes give more indication of the growth or decrease of some other components (countries) of the system than on the changes of the real publication productivity and impact of the country examined. It is our opinion that when used for science policy purposes changes in percentage shares of publications and/or citations have always to be used, and interpreted, together with other scientometric indicators.12 A further problem is that the 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. Title Analytical Chemistry CRC Critical Reviews of Analytical Chemistry Journal of Chromatography Journal of Electroanal ytical Chemistry Journal of Chromatographic Science Chromatography Analytica Chimica Acta Journal of Liquid Chromatography Separation and Purification Methods International Journal of Environmental Analysis The Analyst Journal of the Association of Official Analytical Chemists Separation Science and Technology Talanta Journal of Analytical Applied Pyrolysis Impact factor (Citations/paper , 1981-1985) 5.55 4.73 4.14 4.01 3.93 3.35 3.01 2.93 2.62 2.47 2.34 2.17 2.12 2.07 1.72ANALYTICAL PROCEEDINGS.MARCH 1989. VOL 26 91 16. Analytical Letters A 17. Radiochimica Acta 18. Journal of Labelled Compounds 19. Analusis 20. Thermochimica Acta 21. Analytical Instruments 22. Microchimica Acta 23. Journal of Radioanalytical and 1.61 1.35 1.28 1.22 1.17 1.12 1.11 1.09 0.98 0.97 0.91 0.61 0.48 0.02 24. Bunseki Kagaku 25. Microchemical Journal 26. Journal of Thermal Analysis 27. Annales de Quimica B 28. Chemija Analityczna 30. Journal of Analytical Chemistry 29. Afinidad 0.40 (Moscow) I Nuclear Chemistry UK CHEMOMETRICS DISCUSSION GROUP MULTIVARIATE DATA DISPLAY London Zoo, Friday March 31st, 1989 The aim of this meeting will be to illustrate in non-mathematical and tutorial form various techniques for multivariate data display. The speakers will include statisticians and chemists and it is hoped that there will emerge a dialogue on statistical and chemical approaches to tackling chemometrical problems. Invited speakers include Dr. 0. M. Kvalheim-Latent Projections (University of Bergen, Norway), Dr. P. J. Lewi-Spectral Mapping (Janssen Pharmaceutica, Beerse, Belgium), Professor R. Sibson-Projection Pursuit (University of Bath), Dr. C. S. Gutteridge-Canonical Variates (Cadbury-Schweppes, Reading) and Dr. R. G. Brereton-Chernoff Faces (University of Bristol). The fee for members of the group will be f35.00, and to non-members €45.00. For details write to Mr. P. Nolan, Laboratory of the Government Chemist, Queens Road, Teddington, Middlesex. Edited by L. Bretherick Safety Consultant W Hazards in the Chemical Laboratoe has become established as an essential handbook of safety practices, measures and 2s handling dangerous chemicals. Since the last edition was published in 1981 there have been many changes in legislation, regulations, precautionary safety methods and toxicity assessments which warrant publication of this new 4th edition. In addition coverage has been expanded to include material relating to legislation and safety practices in the USA. Protective PVC Binding 618pp Price €2950 ($54.00) ISBN 0 85186 489 9 RSC Members Price €18.00 ORDERING RSC Members should send their orders to: The Royal Society of Chemistry, Membership Manager, 30 Russell Square, to: The Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 lHN, UK. ROYAL SOCIETY OF lnformat on Services 64 London WClB 5DT, UK. Non-RSC Members should send their orders 1 CHEMISTRY

ISSN:0144-557X    

DOI:10.1039/AP9892600087

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

92 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 Silver Medal Lecture The fifteenth Society for Analytical Chemistry Silver Medal Lecture was presented by Professor D. Littlejohn at the Research and Development Topics in Analytical Chemistry meeting held on July 18th and 19th, 1988, in Plymouth Polytechnic. Becoming Absorbed and Excited in Atomic Spectrometry David Littlejohn Department of Pure and Applied Chemistry, University of Strathclyde, Thomas Graham Building, Cathedral Street, Glasgow G I IXL Research in instrumental methods of analysis undertaken by the Analytical Chemistry Research Group at the University of Strathclyde normally can be classified firstly as the develop- ment of novel instrumental techniques, secondly, improve- ments and modifications to existing techniques, and thirdly, the application of commercial instrumentation in clinical, environmental and chemical analysis projects.Although the Group has active research programmes in HPLC, ion chroma- tography, electroanalytical chemistry, the uses of radioana- lytical tracers, etc., most people associate the group with developments in atomic spectrometry. It is, therefore, not surprising that the 15th SAC Silver Medal lecture should be devoted to a review of some recent advances in the use of the electrothermal graphite tube atomiser in atomic spectrometry. To me, this is both an absorbing and exciting subject! The use of a graphite furnace in atomic absorption spec- trometry is now well established and significant improvements in ETA-AAS technology have been achieved in recent years.There have been improvements in atomiser design and the quality of graphite used to fabricate the tube. A greater understanding of the high temperature reactions that take place in a graphite furnace atomiser has been achieved through a variety of sophisticated studies involving kinetic and ther- modynamic modelling, mass spectrometry, etc. Background correction procedures have greatly improved and most modern commercial instruments are able to cope with a reasonably high level of background absorption, hence minimising the influ- ence of interferences. The availability of powerful microcom- puters has resulted in significant automation of ETA-AAS instrumentation, to the extent that in many modern spectro- meters most parameters are set via a keyboard. The topic that continues to attract most attention in ETA-AAS is the control of chemical interference effects.Over the years, the analytical chemistry research group at the University of Strathclyde has worked on a number of approaches aimed at reducing the effect of chemical interfer- ences, particularly in volatile element determinations. Two main approaches can be used to tackle interference effects. Either the interference is prevented by removing the offending matrix species prior to the atomisation stage, or steps are taken to minimise the influence of the interference reaction on the free atom concentration of the analyte. In many situations, a combination of both prevention and cure is required to minimise chemical interference effects. The most common procedure applied to prevent interfer- ences involves the addition of a reagent to the sample at some stage prior to atomisation.This approach is normally called matrix (or analyte) modification. The modifying agent is added to the sample and standard solutions to either assist removal of matrix components at normal char or ash temperatures or prevent loss of the analyte at elevated char or ash temperatures at which the matrix is vaporised. Many different modifiers have been suggested for different volatile elements [e.g. , Mg(N03)2, (NH4j2HP04, Ni, LiN03, etc.], but many recent studies have shown that palladium is an effective modifier for many elements. Palladium has been used successfully on its own or in combination with other modifiers, such as Mg(N03)2, or with a reducing agent in the form of H2 or ascorbic acid." In the determination of gold in blood fractions, a palladium - molybdenum modifying mixture increased the maximum char temperature for gold from 800 to 1200°C without causing a reduction in the sensitivity for gold that is generally encoun- tered when nickel is used as the modifier.4.j It has been shown that palladium is a better modifier than other agents when applied in the direct analysis of solids injected in the form of a slurry into the atomiser.The addition of 700 mg 1-1 of palladium to slurry samples permitted an increase in the char temperature for lead to 1000 "C in the analysis of fish, liver, pea and kale.6 Various procedures have been used to limit the effects of interference reactions on analyte atoms in a graphite furnace.Most approaches involve the modification of Massmann-type atomisers to allow vaporisation into a higher temperature environment than would be achieved on volatilisation from the tube wall in the conventional manner. The most commonly applied modification is the insertion of a graphite platform into the tube, from which the sample is vaporised during the atomisation stage.' Under optimum conditions, the platform is heated mainly by radiation from the tube and this results in a delay in the vaporisation of the sample. It is generally assumed that this delay will ensure that the analyte species will experience a higher vapour temperature than would have been possible if volatilisation had taken place directly from the tube wall.Vaporisation into a higher temperature environment is known to be beneficial for the reduction of interferences caused by a number of halide salts and may also be beneficial in promoting atom formation for some analytes. An alternative method of achieving high temperature vaporisation in a Massmann-type furnace is the use of a probe rather than a platform. With probe atomisation,s.q the heating of the vaporisation surface (the probe) is separated in time from the heating of the furnace tube. It is therefore easier to have control over the vapour temperature that the analyte and matrix species experience on volatilisation. With the probe, the sample is deposited on to the probe head while it is located in the tube. The specimen can be dried and charred or ashed to remove some of the matrix (with or without the use of a modifier).The probe is then removed from the tube, which is then heated and the probe re-introduced once the temperature has stabilised at the required value. Both the platform and probe procedures are successful at reducing interferences caused by chloride salts, but there isANALYTICAL PROCEEDINGS. MARCH 1989, VOL 26 93 some evidence to suggest that interference reduction is achieved with platform atomisation through temporal separa- tion in the volatilisation of the analyte and matrix as much as by an increase in the effective gas temperature at the time of vaporisation. A two-line lead atomic absorption procedure has been used to obtain an estimate of the vapour temperature experienced by lead atoms with wall, platform and probe atomisation in a Philips SP-9 atomiser.lO,ll The peak height signals for the two lead lines were used to calculate the vapour temperature and it was shown that there was no significant vapour temperature advantage of either platform or probe atomisation over wall atomisation at temperatures lower than 2400 “C.At higher temperatures, significant increases in the vapour temperature experienced by the lead atoms were achieved using probe atomisation, but there was only a margin a 1 i m pr o ve m e n t with p 1 at f or m atom i s at ion, If the vapour temperature experienced by atoms is not substantially greater with platform atomisation compared with wall atomisation, why is it that the platform performs much better in reducing interference effects‘? The most likely explanation is the slight temporal separation that can be achieved in the vaporisation of the analyte and matrix species with platform atomisation.Studies of the time resolved analyte absorption and background absorption signals for lead and gallium in the presence of different chloride salts have shown that in most instances, the best temporal separation of the two signals is achieved with the platform.10 With probe atomisa- tion, the signals for both the analyte and background absorp- tion are narrow, suggesting fast vaporisation rates. When operated at the same atomiser temperature, platform atomisa- tion gives broader peaks, indicating a slower rate of vaporisa- tion. Although only slight temporal resolution of analyte and interferent species is achieved with current designs of probe. effective interference control can be achieved provided the atomiser is set to a temperature of 2500°C or above for all elements.Under such conditions, better performance is often achieved than for platform atomisation. It is ‘mportant to stress that the philosophy of probe atonisation requires that a different approach is taken to the selection of atomiser conditions in comparison with conventional wall atomisation or platform atomisation. Conditions should be selected to minimise interferences and not necessarily to maximise sensi- tivity. This is normally a reasonable approach as in most analyses accuracy is more important than sensitivity. The suitability of probe atomisation for the direct analysis of various samples has been illustrated in studies conducted by the Analytical Chemistry Group at the University of Strathclyde.Spinach,” sediments,g blood and urine samples’’ and plasma protein solution12 have been analysed successfully by using a Philips autoprobe assembly. The elements determined include cadmium, cobalt, chromium, copper, manganese, nickel and lead. Table 1 gives results for the direct analysis of a urine standard, obtained by using aqueous solution calibration and peak area measurements. Table 1. Analysis of Lanonorm metalle 1 (Lot 625202) synthetic urine by probe - ETA-AAS with direct aqueous calibration Concentrationiwg 1 Cd CO Ni Pb Element Probe Assigned Confidence range 3.4 k 0.2 2.9 2.4-3.4 5.7 k 1.7 5.3 4.G6.5 4.6 k 0.5 4.2 3 5-4.9 24 k 3 22.2 19.4-25.0 Besides providing vaporisation into a high temperature environment, the probe concept allows other developments of interest in electrothermal atomisation.It is possible to deposit analyte metals electrochemically on to the probe surface for pre-concentration and extraction of the analyte from the sample matrix.I3 This possibility has been illustrated for the determination of lead in sodium chloride solutions. It has also been possible to provide separate electrical heating of a probe when inserted into a graphite furnace. l 4 The aforementioned interference comparison for platform and probe atomisation indicated that the heating rate of the platform under normal operating conditions was much slower than that of the probe, particularly at the atomisation temperatures of volatile ele- ments, and this allowed temporal resolution between the vaporisation of analyte and matrix in some instances. It would therefore seem desirable to have the possibility of controlling the heating rate of the probe, as well as achieving vaporisation into a high temperature environment.This approach is currently under investigation in our laboratory. When one considers the fairly substantial developments that have been achieved in electrothermal atomisation, it is perhaps not unreasonable to suppose that in the future, more uniform atomiser programmes will be used for the determination of different elements. Traditionally, it has been necessary to optimise the atomiser programme for each individual element ~ selecting quite different char and atomisation temperatures for volatile and refractory analytes. However, ETA-AAS meth- odology and instrumentation have now progressed to a point where it is possible to imagine the use of a simple and rapid programme for the determination of most elements.Injection of the sample into a hot furnace tube can be performed with many atomisers, reducing the dry time to less than 5 s in most instances without significantly affecting signal precision. 15 The use of a universal modifier such as palladium, in conjunction with hydrogen, should allow the application of a standard char temperature of at least 1000 “C for most elements. In order to achieve optimum performance with probe atomisation it is necessary to use temperatures in excess of 2500°C.It would therefore seem reasonable to select a standard atomisation temperature for all elements of, for example, 2700°C. With separate electrical heating of the probe, higher probe temper- atures and greater control of the heating rate would probably extend the use of this device to refractory elements as well as volatile and medium volatile analytes. Table 2. Analysis of chemical samples by FANES (helium discharge) Concentration/pg ml- I Sample Anal yte FANES Other Antifreeze P 1500 1560 WCA fabric B 140 175 Acetic acid based Si 5.5 <9 (5.5)” 200-300 liquor (ex Br 252 process) Fe 1.1 2.2 Terephthalic acid Co 169 179 Mn 428 440 * Obtained by probe electrothermal AAS at Strathclyde. Furnace Atomic Non-thermal Excitation Spectrometry One of the most interesting and “exciting” developments in electrothermal atomiser technology in recent years has been the introduction of the FANES atomiser by Falk and col- leagues.16 This furnace has similar characteristics to conven- tional electrothermal atomisers, with the exception that it can be evacuated to a low pressure (1&20 torr), and a hollow- cathode discharge is established within the atomiser volume using the tube as the cathode in conjunction with an anode at the end of the tube.” When helium is used as the atomiser purge gas, it is possible to excite both metals and non-metals and measure atom and ion emission signals. A list of detection limits achieved with the FANES atomiser in our laboratory has been published recently’s and Table 2 gives details of analyses performed on a variety of industrial samples.Excitation94 ? ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 - - - 120 .g 100 ‘(0 2 v) C a +d Y a - 8 0 60 600 z u) C a c .- c .- 2 500 a al r Y fu a .- 400 300 40 0 20 40 60 80 100 Discharge current/mA Fig. 1. Effect of discharge current on magnesium atomic emission intensity (FANES conditions: helium 15 torr; 2500 ‘C; 0.2 ng of magnesium; 285.2 nrn). U, Peak height; 0, peak area The FANES technique clearly has great potential for use in simultaneous multi-element analysis at trace concentrations. The fact that the atomiser head can also be used for conventional ETA-AAS adds to the attraction of the device. It should be possible further to improve the performance of FANES by implementation of standard ETA methodology, particularly at the dry and char - ash stages.The use of oxygen ashing and matrix modifiers are equally applicable to FANES and it would be interesting to investigate the contribution that platform atomisation can make to reducing chemical interfer- ences at low pressure. It is not possible to use conventional platforms in a FANES tube because the platform is sucked from the tube during the evacuation stage. However, it should i cn w ‘E 1000 2 2 .= 800 e s= ‘v, 600 - 3 - .Id - C a, C * .- c 400 - .- cn u) .- E IJJ 200 - 30 40 60 80 Cu rren tim A Fig. 2. Effect of discharge current on chlorine ionic emission (FANES conditions: helium 15 torr; 1000 “C; 400 ng of chlorine as MgCI,; 479.5 nm). 0, Peak height; +, peak area be possible to devise a means of delaying atomisation until a higher thermal temperature is achieved, which should assist in the removal of some chemical interference effects.As the FANES atomiser is operated at low pressure, analyte vaporisa- tion occurs at a few hundred degrees lower than at atmospheric pressure. It is possible that with careful selection of the atomisation temperature and heating rate, separation in the volatilisation of the analyte and matrix could be achieved for some samples, reducing the likelihood of chemical interfer- ences in the vapour phase. In order to achieve automatic background correction, the FANES system in our laboratory is operated in conjunction with an echelle spectrometer modified for wavelength modula- tion.2” The movement of the refractor plate placed behind the entrance slit is carried out via a scanner controlled by an IBM microcomputer.Besides giving details of the height and area signals for both analyte and background emission, a variety of “data-station” facilities are available for the investigation of FANES signals.18 As the production of FANES signals is quite rapid in comparison with conventional ETA-AAS, fast modu- lation frequencies are used and analysis is normally performed on the basis of peak area signals. Clearly, FANES has great scope for use in both metal and non-metal determination in either sequential or simultaneous multi-element analysis. Although improvements to the atomiser design can be made, there is sufficient evidence to suggest that the technique has considerable potential for future development.Indeed, if a FANES atomiser is operated with a high resolution spec- trometer with wavelength modulation, it is possible to envisage a system that would allow either simultaneous multi-element analysis by FANES or by continuum source atomic absorption spectrometry (CSAAS)20 when the atomiser is operated at atmospheric pressure and a high intensity continuum lamp is added to the instrument. In both conventional ETA-AAS and the FANES derivative there are many discoveries yet to be made, sufficient to keep the subject of electrothermal atomic spectrometry both absorbing and exciting, as far as I am concerned, for many years to come. References 1. Shan, X.-Q., and Kaijin, H., Talanta. 1985. 32. 23. 2. Schlemmer, G., and Welz, B., Spectrochirn. Acta, Part B , 1986, 41, 1157.3 . Voth-Beech, L. M., and Shrader, D. E., J. Anal. At. Spectrom., 1987, 2, 45. 4. Egila, J . , Littlejohn, D., Ottaway, J . M., and Shan, X.-0.. J . Anal. At. Spectrorn., 1987, 2, 293. 5. Shan, X.-Q., Egila, J . , Littlejohn, D., and Ottaway, J . M., J . Anal. At. Spectrorn., 1987. 2, 299.ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 In the years that have elapsed since the RSC published Isotopes: Essential Chemistry and 1 Applications in 1980 there have been many changes and developments which warrant publication of this edition, This book covers the synthesis of a wide range of isotopically labelled compounds, the analytical methods used and many important applications. Contents: Organic Synthesis with Short-lived Positron-emitting Radioisotopes; Radioiodination Techniques; The Radiochromatography of Labelled Compounds; Modem Spectrometric Methods for the Analysis of Labelled Compounds; Localization and Quantitation of Radioactivity in Solid Specimens Using Autoradiography; Isotope Shifts in NMR Spectroscopy Measurement and Applications; The Use of Stable Isotopes in Medicinal Chemistry; Radiopharmaceuticals; Isotopes in Molecular Biology; Industrial Applications of Radioisotopes.95 6 i 8. 9. 10. 11. 12. 13. Lynch, S.. and Littlejohn. D.. J . Anal. A t . Spectronz., submitted for publication. Slavin. W., and Manning, D. C., Prog. Anal. Spectrosc.. 1982, 5. 233. Littlejohn. D.. Lab. Pract.. 1987, 36 (lo), 121. Corr. S . P.. and Littlejohn. D . , I . Anal. A t . Spectrom., 1988.3. 125. Ajayi, 0. 0..and Littlejohn, D., I . Anal. A t . Spectronz., submitted for publication. Ajayi. 0. 0.. Littlejohn, D., and Boss, C. B., Anal. Proc.. 1988, 25, 75. Ajayi. 0. 0.. and Littlejohn, D., J . Anal. At. Spectroni.. submitted for publication. Littlejohn, D., Ajayi, 0. 0.. Egila, J . , Cooksey, B. G., and Pasullean, B., in preparation. 14. 15. 16. 17. 18. 19. Quinn, A. M.. Nichol, R., Miller, L., Little~ohn, D., and Marshall. G. B.. Anal. Proc.. 1988. 25, 95, Kunwar, U. K.. Littlejohn. D., and Halls. D. J . , A d . Proc.. submitted for publication. Falk. H., Hoffmann, E.. and Ludke, C.. Specrrochim. Acra. Purr B , 1984, 39, 283. Littlejohn, D., Carroll, J., Quinn, A. M., Ottaway, J . M.. and Falk, H., Fresenius Z. Anal. Chem., 1986. 323, 762. Littlejohn, D., Anal. Proc.. 1988, 25. 217. Falk, H.. in Caroli. S . . Ediror, "Improved Hollow Cathode Lamps for Atomic Spectrometry," Ellis Horwood Ltd. ,- Chi- Chester, England, 1985. Chapter 4. O'Haver, T. C., Harnly. J . M.. Marshall, J . , Carroll, J . , Littlejohn, D.. and Ottaway, J . M., Analyst, 1985, 10. 451. 20. ISOTOPES: ESSENTIAL CHEMISTRY AND APPLICATIONS I1 Edited by J.R. Jones, University of Surrey ISBN 0 85186 746 4 Special Publication No. 68 (1988) Softcover 272 pp. Price E39.50 ($79.00) ROYAL CHEMISTRY lnformat ion Services For further information, please write to: Royal Society of Chemistry, Sales and Promotion Department, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF, UK. To Order, please write to Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 lHN, UK. or telephone: (0462) 672555 quoting your credit card details. We can now accept Access, Visa, Mastercard & Eurocard. RSC Members are entitled to a discount on most RSC publications and should write to: The Membership Manager, Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridee CB4 4WF. UK.

ISSN:0144-557X    

DOI:10.1039/AP9892600092

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 96 Ronald Belcher Memorial Lecture The fifth Ronald Belcher Memorial Lecture was presented by Dr. J. M. Slater at the Research and Development Topics in Analytical Chemistry meeting held on July 18th and 19th, 1988, in Plymouth Polytechnic. Membrane Design and Photocuring Encapsulation of Flatpack Based Ion-sensitive Field Effect Transistors Jonathan M. Slater" School of Chemistry and Applied Chemistry, University of Wales College of Cardiff, P.O. Box 912, Cardiff CFI . . 3TB" The recent advent of inexpensive computing power has led to a metamorphosis of analytical instrumentation with dramatic changes in the way that experiments are controlled and the analytical data processed and displayed. However, while the size and cost of the microcomputers required has dropped substantially, the sensing instrumentation has remained rela- tively unchanged.Ion-sensitive field effect transistors (ISFETs) offer the tantalising opportunity of using the same technology as the microchip revolution to produce small low-cost sensors. ISFETs are often viewed as the logical progression from conventional ion-selective electrodes (ISEs) which are analy- tically useful but bulky, have a high output impedance and are not particularly well suited to low-cost mass production. 1.2 The new technology challenger is small and has a low output impedance but the hurdle of reliable low cost mass production remains. The approach described in this paper is to utilise a low-cost, industry standard package in conjunction with photoimaging encapsulation and ion-sensitive membrane application methods to exploit the advantages of the device and minimise the tedious produotion requirements associated with labora- tory prototypes.Methodology Encapsulation ISFET devices require encapsulation to isolate and protect all of the sensor chip electrically, apart from the chemically sensitive gate regions, from the measuring environment. Photoimaging encapsulation promises to be compatible with the microfabrication techniques used to produce the electronic chip and with this methodology two options exist, either a photoimaging encapsulant or a photoimaging pattern. The patterning method was developed for this work because it allowed a much wider range of encapsulating agent to be considered.3 Photocured Polymeric Membranes In classical ISE work, poly(viny1 chloride) (PVC) has been the matrix material for some of the most successful electrodes to date.4-6 PVC matrix ion-sensitive membranes have exclusively been formed by solvent casting techniques. Typically, the membrane components are dissolved in a volatile solvent, such as tetrahydrofuran (THF). Although this is convenient for macro-electrodes, the volatile cocktail is difficult to handle on a micro-scale and prone to absorbing moisture from the atmos- * Present address: Centre for Analytical Science, Birkbeck College, 29 Gordon Square, London WClH OPP. phere which weakens the ISFEThembrane bond. As an alternative to PVC, a series of photocuring acrylate type matrixes which polymerise in situ on the ISFET gate were examined.This eliminates the need for a solvent while maintaining compatibility with the microfabrication pro- cedures required for successful mass production. Experimental Sensors A dry film photoresist (Riston 100, DuPont Ltd.) was employed as the encapsulation patterning agent. The Riston was applied several times to the surface of a wafer of ISFET chips and laminated to produce photoresist pillars above the gate regions of the ISFET devices. The wafer was subsequently diced to produce individual ISEFT chips, which were mounted into flatpack mounts (Shinko 16-pin ceramic package) using cyanoacrylate adhesive (Threebond Ltd.) and a specially engineered alumina spacer, which ensured that the pillars were level or slightly above the package surface [Fig.l(a)]. (a) Wire bonds device ISFET gate (bl regions Encapsulant ' 5 w O O pm f Carrier Fig. 1. Wire bonded chip in carrier with Riston pillars (a) before and ( b ) after encapsulation with Epoteck H54 low viscosity epoxy material The device was wire bonded to make an electrical connection and the package flooded with low-viscosity epoxy (Epoteck H54 or other suitable encapsulant). The encapsulant was cured according to the manufacturer's direction and lapped, if97 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 Table 1. Cocktails used for membrane fabrication. Photocured membrane cocktails (4-7) contained 4% benzoyl peroxide and 2% benzoin methyl ether. Components for solvent cast membranes (1 and 8) were added to 3 cm3 of THF - cyclohexanone (1 + 1 ViV) Polymer Membrane Primary (or monomer) No.ion based (% used) 1 Potassium PVC(34) 2 Calcium 3 Calcium 4 Calcium 5 Calcium 6 Calcium 7 Calcium 8 Calcium Loctite 350(32) Loctite 350(60) Butyl Butyl Butyl Butyl methacrylate(45) met hacry late (45) methacrylate(45) methacrylate(45) PVC (32) Solvent mediator (YO used) DOA*(64) DOPPI(60) DOPPt(32) DOPPi(5O) TOPS(50) TPPT(5O) DBPII(5O) DOPP(60) Sensor (YO used) Valinomycin( 2) Calcium salt**(8) Calcium salt**(8) Calcium salt * ( 5 ) Calcium salt* * ( 5 ) Calcium salt * * ( 5 ) Calcium salt*"(5) Calcium salt**(8) * Dioctyl adipate. t Dioctylphenyl phosphonate. $ Trioctyl phosphate. 1 Tripentyl phosphate. )I Dibutyl phthalate. * * Calcium bis{ di[4-( 1,1,3,3-tetramethylbutyI)phenyl]phosphate} Remarks Flexible and non-tacky.Used for system optimisation Sticky membrane with considerable surface exudate Flexible, non-tacky and functional ISFET Slightly sticky but hard membrane of good physical strength and Slightly more tacky, but otherwise similar to membrane 4 good adhesion to chip surface. Good ISFET function (Table 3) Very sticky due to incomplete photopolymerisation. No ISFET Similar to membrane 6 function Flexible and non-tacky membrane of limited adhesion to chip surface. Used as control (Table 3) required, fully to expose the Riston pillars, which were stripped with the proprietory chemical stripper. This resulted in two craters, into which electroactive membrane mixtures could be applied [Fig. l(b)]. Apparatus The flatpack sensor mount allowed full advantage to be taken of the small dimensions and planar surface of the device in designing an FIA manifold to interface sample fluids with the sensor.The flow cell was machined from perspex and utilised a wall jet design in order to minimise the sample volume required; it also incorporated a quick-release mount for the sensor flatpack and a silver - silver chloride reference electrode and is described in detail elsewhere.3 The sample propulsion was effected by a multi-channel peristaltic pump (Ismatec MP13 G-J-4). Sample injections were made with an automated rotary valve (Valco Instruments, N60) controlled by a micro- computer via a home-built interface unit. All connecting tubing was of PTFE (nominal i.d. 1.27 mm). Generally, measure- ments were made at 25 "C in a constant drain current mode (500 FA), achieved by a feedback loop to the reference electrode.The required Vref was recorded on a y - t recorder (Linear Instruments, Model 0555-DPPP) and logged by the microcom- puter. Membranes The FIA system developed was initially characterised and optimised by using conventional ionophore-doped PVC matrix membranes. The membrane layers were applied by solvent casting three measured portions of membrane cocktail (Mem- brane 1, Table 1) at 6-h intervals. Photocured polymeric membranes were prepared from two monomer bases, namely Loctite 350 photocuring adhesive and butyl methacrylate. The Loctite adhesive already contained initiator but for the butyl methacrylate benzoin methyl ether (to produce radical initiation at 349 nm) and benzoyl peroxide were used.Results and Discussions Flow characteristics of the systems were optimised by using classical PVC - valinomycin potassium sensitive membranes (Table 1, membrane 1). A sample volume of 30 mm3 was used for measurements (selected from trials with 10, 30 and 60 mm3 volumes) as maximum signal amplitude was not achieved at the lower sample volume and doubling the sample loop size gave only a marginal increase in signal amplitude. The characteristics of the flow cell determined the magni- tude of the signal with various flow-rates. As the flow-rate increased to 1 cm3 min-1 the diffusion layer decreased, thereby increasing mass transport to the electrode surface. However, at high flow-rates the signal decreased as the sample residence time was too short to allow the maximum sample concentration to diffuse to the surface. Hence, the plateau region of 1 cm3 min-l was adopted for all determinations.All of the sensors were conditioned by pumping a 0.1 M solution of the primary sensor ion chloride over the detector for a period of 15 min before calibration, although calibration traces showed that usually a period of a few minutes was sufficient. A comparison of initial drain current and slope values (Table 2) for conventional and Riston patterned encapsulation shows more consistent data for the latter devices at a fixed reference electrode potential, indicating that the use of Riston as a height-matched encapsulation aid in conjunction with flat-packs facilitates the rapid and reproducible produc- tion of FIA sensors. Table 2.Some parameters, measured at 25"C, of conventionally encapsulated and Riston patterned encapsulated devices with mem- brane (1) Conventional Riston patterned encapsulation encapsulation Individual sensors Mean,? . . . . S.d. . . . . Id*lmA . 1.44 1.67 1.67 1.62 1.67 . 1.52 . 0.159 S+lmV decade - 1 56.8 54.5 53.5 55.4 54.2 54.88 1.137 I,*lmA 1.42 1.38 1.37 1.37 1.38 0.021 - StlmV decade ~ I 57.2 57.1 57 .o 57.1 57.1 - 0.071 * Drain current after 1Omin conditioningin 10- I M potassium chloride i- Determined for first calibration after conditioning. at Vret = 1 V. As an alternative to PVC, a series of photocuring mem- branes which polymerise in situ on the ISFET gate were examined. These offer the advantage of eliminating the solvent compatibility with the microfabrication procedures needed for98 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 ~~ Table 3.Some characteristics of calcium ISFETs with butyl methacrylate matrix membranes Solvent mediator (membrane no.) Property DOPP (4) TOP ( 5 ) Appearance . . . . . . . . Detectionlimith . . . . . . Slope at 25 “C/mV decade ~ Lifetimeid . . . . . . . . . . (withs.d.) . . . . . . . . k&:t.Mg* . . . . . . . . . . kgtt,K . . . . . . . . . . . . kE:t,Na . . . . . . . . . . Usable pH range . . . . . . . . Slightly sticky, transparent 1 x 10-1-2 x 10-5 26(0.41 for n = 4) >28 8 x 10-3 8 X 10- 4-95 1.85 X Tacky, transparent 1 x 10-1-1 x 10-4 20( 1.23 for n = 4) 5-10 6 x 10-3 1.2 x 10-1 1.25 x 10-’ 4-9.5 * Determined by mixed solution method at [interferent] = 10-3 M.PVC/DOPP (8) TPP (6) DBP(7) (control) Very sticky Very sticky Transparent - - 5 x 10-6 - - 30(0.75 for n = 5 ) - - 10-20 - - 6.2 x 10-3 7.2 x 10-3 - - 4.9 x 10-3 - - - - - mass production in order to reduce unit cost. The first material examined was Loctite 350. This is an engineering adhesive designed for bonding glass. It had been evaluated as a potential encapsulant and demonstrated good adhesion to the silicon nitride surface of the ISFET device.3 Incorporating sensor and solvent mediator in this matrix offers the possibility of a highly adhesive photo-patterning membrane whilst the cross linking during polymerisation may minimise leading of electroactive components. Membrane 2 (Table 1) contained similar proportions of polymer solvent mediator to the optimum corresponding PVC matrix membrane (8).This membrane polymerised in ultra- violet light but remained tacky, with macro-membranes exhibiting considerable surface exudate. Membrane 3, with an increased Loctite 350 matrix content, polymerised to produce a flexible, non-tacky macro-membrane and a functional ISFET membrane. The ISFET device, when calibrated in the FIA system with various metal chlorides, was unsatisfactory with respect to slope (12 mV decade-’), detection limits and selectivity towards sodium and potassium. Four types of membrane were prepared using a butyl methacrylate polymer base (Table 1,4-7). Membranes 6 and 7 , using the solvent mediators tripentyl phosphate and dibutyl phthalate, failed to polymerise completely (Tables 1 and 3), suggesting poor solvent mediator polymer compatibility and/or interference in the photo-polymerisation process.ISFET responses were unobtainable (Table 3). The ISFET sensors were conditioned for about 8 min by pumping a solution (0.1 M) of primary ion chloride over the sensors before measurements. The conditioning profile could easily be followed and only brief periods of 6-12 min were required in order to obtain a steady base line. Calibrations were carried out on primary ion chloride standards. The over-all performance is summarised in Table 3. Measurements on the variation of pH for the photocured poly(buty1 methacrylate) system show that the working range lies between pH 4 and 9.5, which compares favourably with the PVC matrix based membranes (Table 3). The working lifetimes of the ISFETs reflected both the physical characteristics and electro- chemical performance of the membranes. The PVC ISFET showed little deterioration in use over 10-20 d until erratic performance indicated physical detachment of the membrane and failure.In contrast, the butyl methacrylate and Loctite 350 membranes did not fail physically over 6 months, but the lifetime associated with use was curtailed by deterioration in the electrochemical performance. The butyl methacrylate matrix membrane (No. 4) had initial slopes of 26 mV decade-’, which did not change appreciably over a 28-d period. However, in days 2848, the slope decreased to 24 mV decade-’, followed by an erratic response indicating breakdown. These type 4 membranes did not exhibit a loss of transparency which was observed with the Loctite matrix membrane and indicated water uptake.7 It is possible that the eventual electrochemical failure of these membranes was due to leaching of electroactive components.Chemical grafting of sensor - solvent mediator to the polymer matrix could circumvent leaching, and although time consuming on the macro-scale, it might be useful for mass-produced micro-devices . The use of Riston as a height matched encapsulation aid in conjunction with flatpacks facilitates the rapid and reprodu- cible production of ISFET sensors for use in FIA. Acrylate based membrane matrix materials are superior to PVC for simplifying fabrication and for adhesion of ion-sensing mem- branes to ISFET gates. From among the acrylate-type mat- rixes, the butyl methacrylate - dioctylphenyl phosphonate - calcium bis{ di[4-( 1,1,3,3-tetramethylbutyl)phenyl]phosphate} sensor system produces the best electrochemical characteris- tics.These qualities and the lifetime of 21 d of this ISFET sensor makes photocuring butyl methacrylate a useful alterna- tive matrix material, especially in view of the ease of fabrication. The Science and Engineering Research Council is thanked for a studentship within the CASE scheme in conjunction with AERE Harwell, whose great interest and work in production of ISFET devices is greatly appreciated. The author also thanks his supervisors, Dr. J. D. R. Thomas and Dr. G. J. Moody, for their enthusiastic help and counselling during these studies. 1. 2. 3. 4. 5. 6. 7. References Janata,J.,andHuber,R. J.,Zon-Sel. ElectrodeRev., 1979,1,31. Janata, J., and Huber, R. J., in Freiser, H., Editor, “Ion- Selective Electrodes in Analytical Chemistry,” Volume 2, Plenum Press, New York and London, 1980, p. 107. Moody, G. J., Slater, J. M., and Thomas, J. D. R., Analyst, 1988, 113, 104. Moody, G. J., Oke, R. B., and Thomas, J . D. R.,Analyst, 1970, 95, 910. Moody, G. J., and Thomas, J. D. R., in Freiser, H., Editor, “Ion-Selective Electrodes in Analytical Chemistry,” Volume 1, Plenum Press, New York and London, 1978, p. 339. Moody, G. J., and Thomas, J . D. R., in Covington, A. K., Editor, “Ion-Selective Electrode Methodology,” Volume 1, CRC Press, Boca Raton, FL, 1979, p. 11 1. Slater, J. M., PhD Thesis, University of Wales, 1987.

ISSN:0144-557X    

DOI:10.1039/AP9892600096

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS. MARCH 1980. VOL 26 99 Laboratory Information Management Systems The following are summaries of five of the papers presented at a Meeting of the East Anglia Region held on May 5th, 1988, held at Messrs. Smith, Kline and French, Welwyn Garden City, Hertfordshi re. Current and Future Impact of LIMS in Quality Control A. A. Wagland Roche Products Limited, Welwyn Garden City, Hertfordshire The past few years have seen an enormous growth in the amount of data that has to be stored by the quality control departments within the pharmaceutical industry. These data must be carefully recorded in an easily readable form, they must be thoroughly checked and approved by a responsible person and must be stored for a number of years. Frequently, records are hand-written and the various documents created from them involve transcription of data with all the concomi- tant risks of error.Some 10 years ago, the possibility of computerising a control laboratory system with the aims of avoiding unnecessary transcription, increasing legibility. decreasing manual checking and increasing laboratory efficiency, was remote. Design and Implementation At this time, no quality control orientated system was commercially available; indeed, no LIMS system appeared to exist at all, especially if it was not IBM-based and, therefore, acceptable to data-processing management. In order to minimise the impact of computerisation on the laboratory staff, a system has to be designed initially to be relatively simple and as similar to an existing manual system as possible.At the same time one must be cognisant of the fact that the system should be as universal as possible, requiring only the minimum of customisation for use by other potential users. Certain major decisions have to be made at this time. For example. one may decide: (i) to restrict the system to the control laboratory; (ii) not initially to consider stability studies, customer services or research services; (iii) not initially to consider direct links with other computer systems within the company; and (iv) not initially to attempt to link with instruments. These decisions may be made in order to: ( i ) simplify design, installation and testing; (ii) minimise costs of programming; and (iii) avoid using a relatively large computer for both database management and data acquisition in order to maintain real-time speed.Nevertheless, these future require- ments must be kept in mind by ensuring that the system could be easily expanded to encompass them later. Finally, certain positive requirements have to be incorporated. The system must: (i) be easily understood by the users; (ii) be ‘user friendly’; (iii) be as secure as the existing manual system; (iv) save time; (v) be cost effective; (vi) enhance the management of the laboratories; (vii) satisfy the requirements of the regulatory authorities; (viii) improve data retrieval; (ix) produce Certificates of Analysis; (x) make provision for specifications; (xi) check results against relevant specifications; (xii) provide adequate backup facilities; and (xiii) work in real time.Our first system. using a Perkin-Elmer 3210 computer with six terminals and three printers, was operational in about 4 months. The computer had two megabytes of main memory and an 80 megabyte data storage disk of which the database occupied 40 megabytes. This system was used to explore the capability of QC - LIMS. A few errors in design were found and rapidly rectified. A few months later, a second, improved version was installed and used real time, initially alongside the manual system but soon replacing it. It was found that this manual system provided an adequate fallback if computer failure occurred. Impact of the System in Use Ease of Use Understanding and user friendliness are very subjective. Essentially these terms imply that the user, particularly the laboratory staff, should not have to learn a lot about computers.nor should they need much training; the system should tell them what to do. This ease of use is achieved by careful design of screens and by the use of “help” screens where needed. In practice, all we had to do was to train the analyst how to log into the system and in the use of certain security codes. More training was needed at the quality manager level because he had to make more decisions and had to be able to design his own ad hoc reports. Fortunately, the designer of the system and the system manager were deeply involved with the original design and were already familiar with computers and their operation. Perhaps the most difficult part of implementa- tion is the establishment of the fundamental data-sets on which the operation of the system depended.The establishment of the product specifications is, to some extent, naturally tedious. It came as a pleasant surprise to find that writing specifications was easy because the system prompted the writer for all possible items. Indeed, after a short time and with a little training, the job was given to a secretary to perform. Security Any quality control system used by the pharmaceutical industry must be secure in two aspects. Firstly. it must have security of access at different levels in order to prevent unauthorised persons performing tasks which they are not allowed to do. Secondly, the data must be secure so that unauthorised persons cannot alter the contents of the database once these have been confirmed.Of course, the system manager must have access to the whole system for maintenance purposes and he must, therefore, have access to all the data within the system and be fully familiar with the need for security. In practice, we found that the security systems offered by Perkin-Elmer were completely adequate. To date we have not found any unauthorised access to the system. nor have unauthorised changes been made. This can be checked in100 ANALYTICAL PROCEEDINGS. MARCH 1989, VOL 26 several ways, the best of which is by the use of an automatic audit facility . Time Saving It is very difficult to estimate how much time can be saved by replacing a manual by a computer system. In fact, at the analyst level, little if any time is saved because he has, at present, to enter data both on to a worksheet and into the computer.However, much of the data has only to be entered once and so much less walking about collecting report sheets is required. At the manager level, time is saved, especially in checking results because the computer aids in this respect. We have demon- strated that about 70% of time is saved in the issuing of certificates of analysis. Much time is saved in issuing manage- ment reports, many of which can be designed in advance and generated at the touch of a button. Cost Effectiveness Initially, when the system was installed, we estimated that the laboratory could operate with two less persons, viz., a sample clerk and a certificate clerk. This proved to be true. Later, when the system had been running for a year or two, we were able to show a 15-20% increase in the number of samples analysed per uizizurn by each analyst.Of course, it is not possible to claim that all this saving was due entirely to QC - LIMS. A substantial amount, mainly due to a significant improvement in sample recording and tracking, was certainly attributable to LIMS. One must, however, offset the mainte- nance and running costs against these apparent savings. All in all, an audit of the system resulted in a management decision to expand it significantly. Management Aspects It is perhaps at the management level that the largest impact has been felt. The database has been increased in size to 360 megabytes, giving at least 2-3 years of on-line data, all of which are immediately accessible to a manager without him having to extract them manually from paper records.Trend analyses are easy to obtain, assisting in trouble shooting, in the validation of production processes and analytical methods and in the compilation of data for the assembly of product licence submissions to the DHSS. The costs of analyses can be estimated easily, enabling standard costs to be defined. Current costs can be compared with these and the value of new analytical methods deter- mined. In fact, the uses to which the data are put are limited only by the imagination of the various managers. One may summarise the current impact of a LIMS system by stating that the replacement of a manual data storage system by one based on a computer database simply means that data are at least as secure, much more rapidly available and very much easier to manipulate without the danger of transcription errors. The impact is most apparent at the management level but does impose, in general, more rigid disciplines on all users than does a manual system.I leave you to consider whether this last point is desirable or not. The Future The future impact of a LIMS system will depend on the attitudes of four groups of persons: (i) the suppliers of LIMS systems; (ii) the users of the systems; (iii) the attitude of corporate management to computerisation; and (iv) the attitude of corporate data-processing management. It is becoming increasingly evident that no computer system can stand alone for very long. Indeed, I have heard it said that a microcomputer that is not attached to a network of other computers is like a telephone that is not connected to the national network.Perhaps a stand-alone LIMS system is not as useless as that, but the full power of the system cannot be realised until it can communicate with other systems within, and eventually between, companies. This is where corporate management is important. Without their support, the exten- sion of a basic system will be almost impossible. It is necessary that any LIMS system and other corporate systems shall communicate, demanding many common data structures and communication protocols. Some companies already have this enlightened attitude, which allows LIMS to access the stock control system, enabling sample data to be recorded in advance of delivery to the test laboratory and for material released via LIMS to become immediately available for use.Similarly, the linking of a LIMS system to a production control system will provide many advantages relating to sample scheduling. The incorporation of in-process results in the LIMS database will reduce the need for some end-product testing, thereby enhancing the speed of release with a potential diminution in stock levels. The ability of one company to send certificates of analysis and specifications to another by electronic means would also be of great value, saving both labour and time at both locations. The achievement of such far-reaching possibilities implies that the designers and users of the total systems within and between companies must co-operate. In fact, I suspect that I am talking about a near impossibility at present because it really means a complete redesign of corporate systems taking LIMS into consideration from the time of initiation of design.In the very near future, LIMS and its partner in the computerisation of company data management systems, a PIMS. or production management system, must occupy the detailed attention of the top management of all production orientated companies. LIMS in the Pesticide Residue Laboratory P. J. Snowdon Schering Agrochemicals, Chesterford Park Research Station, Saffron Walden, Essex CB I0 IXL The Residue Analysis Department at Schering Agrochemicals, Chesterford Park. currently handles an annual throughput of around 8000 samples, generating some 25 000 chromatographic analyses (GC and HPLC) of pesticides and known metabolites in various crop and environmental substrates.All data are produced in compliance with Good Laboratory Practice (GLP) regulations and form part of the registration packages (along- side metabolism and toxicology data) submitted to inter- national regulatory bodies such as the United States Environ- mental Protection Agency (USEPA). Since the implementation of a LIMS system in 1987. all chromatographic data handling aspects have been com- puterised and a database has been fully configured for the management of residue study information. System Description The chosen LIMS uses a Beckman CALS Laboratory Manager and PeakPro software running on a Hewlett-Packard HPl000 A series computer with a 500 Mb disc drive and a 6250 bpi tape unit.This system currently supports ten colour graphics terminals (including one PC) in laboratory and office locationsANALYTICAL PROCEEDINGS. MARCH 1989. VOL 26 Study Dictionary 101 Formulation Dictionary with one X-Y plotter and seven system printers (two of which are dedicated to label printing and another which permits letter quality output). Chromatographs are linked to the system via digimetries. These are analogue to digital (A/D) converter units which digitise analogue signals on-line in real time and send them directly to the processor via a 20-mA current loop. Two of these loops have been installed, each supporting 11 instru- ments. The maximum allowable is 15 instruments per loop, beyond which further loops can be added.Configuration Residue analyses are typically grouped according to chemical, crop, territory and year combinations. The LIMS database has. therefore, been built on a ‘.study basis” rather than on individual samples. It is this aspect which most distinguishes the residue analysis configuration and indeed was identified as a fundamental requirement of the system. The configuration is controlled by a series of inter-linked answer files known as dictionaries. These contain fields which define the specifications and procedures necessary to process each study, and within them, each sample. The organisation of the dictionary is represented in Fig. 1. Test protocol Declaration of variables I, 1 Formulation used Active ingredients A.i. concentration n Chemical (IUPAC) names Product code Study type R&D objective No.Startiend dates Study Director Testing protocol Consignment Dictionary Study status Study title Related studies Arrival date Freight information Study numbers 1 Sample Database 1 Sample number Sample history details approved Analysis runsheet No. Date logged Date archived Analyst i d . Date tested Test resu Its Chromatography method ref. Date( s ) va I i d a t e d r Fo rt if i ca t i on I eve I I ~- I I I I Report Dictionary I Definition of report procedures/formats for information retrieval e.g., Analysis runsheets Status reports Results tables Fig. 1. Configuration of dictionaries Operation A residue study is initiated by entering the appropriate fields into a record of the study dictionary. This is achieved by using “full-screen” data entry (arbitrary selection of fields by movement of a cursor over the screen, rather than single, sequential responses to “line-mode” prompts), made possible by the “block-mode’’ facility of the graphics terminals.All of the main functions performed in the system now utilise this feature working from user-designed screens. These screens can be updated or completely re-built by the user as the system develops alongside changing departmental requirements. Once established, the study dictionary record (or study file) essentially holds the protocol for the study and is the source of study status information. Maintenance operations, as with all the dictionaries, are controlled by a non-hierarchical system security profile, again user-configurable.User identification for any operation is preserved via the log-in access password and all events are logged in a file maintained by the system. Revisions to dictionary records are also retained. These are important aspects in relation to GLP compliance. Analyses or “tests” assigned to a study are specified in the study file record. The tests are selected from the entries in the test dictionary and may include simplistic procedures such as recording sample weights or comments, in addition to defining specific GC or HPLC assays. At sample log-in, all relevant field trial information is entered for each sample; common details can be “propagated” through a multiple sample log-in screen. Unique numbers are assigned to each sample and labels are generated automatic- ally.Study specifications and required tests become attached to the samples via the dictionaries. Sample status becomes “logged awaiting testing” and is updated by the system sample by sample as studies proceed. GC and HPLC analyses (testing) are performed in batches. An analyst working on a given study builds a “runsheet” of samples selected from a list of those requiring the particular test for the particular study. The runsheet also includes any calibration standards and recovery efficiency tests needed for the batch. Chromatography Data Handling The PeakPro software package is purpose-built for chromato- graphic data handling. Acquisition (AC) methods define data collection rates and times; digitised chromatograms are stored in raw data (R) files and interpreted by analysis (GC) methods, which define base-line fit, etc., and also store multi-level calibration information using polynomial curve-fit algorithms if required.GC methods can be built using a graphics method development option which, as implied, allows chromatograms to be displayed on-screen and manipulated in the graphics mode by cursor placement. The effects of integration par- ameters can be readily observed and adjusted towards a resilient method which, for a particular assay, will handle a range of data files with various co-extractive backgrounds. The processing of raw data files by a GC method generates the corresponding results (C) files. A snapshot of the GC method at the time of analysis is always retained with the latter (GLP compliance).Batch analysis can be executed through templates, which are stored sets of chromatogram file names containing associated calculation parameters such as sample weight and dilution factor. By building and saving templates corresponding to the runsheet of samples described in the previous section, the appropriate chromatography files are linked with sample i.d. numbers and analysis results are posted into the laboratory manager database. This approach allows a review of data before posting in order to accommodate events such as injection failures. On completion of testing, sample status becomes “tested awaiting validation.” Results can be reviewed batch by batch in the full-screen mode and validated by one or more keystrokes as appropriate. Access is controlled by the system security profile and the validator’s i.d.is preserved alongside the action taken. Rejected samples may be scheduled for re-testing, in which case a valid reason will be prompted for.ANALYTICAL PROCEEDINGS. MARCH lY89. LOL 102 Reporting and Archiving All specification, status and test data can be retrieved and reported at any time either by user-written procedures or on an interactive basis for ud hoc enquiries. Output can be directed either to a screen or to a specified print device. Test results can be tabulated alongside crop treatment details and, when required, can be interpreted further by trend analysis software to produce, for example, residue decline curves. On completion of a given study, all the associated data. including GC - HPLC raw data files, can be transferred on to magnetic tape for archive storage.For audit purposes, all event log entries can also be stored to allow reconstruction of the study. Future Aims LIMS are dynamic systems. As such. they should be encour- aged to develop and grow with changing user requirements and environments. Short-term aims for this residue analysis appli- cation are the implementation of text formatting for full formal reports, the interfacing of laboratory balances for direct sample weight input (event-driven acquisition), the development of two-way communication (and hence enhanced control) with GC - HPLC instrumentation and the continuing development of communications with other computer systems. Justify a LlMS System G. Davison Syntex Pharmaceuticals Ltd., The Ridgeway, Iver, Buckinghamshire SLO 9JW In purchasing capital equipment the following points should be considered.request. 7. Use your staff for their ideas and ensure they support the 1. 3 i.. 3. 4. 5 . 6. Identify what you want, in full detail. This must include cost, servicing, installation, training, delivery. etc. Describe the problem in getting what you want. Identify both the obvious and less obvious decision makers on whether or not the capital request is approved. Know who will support and who will be against your request among your peers and superiors. Lobby management well in advance of your purchases. Be persistent; if you give up easily the first time management raise objections then they will assume the request is not important.8. Lobk for benefits the request, if approved, would bring to your company, e . g . . ( u ) with this equipment our quality costs as a percentage of turnover will stay the same, not go up: ( b ) company must adapt to the future, this equipment is the future: (c) other successful companies use this equipment: and ( d ) get a consultants report, which will inevitably endorse your opinion. 9. Do not state anything in justification that is not true. 10. After purchase, be sure to show item purchased to decision makers while at the same time telling them of the benefits their wise decision has brought to the company. LlMS for the End User A. D. Henderson Smith Kline & French Laboratories Limited, Welwyn Garden City, Hertfordshire AL7 1 EY In October 1984, we installed the Beckman Laboratory Management System in our analytical laboratories.Our prime objective in the quality control (QC) laboratory was to supply information more quickly to the manufacturing and production lines, so avoiding delays. We were also looking for simplified procedural control and to improve our ability to meet the requirements of good manufacturing practices. 1 In August 1987. we completed the addition of computer terminals in the production areas of the Warehouse, Materials Management, Inspection Control and Pellet Blending. The installation of these terminals has brought direct benefit to the “end user” from both inside and outside the laboratory. Examples of the benefits to the “end user’‘ managers and supervisors from the laboratories and to our production areas are presented here.“End User” Benefits Ten examples are given below. 1. Internal and External Certificates of Analysis These can be generated automatically by the laboratory secretary without the need for cross-checking of the results by a technical man age r . 2. List of Sample Types This gives the manager and supervisor direct access to summary lists of samples analysed in the laboratory. 3. Daily (or Weekly) Approvals Once a sample has been “approved” by a laboratory manager. it is automatically accessed by means of a daily listing of approvals. This can be accessed by our QC inspectors and warehouse staff. These lists are then used to update the production stock control systems to a change in product status. 4. Weekly Priority Listings Sample priority assignment by means of automatically gener- ated sample lists has greatly improved our sample management in the QC laboratories.It has replaced the previous manual system in which the laboratory was very dependent on information from the production planning department. 5. Weekly Priority Listings Represented by Index Table/Graph The information from example (4) above can be transferred to a “LOTUS 1,2,3” spreadsheet to produce a weekly index table of priorities and a weekly graph of outstanding samples. This allows the laboratory manager to follow easily the sample trends through his laboratory on a weekly basis.ANALYTICAL PROCEEDINGS. MARCH 1989. VOL 26 103 6. Monthly “Reject” List Exception reports are generated on the first day of each month.A list of ”rejected“ products is a useful reminder to the production manufacturing manager that a serious problem has arisen. 7. Monthly Quality Performance Reports2 In the same way as for example (5) above, the information obtained from the automatically generated monthly reports can be transferred to a LOTUS 1J.3 spreadsheet. This can include information on out batches produced. batches repor- ted, re-works, rejects, analytical retests and time costings, etc. The time taken to generate the data is minimal and this leaves more time for monthly performance reviews by senior managers. 8. Analytical Results Trend Cards Access to terminals in the production areas allows the production managers to obtain trend-card information on analytical results directly from the laboratory database.The addition of production information, such as our percentage coating to a sustained release product, can make the interpretation of trend data easier. 9. Monthly Costing Reports The automatic generation of specific product costing reports makes it easier to charge the laboratory customer areas. 10. Yearly Laboratory Samples and Costings End of year laboratory management reports are facilitated by the automatic generation of a number of sample types and their hourly costings. Future Plans A second computer is to be installed in 1988 in order to improve the information communications between our development laboratories. The extra computing power will allow us to add our inspection control and commercial stability functions on to the LIMS.This will increase the number of “end users” on the system. The system will be linked directly to future production- based computers in order to automate further our informa- tion transfers. Conclusions The addition of computer terminals within our production areas has increased the number of “end users“ on the system. This has reduced the number of disruptive phone calls to the laboratory as outside users now perform their own searches of the sample database and determine the status of samples currently under test. Paperwork and filing systems in these areas have been replaced by the computer terminal. References 1. Henderson. A. D.. Anal. Proc. 1988. 25. 147. 2. Chaeffer. R.. and Stoker. J . R.. Pharm. Technol.. June 1986, p. 54. Hewlett-Packard‘s LABSAM in an Integrated System 1.J. Smith Development Computing, Glaxo Group Research, Ware, Hertfordshire SG 12 ODJ Within Glaxo Group Research (GGR) computers play an important role in assisting the identification and development of new pharmaceutical products. I am a senior analyst programmer in the Computer Science Division of GGR and have been involved in the specification of requirements for the Pharmacy Division. This has included an assessment of Hewlett-Packard’s (HP) LABSAM as a laboratory informa- tion management system (LIMS). The analytical laboratories handle various classes of sam- ples. including those for chemical development, toxicology and clinical trials. The single major class of sample is stability. which accounts for approximately 50% of the total. Most analysts in Glaxo currently rely on paper-based systems for the recording and reporting of data.This paper summarises the development of computer systems to suit the various require- ments of GGR staff, including the collation and management of information at the laboratory level with particular reference to LABSAM. It is intended that the computerisation of the analytical laboratories will increase accuracy, productivity and com- pliance with Good Laboratory Practice (GLP) and assist in the planning of tasks. With a computerised laboratory, many benefits will be provided by other systems to which it is linked. Information Requirements Different levels within any organisation require different kinds of information. High up the organisation a manager needs to be informed at a summary level of all the organisation’s activities.The first question a systems analyst usually asks is “To what use will the information be put?“ Within any organisation there will be several answers, because people’s information require- ments change according to their level and role within the company. At the top level, information tends to be ill- structured, ad hoc, informal, uncertain and concerned with the future. At the middle levels. data tend to be structured, formal, regular and concerned with the near future. At the lower levels. information is repetitive, specific and programmable with immediate and short-term time scales. A total solution addresses all these requirements. For stability studies, the information requirements can be split into four levels: (1) Pharmacy Project Management; (2) Stability Project Databases; (3) Laboratory Information Management; and (4) Data Acquisition and Control. The LABSAM system which we are currently defining for the analytical division will form part of the system that will address these requirements and will have the links to other sub-systems that are detailed in Table 1.Systems Approach The data processing approach to providing an over-all solution is to consider the organisation as a complex system of interdependent elements which are interacting with each other and their environment. A system consists of ”a whole composed of parts in an orderly arrangement according to a scheme or plan .” Usually the whole system is too large or too complex for an application team to handle at any one time.Therefore, it is necessary to104 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 Table 1. Links in the integrated system Sub-system Reason for connection Stability system Control and manufacturing Product specifications Methods CPAC - LAS Automatic scheduling of test (Login) Return of summary results Automatic scheduling of tests Return of summary results Transfer of specification test limits Transfer of calculation parameters and Sequence generation for CPAC Passing of sample amount data Return of chromatography results Automatic data capture from textual help screens Instrument interface instruments divide the total system into sub-systems. which in turn may be divided into an integrated set of sub-systems. In practice, systems that have close relationships are grouped together.This will usually be carried out according to some logical or functional criteria, but the availability of computer systems and packages influences the grouping of sub-systems. For example. LABSAM spans the LIMS level and the data acquisition level and in some circumstances it is appropriate to view these two levels as one sub-system. In order to help develop systems, and in particular integrated systems, a number of advantages are gained by employing a structured systems design methodology during the entire life cycle of the system. The system life cycle is outlined below: 1. Project initiation. 2. Analysis. 3. Design. 4. Construction. 5. Testing (unit, systems and acceptance). 6. Implementation. 7.Maintenance and enhancement. In addition to assisting with the integration of systems, the major advantages of a structured methodology are: (1) a framework for development is defined; (2) review procedures are defined; (3) the development of flexible systems is encouraged; (4) a check list for management is provided; and ( 5 ) planning is improved. . Functions Required of a Laboratory System Our strategy was to look for a commercial system which would provide a large percentage of the whole stability system as this would reduce the number of communication paths between systems. It soon became apparent that no commercial system addressed our requirements so we began to look for systems that could be put together to build the total system. The evaluation process took many months, during which time the user requirements, hardware and software options kept changing.Sub-systems had to be found that would adapt well to changes, and flexibility became a keyword. As with all systems used by the Pharmacy Division, a laboratory system should conform to GLP. The major implica- tion of this is that data should be audited. Over 100 analysts handle about 20000 stability samples a year. A significant amount of time is spent keeping track of all these samples. collecting data, reporting results and preparing submissions to regulatory bodies according to GLP. One example of unnecessary effort imposed by a paper- based system is the transcription of the results of chemical tests from the analyst’s notebook into a form which can be sent to the stability section.Here it is transcribed on to the stability database and a computerised report produced on paper which is sent back to the analyst to check against the notebook. Corrections are made to the report, which is returned to the stability section so they can update the computer. Reporting of data in a non-computerised environment is lengthy but flexible. The secretary who constructs formal reports will always be indispensable, but computer systems are extremely good at generating reports of a routine nature and can help the analyst and secretary to produce the more complex reports which are not needed on a regular basis. A LIMS system should provide this facility in the form of hard copy reports and electronic ”reporting” to other computer systems.In 1986 HP’s LABSAM was selected as the best available LIMS and data acquisition system for our requirements. Additionally, the use of HP’s Laboratory Automation Soft- ware (LAS) on HP 1000 machines and the development of a statistical calculations package (CPAC) by a third party for use in conjunction with LAS had some bearing on our choice. LABSAM’s Functionality No LABSAM systems are currently being used by analysts within Glaxo. Three pilot studies were carried out to assess the product and my experience gained on the systems produced during these studies formed the basis of my knowledge of the product. LABSAM provides the functionality that would be expected from a laboratory system. The five major functions are: (1) sample login; (2) result entry; (3) validation; (4) reporting; and ( 5 ) full audit trail.In addition to this list, LABSAM has a data capture module called the On-line Handler. We have found a number of shortcomings with this module which have led to the initiation of the development of a data capture system that will interface to the LABSAM system. LABSAM could be released to the analytical laboratories with the minimum of customisation. but our strategy is to provide a system that accomplishes most, or all, of the requirements of an integrated system because of the benefits that this will provide. LABSAM has a two level key system which is termed: KEY 1-BATCH level KEY 2-SAMPLE level This key system is shown in Table 2. Table 2. Example of a two level key system Level 1 Batch level key Level 2 Sample level key Master data e.g..Product details Master data e.g.. Assigned analyst Test data e.g.. Assay. pH These keys can be used to allow subsets of samples to be collated within a batch. For example, the BATCH level could hold the stability programme details, the time of storage. etc., and the SAMPLE level would consist of the conditions of storage within which analytical tests are scheduled. If required a single level key can be used on the same system. For example, the testing of clinical trials samples is performed under a single batch number with no sub-sets of samples. These batches can co-exist with the two level key used for stability samples. All test data are held by LABSAM within Identification Codes (IDCs) which form the basis of the definition of the data.IDCs are defined before they can be used to hold data. Their definition is flexible and allows a number of functions to be performed. These include the validation of data input in terms of the format of the data and a check against specification limits. One of the features of LABSAM IDCs is that. as a result is being entered into an IDC. an evaluation routine (a FORTRAN program) can be run automatically to perform validation of the entered data, calculate data into other IDCs or. in fact, to perform any function which the operating system permits. LABSAM IDCs have what is called a preliminary value and aANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 105 final result. A preliminary value is defined as the raw data and is the value first recorded. A final result may be the same as the preliminary value, e.g., pH.or may be a mean of a number of preliminary values, e.g.. assay, the difference between prelimi- nary values, e.g., mass by difference, or any other calculation specified with the definition of the IDC. Various types of IDCs exist, including master data IDCs. These can be used to hold information about the batch or sample. LABSAM has an Auxiliary File System (AFS), which can be used to hold data centrally in either system-defined files or files defined specifically for the particular LABSAM system. For example, there is a system file which is used to hold specification test result limits. This file can be referenced within the IDC definition so as to check results being entered into the system. Holding the data centrally in this manner helps with the maintenance of the data.As an example of how the AFS can be applied to a customised system, a file was used during the pilot studies to hold product details against the stability programme reference number. When a stability batch was logged into the system the product details in the AFS file were referenced so as to write the data contained there into the master data IDCs at the batch level. Sample login can prove to be a laborious task in its simplest form. Where the same sets of test IDCs are used regularly the system can provide assistance. The validation procedure provided by LABSAM allows up to five levels of authorisation. Batches and analysts can be given various levels of authorisation for the validation of test results. This provides the means to set particular batches, e.g., stability or clinical trials samples.to require authorisation by specific levels of personnel. When data are entered into an IDC, the date, time and identity of the analyst are automatic- ally assigned to the data. In the light of the regulatory authority's interpretation of GLP, LABSAM's best asset is its audit trail which prevents overwritten or deleted data from being lost. The editing of data in a paper-based system allows results and derived results to be crossed out but left legible. LABSAM mimics this process by ensuring that all changes to data held within IDCs are subject to the audit trail function. When data are altered, a reason for the change must be supplied by the analyst.Additionally, the data, time and user's identity are automatically linked to the new result. Audit trails are not easy to provide on computer systems. I have been responsible for the development of a similar, but more basic, audit trail facility on a relational database and I am impressed by the way in which LABSAM can store and report this information. It should be noted that the AFS does not have the audit trail facility and. therefore, the data should be secured by restricting access to the files to specific personnel. Modules are assigned to individuals, thus providing a mechan- ism for the security of data. Each user has specific modules which he or she can use. LABQUEST is an integral part of LABSAM and allows ad hoc searching of the main database. This is a powerful module which can be used to generate reports of the data in a customised format.Command files can be generated to assist users in the selection of data. These can be copied and modified to suit specific search requirements. Integration of LABSAM into the Over-all System Many of the manual entries into LABSAM can be overcome by interfacing the LABSAM system with other systems. One of the links which we intend to provide is a link to the stability system running on VAX machines. The VAX system will hold the protocol lists for the testing of stability samples. The current set of these protocols will be passed to the LABSAM system at regular intervals and will be logged in automatically by a FORTRAN program written specifically for this purpose. A similar process will occur after all the test results for a batch have been finally validated and will return summary data to the VAX system for inclusion in reports. Another example of the customisation of LABSAM to fit into an integrated system is a function which writes the product details from the Control and Manufacturing database into the AFS. The transfer of files between VAX and HP 1000 systems will be provided by NS - VAX (a HP product) running on a DEC ethernet system. The instrument interface will be designed such that it will appear to be a part of the LABSAM system. This is made possible by the access tools provided with the LABSAM product. The data capture process will allow analysts to perform tests from which the results generated will be displayed on a worklist on a terminal screen adjacent to the instrument. As results are accepted by the analyst, derived data will be displayed on the screen. The LABSAM audit facility will function within the instrument interface, thus demonstrat- ing the dependency of one system on another. Conclusion Today technology provides endless packages which are valu- able in their own right, but the full benefit of all these packages will only be realised when they are integrated together. Applications should be flexible and allow expansion of the options available to scientists as new technologies emerge. LABSAM suits the requirements of an analytical laboratory system as part of an integrated system within Glaxo. Links to other systems can be built, thus providing data for higher level databases.

ISSN:0144-557X    

DOI:10.1039/AP9892600099

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

106 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 SAC 89 July 30-August 5 , 1989, Cambridge The programme for the SAC 89 international conference on analytical chemistry, to be held in the University of Cam- bridge, has now largely been arranged and is summarised below. The various scientific contributions will be presented in lecture and poster sessions. In order to give due weight to poster presentations, these presentations will be given in after-lunch sessions at which time no lecture sessions will be held. There will be the traditional workshops and, on Wednesday, update courses will be held on a variety of subjects for which separate registration will be required. A comprehensive programme of tours, both cultural and scientific, and a variety of social events have been arranged.The workshops will be held on Tuesday and Thursday, while poster sessions will be held on Monday, Tuesday, Thursday and Friday. Monday, Tuesday, Thursday and Friday will also be devoted to lectures, which will include plenary and invited lectures by international authorities. DAILY TIMETABLE OF SCIENTIFIC PROGRAMME SUMMARY Monday, July 31, 1989 Plenary lecture: “Flow Injection and Chromatography. Twins or Siblings?” J. RfiiiEka (University of Washington, Seattle, USA). Other lecture themes: Electroanalytical Chemistry; Food; Flow Analysis; General Analytical Chemistry (particularly polymer analysis). Poster themes: Food; Electroanalytical Chemistry; Flow Analysis. Tuesday, August 1, 1989 Plenary lecture: “Practical Applications of an Understanding of Chiral Recognition Requirements,” W.H. Pirkle (University of Illinois at Urbana-Champaign, USA). Other lecture themes: Chromatography; Sensors; Spectro- scopy; General Analytical Chemistry; Automatic Methods. Poster themes: Chromatography; Sensors; General Analytical Chemistry. Workshops: 1. “Low Cost Flow Injection Analysis Equip- ment,” J. F. Tyson (Loughborough University of Technology). 2,3. “Sensors,” A. G. Fogg (Loughborough University of Technology) and B. J. Birch (Unilever Research, Sharnbrook, Bedford). 4. “LIMS/Data Handling,” S. P. Maj (Norwich City College of Further and Higher Education). 5 . “Immunoaffinity Columns,” A. A. Crimes (Unilever Research, Sharnbrook, Bedford). Scientific visit: Philips Scientific (Spectroscopy). Wednesday, August 2 , 1989 Updates: All-day courses (requiring separate registration) on: 1, “Chiral Separation,” D.R. Taylor (University of Manches- ter Institute of Science and Technology); 2, “Chemilumines- cence and Bioluminescence,” P. J. Worsfold (University of Hull); 3, “Near Infrared Spectroscopy,” A. M. C. Davies (Oxford Analytical Instruments Ltd.); 4, “Laser Based Ana- lytical Mass Spectrometry,” R. J. Donovan (University of Edinburgh); 5 , “Information Technologies for Analytical Chemists,” C. Teague (Royal Society of Chemistry, Cam- bridge). Thursday, August 3 , 1989 Plenary lecture: “Evolution in Chemometrics,” G. Kateman (Katholieke Universiteit, Nijmegen, The Netherlands). Other lecture themes: Atomic Spectroscopy; Mass Spec- trometry; Chemometrics; Chromatography; High Energy Techniques. Poster themes: Atomic Spectroscopy; General Analytical Chemistry; Chemometrics. Workshops: As for Tuesday.Scientific visit: Philips Scientific (Chromatography). Friday, August 4, 1989 Plenary lecture: “Light and Life-Some Recent Applications of Chemiluminescence and Enzymes in Analytical Chemistry ,” A. Townshend (University of Hull). Other lecture themes: Atomic Spectroscopy; Molecular Spec- troscopy; Micro and Chemical Methods; Environmental Analysis. Poster themes: Micro and Chemical Methods; Molecular Spectroscopy; Atomic Spectroscopy; Environmental Analysis. LECTURES Monday Food-Is It Legal, Is It Safe? Invited lecture. R. L. S. Patterson, Institute of Food Research, Bristol; “Verification of species origin of meats.” “Identification of fish species,” I.Mackie (Torrey Research Station, Aberdeen). “Authentication of apple juices and whisky by pyrolysis - mass spectrometry,” C. S. Gutteridge (The Lord Zuckerman Research Centre, Reading). “Analysis of synthetic colours in foods-where are we now?” J. P. Chaytor (Peter Chaytor and Associates, Milton Keynes). “Toxic Honey-The New Zealand Story,” J. Love (DSIR, Christchurch, New Zealand). “Are chromatographic methods suitable for the determina- tion of aflatoxins in peanut butter?” M. P. K. Dell and S. J. Haswell (Thames Polytechnic, Woolwich, London). “The use of immunoaffinity columns in aflatoxin analysis with special reference to milk products,” A. A. Crimes, J. M. Miller and G. M. Walden (Unilever Research, Colworth Laboratory, Bedford). “Assessment of the Aflatest Mycotoxin testing system for monitoring of raw materials and feeds,” S.E. Bryan (BOCM Silcock, Selby, Yorkshire). Monday Electroanalytical Chemistry “Application of glassy carbon and modified glassy carbon in analytical chemistry,” B. Vucurovic and M. Lausevic (Univer- sity of Belgrade, Faculty of Technology and Metallurgy), Z. Lausevic (The Institute for Nuclear Science Boris Kidric, Belgrade) and M. Rajkovic (University of Belgrade Faculty of Agriculture, Zemun, Czechoslovakia). “Determination of aluminium in haemodialysis concentrates by adsorption voltammetry-comparison with atomic absorp- tion spectrometry.” B. Gammelgaard (Royal Danish School of Pharmacy, Copenhagen, Denmark). “Adsorptive stripping voltammetry of some biologically important molecules,” Josino C.Moreira and Arnold G. Fogg (Loughborough University of Technology). “Radiotracer studies on the functioning of neutral carrier type ion selective electrodes,” Natalie K. Harris, G. J. Moody and J. D. R. Thomas (University of Wales College of Cardiff). “Voltammetry in frozen electrolytes,” T. E. Edmonds and S. K. N. Bath (Loughborough University of Technology).ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 107 Monday Tuesday Electroanalytical Chemistry - Midlands Region Symposium Invited lecture. S. Brukenstein, SUNY at Buffalo, NY; “In situ applications of the quartz crystal microbalance. ” “Amplified mass immunosorbent assay with a piezoelectric quartz crystal microbalance ,” Michael D . Ward and Richard C. Ebersole (E. I. du Pont de Nemours and Co., Wilmington, Delaware, USA).“Theory and application of acoustic wave sensors for liquid media,” Michael Thompson (University of Toronto, Canada), Ljubinka Rajkovic and Biljana Cavic (University of Belgrade, Yugoslavia). Monday Flow Analysis “Modified simplex approach in the optimisation of enzyme electrodes for flow injection analysis,” S. K. Beh, G. J. Moody and J. D. R. Thomas (University of Wales College of Cardiff). “Effect of coated open-tubular inorganic based solid-state ion selective electrodes on dispersion in flow injection analy- sis,” Jacobus F. Van Staden (University of Pretoria, RSA). “Applications of the single well stirred tank model ’for dispersion in flow injection analysis,” J. F. Tyson (University of Technology, Loughborough).“Membrane separation in continuous flow and flow injection systems with dynamic dialysis” Jacobus F. Van Staden and Ancel Van Rensburg (University of Pretoria, RSA). “Continuous flow chemiluminescent determination of some corticosteroids,” A.C. Calokerinos and I. I. Koukli (Univer- sity of Athens, Greece). “Flow injection determination of trace cationic and anionic impurities in fine chemicals,” A. B. Marsden and J. F. Tyson (University of Technology, Loughborough). “A sensitive spectrofluorimetric method for aluminium determination and its automation by flow injection analysis (FIA),” P. Fernandez, C. Perez Conde, A. M. Gutierrez and C. Camara (Universidad Complutense, Madrid, Spain). “Shapes of normal and reverse flow injection systems online formation of iodine,” Arnold G.Fogg, Xiangwen Wang and Julian F. Tyson (University of Technology, Loughborough). Monday General Analytical Chemistry “The analysis of polyether sulphone,” I. G. Hinton (Ciba Giegy Plastics, Duxford). “Characterisation of the ester cross linkage between cotton cellulose and polycarboxylic acids in cotton fabrics using FTIR - photoacoustic spectroscopy,” Charles Q . Yang (Marshall University, Huntingdon, WV, USA). “Applications of FTIR - photoacoustic spectroscopy to the near-surface analysis of polymeric materials ,” Charles Q. Yang (Marshall University, Huntingdon, WV, USA). “Determination of non-removable contamination on some stainless steels,” A. Belfiore, G. Panciatici and M. Poggianti (CRESAM, Pisa, Italy). “An investigation of chemiluminescence reaction in Luminol - iodine - arsenic(II1) system,” Li Shuling and He Yinglu (Academy of Geological Science, Beijing, P.R. China). “Application of thermogravimetric analyser (TGA) to the determination of diffusion coefficient and water content ,” Toshio Ogawa (Kanazawa Institute of Technology , Japan). “Molecular size distribution of peptides by gel-permeation chromatography in milk products,” Danielle Baylocq (Centre D’Etudes Pharmaceutique, Chatenay-Malbry, France). Chromatography Invited lecture. V. Schurig, University of Tubingen; “Separa- tion of isotopic and enantiomeric compositions by complexa- tion gas chromatography. ” “Gas chromatographic separation of hydrocarbons on chitin and chitosan as stationary phases,” Jama Tuddin Mohd Daud and Harry Agusnar (Universiti Kebangsaan, Malaysia).“Pyrolysis gas chromatography of separated zones on thin layer chromatograms,” S. J. Lyle (King Fahd University of Petroleum and Minerals, Dhahran, Saudi Arabia). “Gas chromatographic determination of dibutyltin and dioctyltin dichlorides as hydride derivatives,” Sinikka Vainio- talo and Leila Hayri (Institute of Occupational Health, Helsinki, Finland). “Selectivity and column comparisons in supercritical fluid chromatography,” Roger M. Smith, M. Marsin Sanagi, Vince B. Evans and Simon Cocks (Loughborough University of Technology). “The use of soft gels in size exclusion liquid chromatography with instrumentation for HPLC,” J. Cacho and E. Castells (University of Zaragoza, Spain). “The use of a chelating resin containing the N-(hydroxy- methy1)thioamide in ion chromatographic analysis,” Chuen- Ying Liu, Huan-Tsung Chang and Tan-Jui Chai (National Taiwan University, Taiwan).“Improved reproducibility for the separation of basic drugs on silica columns,” Roger M. Smith and James P. Westlake (Loughborough University of Technology), Richard Gill and M. David Osselton (Home Office Forensic Science Service, Aldermaston, Berkshire). “Prediction of retention time in liquid chromatography, ” Sheila Sharp, Jean W. Baty and J . D. Baty (Ninewells Hospital, Dundee). “Studies on optimum method of solvent systems in high- performance liquid chromatography. Part 2. Prediction of retention time in any kind of multi-step binary linear gradient elution,” Qingcai Jiao and Yaozu Chen (Lanzhou University), Zhixian Shi (Academia Sinica Xining, P.R. China). Tuesday Sensors Invited lecture. J. N. Miller, Loughborough University of Technology; “Immunosensors; Problems and Prospects.” “Development of amperometric flow injection monitors and disposable sensor devices for the determination of nitrate ,” Arnold G. Fogg, S . Paul Scullion and Tony E. Edmonds (Loughborough University of Technology). “Poly(viny1 chloride) and liquid membrane electrodes for selective determination of cocaine and heroin,” Saad S. M. Hassan and M. A. Hamada (Qatar University). “Evaluation of a new sodium selective electrode ,” Martin Telting, Malcolm R. Smyth and Dermot Diamond (NIHE, Dublin), Eileen Seward, Gyula Svehla and Anthony M. McKervey (University College, Cork). “Development of an optical fibre aluminium sensor in a flowing system,” E.Blanco Gonzalez, R. Pereiro Garcia, M. E. Diaz Garcia, A. Sanz-Medel (University of Oviedo, Spain), and R. Narayanaswamy (UMIST, Manchester). “Electrochemical sensors based upon capillary fill systems,” B. J. Birch and I. W. Burns (Unilever Research, Colworth Laboratory, Bedford). “Sensors based on polymer modified electrodes ,” Malcolm R. Smyth, Dona1 Leech, Mary Meaney and Johannes G. Vos (NIHE, Dublin), Pilar Dominguez, Jose-Maria Fernandez Alvarez and Tun0 Blanco (University of Oviedo, Spain). “The preparation of polypyrrole layers for NO, gas sensors,” Jonathan M. Slater and Esther Watt (Birkbeck College, London). “A sensor for trace levels of phenols in water,” E. S.108 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 Bridgeland, V.H. P. Colclough, R. A. Jewsbury and N. D. Martin (The Polytechnic, Huddersfield). “Immobilisation of components of antigen - antibody reaction on the surface of semiconductor structure and characteristic of the product ,” Vladimir Zaitsev, Larisa Kolo- mietz and Victor Scopenco (Kiev State University, USSR). Tuesday General Analytical Chemistry “Fourier transform Raman spectroscopy in industrial research,” Stephen P. Church, Peter J. Stephenson and Pat J. Hendra (Courtaulds Research, Coventry, and The University, Southampton). “Surface enhanced Raman spectroscopy: toward the ulti- mate tool for trace organic analysis,” T. Vo-Dinh (Oak Ridge National Laboratory, Tennessee, USA). “Accelerator mass spectroscopy of fully stripped W l ions at the Munich Tandem Accelerator,” J.Heinzl (Technische Universitat, Miinchen, FRG). Continuous flow molecular emission cavity analysis of cephalosporins,” A. C. Calokerinos and N. Grekas (University of Athens, Greece). Tuesday General Analytical Chemistry “Synergistic extraction for the separation of palladium from platinum,” Geum-hee Lee and Koo-soon Chung (Sogang University, Seoul, Korea). “Applications of a novel programmable thermal vapourising injector to the analysis of food constituents and contaminants,” 1. S. Gilkison (Philips Scientific, Cambridge). “Optimisation of liquid scintillation technique to low level measurements (14C,3H, 90Sr),” G. Rauret, J. S. Mestres, J. F. Garcia, M. M. Ribera and P. Rajadel (University of Barce- lona, Spain). “A study on the rate of degradation of a tropical crude oil by marine bacteria,” M.D. Pauzi Abdullah and Nor M. Mahadi (University of Kebangsaan, Malaysia). “Determination of bismuth by hydride generation atomic absorption spectrometry coupled with flow injection analysis and a membrane phase separator,” P. K. Hon and W. F. Chan (The Chinese University of Hong Kong). Tuesday Automatic Methods Invited lecture. D. Betteridge, BP Research, Sunbury-on- Thames, Middlesex; “Dispersed automated analysis-the major challenge for analysts.” ‘‘QuANTuM-a combined LIMS and spectral database,” N. Cook and D . McLauchlin (Kodak, Harrow). “Distributed System Modelling-implications and applica- tions to laboratory automation,” S. P. Maj (Norwich City College of Further and Higher Education).“QUARTS: quality assurance real time system,” P. J. Stevens (Glaxochem, Montrose, Angus). “Automated sample preparation using the BP Cartesian robotics system,” M. Crook and C. Davies (B.P. Research Centre, Sunbury-on-Thames). “Integrated Intelligent Instruments (13) in materials and environmental sciences,” S. A. Liebman, A. P. Snyder, M. B. Wasserman, M. E. Brooks, E. J. Levy, J. Watkins, S. Lurcott and S. O’Neill (Aberdeen Proving Ground, MD, USA). Thursday Chemometrics Invited lecture. M. Thompson, Birkbeck College, London ; “Robust statistics for analysts. ” “Standardless quantitative X-ray phase analysis-estimation of precision,” L. S. Zevin (Ben Gurion University of the Negev, Israel). “High-precision, high-accuracy analysis at major levels by atomic absorption spectrometry,” G.Tyler, B. Field and G. Hibberd (Varian Associates Ltd., Walton-on-Thames, Sur- “Selecting sampling techniques for mycotoxin contaminated food,” S. J. Haswell and P. Dell (Thames Polytechnic, London). “Chemometrics in clinical chemistry ,” J. Thompson (Birm- ingham University). “Clustering and classification: a training set of infrared spectra,” M. J. Adams and D . A. E. Rendell (Wolverhampton Polytechnic). “Expert system for classification and identification of toxic air pollutants from mass spectra,” Donald R. Scott (USEPA, Research Triangle Park, NC, USA). “Application of chemometrics to industrial spectroscopy problems,” P. J. Tayler and R. A. Hearmon (ICI Wilton, Middlesbrough). “Simultaneous determination of six amino acids by direct ultraviolet spectrophotometry combined with the Kalman filter,” Xinan Liu and Ying Gao (No.502, Institute of Chemical Defense, P.O. Box 1044, Beijing 102205, PRC), Leming Shi and Shengzhe Nie (Star Institute of Applied Chemistry, Hezuohua Road, Hefei, Anhui, PRC), Zhihong Xu (Institute of Chemical Metallurgy, Academia Sinica, Beijing 100080, PRC). rey). Paper by R. L. Tranter (Glaxo, Barnard Castle). Thursday Atomic Spectroscopy “Atomisation studies in electrothermal AAS using radioactive tracers,” M. Mansha Chaudhry and David Littlejohn (Univer- sity of Strathclyde) and John E. Whitley (Scottish Universities Research and Reactor Centre, East Kilbride). “Recent developments in atomiser , source inductively coupled plasmas in atomic fluorescence spectrometry (ASIA),” S.Greenfield, T. M. Durrani, S. Kaya and J. F. Tyson (Loughborough University of Technology). “Investigation of interference effects in furnace atomic non-thermal excitation spectrometry (FANES) ,” Sean Lynch, David Bolland and David Littlejohn (University of Strathclyde, Glasgow). Invited lecture. J. Marshall, ICI Warrington; “Atomic spectrometry towards the millenium.” “Quantitative elemental analysis by interfaced chromato- graphy and atomic emission spectrometry,’’ Peter C. Uden (University of Massachusetts, Amherst). “Speciation of vanadium present in a model yeast system,” Bharti Patel, Stephen J. Haswell and Roman Grzeskowiak (Thames Polytechnic, London). “Determination of trace elements in trimethylgallium by electrothermal atomic absorption spectrometrty and induc- tively coupled plasma atomic emission spectrometry,” Kikuo Takeda and Masao Minobe (Sumimoto Chemical Ltd., Ehime, Japan).“Flow injection determination of trace elements in organic matrices in the anaerobic-sealant industry with direct current plasma atomic emission spectrometry,” M. C. Brennan [Locite (Irl.) Dublin] and G. Svehla (University College, Cork). “Decomposition of cinnabar and organomercurials in geol- ogical materials with nitric acid - sulphuric acid mixture for the determination of total mercury by cold vapour atomic absorp- tion spectrometry,” Arnold Kuldvere (Geological Survey of Norway, Trondheim, Norway). Thursday General Analytical Chemistry “Quantitation of amino acids in biological samples by liquid chromatography and various sources of error causing discre- pancies in the results,” G.Ali Qureshi and A. RasheedANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 109 Qureshi (Karolinska Institute, Huddinge University Hospital, Stockholm, Sweden). “Chromatographic behaviour and analytical applications of synthetic and biologically derived metal sequestering reagents,” J. D. Glennon, C. Ryan, S. Srijaranai, A. T. Senior and N. Mitchell (University College, Cork). “Chiroptical and multi-channel detection methods for opti- misation in chiral HPLC,” Anthony F. Fell, Graham Ley, Brian Clark and Barry Kaye (University of Bradford and Pfizer Central Research, Sandwich, Kent). “Gas chromatographic be haviour of anilines on liquid crystal and polyester stationary phases,” Albertine E. Habboush, Sabri M.Farroha and Nabeel S. Othman (University of Baghdad, Iraq). “Neutron activation analysis of gold in geological materials,” N. R. Das, T. K. Baidya, P. S. Chakrabortry and S. N. Bhattacharyya (Saha Institute of Nuclear Physics, Calcutta, and Jadavpur University, Calcutta, India). “Synthetic definitive multi-element standard and its applica- tion to radioactivation analysis of biological materials,” Nobuo Suzuki, Yoshihiro Iwata and Hisanori Imura (Tohoku Univer- sity, Sendai, Japan). “Quantitative determination of low energy beta-emitter radionuclides deposited on surfaces by attapulgite treatment ,” A. Belfiore, A. Lo Moro, G. Pantiatici and G. Raspi (CRESAM, Pisa, and Universita di Pisa, Italy). “Fission products determination in high level waste solution by WDXRF.Spectral interference correction by intensity ratio,” Ivone Mulako Sat0 (IPEN/CNEN/SP, Sao Paulo, Brazil) . “A non-destructive method for the determination of impuri- ties in nuclear grade aluminium oxide pellets by X-ray fluorescence spectrometry,” Vera L. R. Salvador, Wilson S. Scapin Jr. and Ivone M. Sat0 (IPEN/CNEW/SP, Sao Paulo, Brazil). Thursday Combined Techniques in Molecular Spectroscopy. 1. Invited lecture. D. E. Games, University College of Swansea; “Recent developments of SFC - MS systems and their applications. ” “Supercritical fluid extraction - supercritical fluid chromato- graphy - mass spectrometry and SFE/SFC/IR of organic compounds in fibre finishes,” P. J. Stephenson and A. Mackenzie (Courtaulds Research, Coventry). “A dedicated bench top mass spectrometer with improved LC - MS performance and versatility,” W.H. McFadden and J. K. Wellig (Finnegan MAT, Heme1 Hempstead). “Applications of a novel geometry tandem mass spec- trometer in the pharmaceutical industry,” s. B. Wilson (V.G. Tritech, Wythenshawe, Manchester). Invited lecture. C. J. W. Brooks, University of Glasgow; “Some functional group derivatives useful in GC - MS”. “A novel derivatisation and determination of acylcarnitines by GC - MS,” S. Lowes and M. E. Rose (Open University, Milton Keynes, Buckinghamshire). “Gas chromatography - mass spectrometry applications using an ion trap mass spectrometer,” C. S. Creaser, D. Mitchell and K. O’Neill (University of East Anglia, Norwich, Norfolk). “The use of a mass selective detector to study fatty acid profiles in cancer cells grown in culture,” S.Pazouki, J. D. Baty (Ninewells Hospital, Dundee) and H. Wallace and C. Coleman (Aberdeen Royal Infirmary). Friday Environmental “A spectrophotometric field monitor for water quality parameters,” Paul J. Worsfold and Richard C. Benson (University of Hull) and Frank W. Sweeting (Wessex Water, Bristol). “The speciation of heavy metals in sediment fractions from Cadiz Bay,” I. Antequera and M. Garcia Vargas (University of Cadiz, Spain). “Re-examination of archived specimens from the Great Lakes for specific congeners of PCBs,” R. Turle, R. J. Norstrom and H. T. Won (Environment Canada, Ottawa, Canada). “Aspects of chemical marine monitoring and the impact of organotins in Strangford Lough, Northern Ireland,” C.A. Donaghy, M. Harriott and D. Thorburn Burns (The Queen’s University of Belfast). “Formic acid-a biolgical indicator of formaldehyde expo- sure,” Pirkko Pfaffli (Institute of Occupational Health, Hel- sinki). “Analysis of Antarctic snow and ice,” E. W. Wolff, R. Mulvaney, D. A . Peel and A. P. Reid (British Antarctic Survey, Cambridge). “Determination of arsenic, manganese and iron in fly ash and their use as tracers of air pollution,” C. Nerin, R. Zufiaurre and J. Cacho (University of Zaragosa, Spain). “Speciation of butyltin ions by high-performance liquid chromatography with various spectroscopic detectors,” J . I. Garcia Alonso and A. Sanz-Medel (University of Oviedo, Spain) and L. Ebdon (Plymouth Polytechnic). “Environmental monitoring of the LLW storage site on a Pacific Ocean islet off Taiwan,” C.M. Tsai (Atomic Energy Council, Taipei, Taiwan), C. Chung (National Tsing Hua University, Taiwan). Friday Micro and Chemical Methods Invited lecture. D. W. Wilson, Woodford Green, Essex; “Analytical Evolution. ” “Analytical applications of total reflection X-ray fluores- cence spectroscopy,” S. J. Haswell and S. Mukhtar (Thames Polytechnic, London). “VESICLES: New ordered medium for developing fluores- cence and phosphorescence at room temperature,” M. E. Diaz Garcia, M. R. Fernandez de la Campa and A. Sanz-Medel (University of Oviedo, Spain). “The acidimetric titration of tungstate complexed by poly- 01s: principle and practice,” J. F. Verchere, J. P. Sauvage and G. R. Rapaumbya (Laboratoire de Chemie Macromoleculaire, Mont Saint Aigan, France).“Analysis of the ceramic super conductor YBa2Cu307,” M. A. Malati (Mid-Kent College of Higher and Further Educa- tion, Chatham, Kent). “A new method for organic hydroxyl group determination,” Teresa Gajewska (Industrial Chemistry Research Institute, Warsaw, Poland). “Peculiarities of using non-aqueous media in spectropho- tometry,” K. D. Arakchaa (USSR Academy of Sciences, Kyzyl, USSR), S. B. Savvin, T. V. Petrova and T. G. Jerayan (USSR Academy of Sciences, Moscow, USSR). “Rapid terpenols concentration and their subsequent spec- trophotometric determination,” J. Cacho, and V. Ferreira (University of Zaragosa, Spain). “Fast gas chromatographic separations with ultraviolet photodiode array spectrophotometric identification,” V.Lagesson (Faculty of Health Sciences Linkoping, Sweden). Friday Combined Techniques in Molecular Spectroscopy. 2. Invited lecture. A. F. Fell, University of Bradford; “Advances in computer-aided multi-channel detection in LC - UV and LC “Analysis of Triacylglycerols by HPLC - GC and LC - MS,” N. W. Rawle, R. G. Willis and J. D. Baty (Ninewells Hospital, Dundee). - FL.”110 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 “Application of a high-performance GLC - MS system for the study of wide volatility ranges of alkanes extracted from biological sources,” W. McDonald and P. J. Baugh (University of Salford). “Laser mass spectrometry,’’ D. L. Andrews (University of East Anglia, Norwich). Invited lecture. D. Mattson, Mattson Instruments Inc., Madison, WI, USA; “GC - FTIR.” “Supercritical fluid chromatography - infrared spectro- scopy,” K.H. Bartle and M. Raynor (University of Leeds). “TGA coupled to FTIR spectroscopy for polymer analysis,” J. E. Sellors and R. A. Spragg (Perkin-Elmer Ltd., Beacons- field, Buckinghamshire). “Industrial uses of FT-IR,” B. W. Cook and J. M. Chalmers (ICI Chemicals and Polymers Ltd., Runcorn, Cheshire). Friday Atomic Spectroscopy “Quantitative analysis by laser ablation and atomic spec- trometry-pipe dream or reality,” Michael Thompson (Birk- beck College, London), Simon Chenery (Imperial College, London) and Leslie Brett (The Royal Arsenal East, Woolwich, London). “A comparison of solid sampling methods for ICP-OES and ICP-MS,” S. A. Darke and C. J. Pickford (Harwell Labora- tory, Didcot) and J.F. Tyson (Loughborough University of Technology). “ICP-OES analysis of small sample volumes with rapid background correction,” Fiona Diver, Louise M. Garden, Guy Wiltshire, Robbin Nichol, Allan M. Ure and David Littlejohn (University of Strathclyde, Glasgow). “On-line pre-concentration and sample clean-up using con- tinuous precipitation and filtration in flow injection flame atomic absorption spectrometry,’’ C. E. Adeeyinwo, E. Debrah and J. F. Tyson (Loughborough University of Tech- nology). Friday Atomic Spectroscopy The Alan Date Memorial Session on ICP-MS Invited Lecture. R. S. Houk, Iowa State University; “Fun- damental studies in inductively coupled plasma mass spec- t rome t r y . ’’ “Alan Date, his career and achievements,” J. Mather (British Geological Survey, London).“Collaborative work at the University of Surrey,” A. L. Gray (University of Surrey). “New sample introduction techniques for ICP-MS ,” R. Hutton (VG Analytical, Winsford). “Flow injection strategies in ICP spectrometry,’’ C. McLeod (Sheffield City Polytechnic). POSTERS Monday Food “Chemical indicators of decomposition for surimi and surimi- based products,” Thomas A. Hollingsworth, Jr., Marleen M. Wekell, John J. Sullivan, James D. Torkelson, Jr. and Harold R. Throm (US FDA, Seattle, WA, USA). “Simultaneous flow injection determination of total and free calcium in milk,” Ancel van Rensburg and Jacobus F. van Staden (University of Pretoria, RSA). “Trypsin inhibitors analysis: direct chromatographic titra- tion,” G. Raspi, A. Lo Moro and M.Spinetti (Universita di Pisa, Italy). “Determination of lead in food slurry samples by hydride generation AAS using different acid - oxidant mixtures,” Yolanda Madrid, Milagros Bonilla and Carmen Camara (Complutense University, Madrid). “Ion-selective electrode determination of sodium in dairy products,” R. Perez-Olmos and J. M. Castresane (University of Basque Country, Bilbao, Spain). “A comparison of detection methods for the enzymatic determination of ascorbic acid,” G. M. Greenway, E. Elba- sheir and Y . H. Yip (University of Hull and Humberside College of Higher Education). “Direct determination of molybdenum in milk by elec- trothermal atomic absorption spectrometry,” P. Bermejo Barrera, C. Pita-Calvo, F. Bermejo-Martinez and J. A. Cocho de Juan (Santiago de Compostela, Spain).“Identification of fl-hexachlorocyclohexane (PHCH) in young goat meat,” J. J. Sanchez Saez, M. D. Herce Garralleta, M. L. Folgueiras Alonso and J. Balea Otero (Centro Nacional de Alimentacion, Majadahonda, Madrid). “Identification of dichlorobenzene in edible oil and mineral water bottled in poly(viny1 chloride) (PVC) containers,” J. J. Sanchez Saez, M. D. Herce Garraleta and J. Balea Otero (Centro Nacional de Alimentacion, Majadahonda, Madrid). “Determination of amino acids in fruit juice by HPLC,” J. Cacho, A. Guitart and P. Hernandez Orte (University of Zaragosa, Spain). Monday Electroanalytical Chemistry “Polarographic studies of drugs of imadazole derivatives,” Zbigniew Fijalek, Jerzy Chodkowski and Malgorzata War- owna (Medical University, Warsaw, Poland). “Determination of cholesterol by biocoulometry using porous carbon felt,” Shunici Uchiama, Shuichi Kato and Shuici Suzuki (Saitama Institute of Technology, Japan), Osamu Hamamoto (Mitsui Engineering and Shipbuilding Co., Chiba, Japan).“Cyclic voltammetric analysis of the oxidative dimerisation of naphthoquinones,” H. D. Nelson, G. Lachmann and J. A. K. du Plessis (Potchefstroom University, RSA). “Polarographic determination methods of cloxazolam,” F. J. Rodriguez, R. M. Jimenez and R. M. Alonso (University of Basque Country, Bilbao, Spain). “Constant current coulometry for precise and accurate determination of composition element of CdTe semiconductor material,” M. L. Lee and M. H. Yang (National Tsing Hua University, Taiwan). “A coulometric determination of thioglycollic acid using the depolarisation end-point detection on glassy carbon - calomel indicating couple,” Vladislava M.Jovanovic and Momir S. Jovanovic (University of Belgrade, Jugoslavia) . “Application of the standard additions method in the resolution of the cobalt and nickel voltammetric peaks in real samples ,” Clinio Locatelli and Francesco Fagioli (University of Ferrara, Italy). “Water determination in ascorbic acid using pH glass electrode,” M. R. 0. Karim and Th. M. Karadaglic (Salahad- din University, Iraq). Monday Flow Analysis “Selective determination of Triton-type non-ionic surfactants in water by online clean-up and FIA,” M. E. Leon Gonzalez, M. J. Santos-Delgado and L. M. Polo-Diez (Universidad Complutense, Madrid, Spain).“Optimisation of flow-through sandwich ISE’s for use in FIA,” Julia M. C. S. Magalhaes and Adelio A. S. C. Machado [CIQ(UP) Porto, Portugal]. “Spectrophotometric determination of cobalt as tetrathio- cyanatocobaltate(I1) after flow injection extraction with ethylenebis(tripheny1phosphonium) cation,” M. Chimpalee,111 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 M. Harriott and D. Thorburn Burns (The Queen’s University of Belfast). Ti1 es d ay Chromatography “Synthesis and characterisation of new polymeric reversed phases for use in high-performance liquid chromatography,” S . 0. Akapo, T. M. Kong and C. F. Simpson (Birkbeck College, University of London). “Dynamic headspace gas chromatography analysis: applica- tion in chimiotaxonomy of truffles,” Thierry Talou and Antoine Guset (INPT, Toulouse, France).“A comparison among different methods for the ion chromatographic determination of nitrite in the presence of a large amount of chloride ,” Paolo Pastore, Irma Lavagnini, Andrea Boaretto and Franci Magno (University of Padova, Italy). “Chelating solid phases,” J. D. Glennon and S. Srijaranai (University College, Cork). “A chromatographic study on TBP degradation in the system TBP - kerosine - HND,” A. M. Al-ani (Nuclear Research Centre, Baghdad, Iraq). “Derivatisation with phenyl isocyanate. Application to polyhydroxylated compounds,” Arlette Baillet (Centre D’Etudes Pharmaceutiques, Chatenay-Malbry, France). “Determination of vinyl chloride monomer residues in poly(viny1 chloride) by gas - liquid chromatography,” Guber- ska Jadwiga (8, Rydygiera St., Warsaw, Poland).Ti4 es d ay Sensors “Alternative membrane support matrices for ISFETS ,” S. Johnson, G. J. Moody and J. D. R. Thomas (University of Wales College of Cardiff). “Potentiometric sensing of guanidinium with polyether-type neutral carriers,” F. N. Assubaie, G. J. Moody and J. D. R. Thomas (University of Wales College of Cardiff). “Analytical performance and applications of double-mem- brane ion-selective electrodes. Part 1. Determination of nitrates,” Jose Aznarez. Carmelo Diaz, Juan Carlos Vidal and Javier Galban (University of Zaragosa, Spain). “Analytical performance and applications of double-mem- brane ion-selective electrodes. Part 2. Determination of potassium and metoclopramide ,” Jose Aznarez, Carmelo Diaz, Juan Carlos Vidal and Javier Galban (University of Zaragosa, Spain).“New types of bromide selective membrane electrodes based on methyl methacrylate matrices, and their use in drug analysis,” T. Pastor and M. Pastor (Faculty of Sciences, Belgrade), K. Kalajdzievski (Faculty of Sciences, Skopje, Yugoslavia). “Development of a test rig for evaluating metal oxide gas sensors in solvent analysis,” A. Bruce and S. J. Haswell (Thames Polytechnic, Woolwich, London). Tuesday General “Monitoring of XSKe concentration in atmosphere by a portable sampling system,” J. G. Lo (National Tsing Hua University, Taiwan), Y. C. Yand and K. D. Jow (Atomic Energy Council, Taiwan). “Characterisation of complexation equilibria in the AgI(s) - I-(aq), C1-(aq) system using radiochemical procedures,” I.Taljaard and P. 0. Coetzee (Rand Afrikaans University, Johannesburg, RSA). “Titrations with standard solutions of manganese(II1) and manganese(1V) by biamperometric end-point detection method,” T. Pastor, M. Dobricic and M. Pastor (Faculty of Sciences, Belgrade, Yugoslavia). “Linearity of Gran plots for multi-step titrations,” Carlo Macca (University of Padova, Italy). “A simple radioisotopic method for measurement of DNA repair synthesis in pollen,” S. V. Andreichenko and D. M. Grodzinsky (Kiev Medical Institute, USSR). “The occurrence, transport and turnover of mercury in an aquatic milieu-analytical methods and results,“ D. C. Baxter, W. Frech and E. Lundberg (University of Umea, Sweden). “Fluorescent phase modulation techniques for the study of solution rotational kinetics,” J.Birmingham (Unilever Research, Port Sunlight Laboratory, Cheshire). “Depth profiling by impulse response photothermal beam deflection spectroscopy,” S. A. Johnson and R. M. Miller (Unilever Research, Port Sunlight Laboratory, Cheshire). “Quantitative 3-D structural studies of materials by confocal scanning microscopy,” D. J . Joyner, N. J. Ness and M. Moss (Unilever Research, Port Sunlight Laboratory, Cheshire). Thursday Atomic Spectroscopy “Analysis of phosphorus and germanium dopants in silica optic fibres,” T. J. Elms and R. R. Pierson (Telecom Research Laboratories, Clayton, Victoria, Australia). “Analysis of heavy metal fluoride (HMF) glasses and starting materials,” R. N. M. Barrett (Telecom Research Laboratories, Clayton, Victoria, Australia).“Determination of cadmium by electrothermal AAS after deposition on a L’vov platform ,” Juan Carlos Vidal, Francisco Monreal and Juan Ramon Castillo (University of Zaragosa, Spain). “Determination of vanadium in water by electrothermal atomisation atomic absorption spectrometry with graphite tube pre-heating,” P. Bermejo Barrera, A. Bermejo Barrera and F. Bermejo Martinez (Santiago de Compostela, Spain). “PVC sample treatment and determination of metallic additives by electrothermal and flame atomic absorption spectrometry,” M. A. Belarra, J. M. Anzano and J. R. Castillo (University of Zaragosa, Spain). “Gas phase sample introduction in atomic spectroscopy speciation of As(III)/(V), Sb(III)/(V), Sn(II)/(IV), Se(1V) and In(II1) using volatile covalent hydrides,” J.R. Castillo, J. M. Mir and M. T. Gomez (University of Zaragosa, Spain). “Volatilisation of metal complexes for direct introduction of vapour-phase sample in atomic absorption spectrometry with flame, silica tube and graphite furnace,” J. R. Castillo, J. M. Mir and C. Bendicho (University of Zaragosa, Spain). “Introduction of biological samples in atomic spectrometry,” J. R. Castillo, A. Fernandez, A. Lopez Molinero and M. C. Martinez (University of Zaragosa, Spain). “The determination of heavy metals in shellfish using graphite furnace atomic absorption spectroscopy and X-ray microanalysis,” C. A. Donaghy, M. Harriott and D. Thorburn Burns (The Queens University of Belfast). “Determination of nickel in biological samples by elec- trothermal atomic absorption spectrometry using a previous extraction with 1,5-bis(di-2-pyridylmethyl)thiocarbonohydraz- ide,” J.M. Cano Pavon, E. Vereda, C. Bosch and A. Garcia de Torres (University of Malaga, Spain). “A novel spectrometer and background correction system for simultaneous multi-element analysis by atomic absorption and atomic emission spectrometry,” Robbin Nichol, Claire Smith, David Bolland and David Littlejohn (University of Strathclyde, Glasgow). “Speciation of antimony in environmental materials using hydride generation atomic absorption spectrometry,” Bashir Mohammad, Allan M. Ure and David Littlejohn (University of Strathclyde, Glasgow). “Analysis of biological slurries by electrothermal atomic absorption spectrometry,” Sean Lynch, David Bolland and David Littlejohn (University of Strathclyde, Glasgow).112 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 “Development in probe atomisation for electrothermal atomic absorption spectrometry,” Mansha Chaudhry, J.Campbell Murray, Robbin Nichol and David Littlejohn (University of Strathclyde, Glasgow). “Advances and prospects in flame spectrometry of traces,” E. D. Prudnikov (State University of Leningrad, USSR). “Solid phase extraction cartridge for trace metals,” S. Srijaranai and J . D. Glennon (University College, Cork). Thursday Chemometrics “General aspects of errors theory in analysis,” E. D. Prudnikov (State University of Leningrad, USSR). Friday Micro and Chemical Methods “The determination of very low fluoride levels by alizarin fluorine blue - lanthanum solvent extraction absorptiometry ,” Marie M.Ferris and Michael A. Leonard (The Queens University of Belfast). “The effect of anions in the aqueous phase on the spectral characteristics of the extractable ternary nickel bisdiaryl thiocarbazonate - 1,2’-bipyridyl (or 1,lO-phenanthroline) com- plexes,” A. M. Kiwan, M. Y. Khalid, A. A. Bahajaj, F. M. Hassan and W. Hamdan (University of Kuwait). “Determination of molybdenum in soil samples by dithiol MIBK method,” Anneli Mikkonen and Jouni Tummavouri (University of Jyvaskyla, Finland). “Extraction and spectrophotometric determination of titan- ium and vanadium with Eriochrome Cyanine R in presence of a cationic surfactant,” Jose Aznarez, Juan Carlos Vidal, Miguel Angel Navas, Rafael Olivera and Carmelo Diaz (University of Zaragosa, Spain). “Synergic extraction of Cu(I1) with purified LIX 54 and neutral organophosphorus esters,” M.J. Zapatero, M. A. Olazabal and J . M. Castresane (University of Basque Country, Bilbao, Spain). “Sources of error in total chromium determination following perchloric acid oxidation. A reinterpretation ,” Kenneth E. Collins and Carol H. Collins (Universidade Estadual de Campinas, Brazil) , Cielita Archundia (Universidad Nacional Autonoma de Mexico). “Spectrophotometric determination of bismuth after extrac- tion of 1-naphthylmethyl triphenylphosphonium tetraiodo bismuthate(II1) with microcrystalline benzophenone ,” D . Chimpalee and D. Thorburn Burns (The Queens University of Belfast). “Spectrophotometric studies on Sc(III), Y(II1) and La(II1) chelates with 6-phenylazo-3-0-arsonphenylazo chromotropic acid,” L.M. Shafik and H. Ibrahim (Central Services Laboratory, Cairo, and Cairo University, Egypt). “Mixed ligand-sulphito complexes of chromium(II1) ,” Kamal A. R. Salib, Salah B. El-Maraghy and Saied M. El-Sayed (Ain Shams University, Cairo, Egypt). “Interference of nitrile group in cyanide determination in polluted waters by the standard method,” R. Rubio, M. T. Galceran and G. Rauret (University of Barcelona, Spain). “A new method for the determination of total carbonate by ligand exchange,” M. D. Galindo Riano, M. Garcia Vargas and J. A. Munos Legva (University of Cadiz, Spain). “Synthesis of 5-(4,5-dimethyl-2-thiazolylazo)-2,3-diamino- toluene and its application to the spectrophotometric determi- nation of palladium,” Zhang Guang, Zhang Xiao-ling and Hu Yan-rong (Shaan Xi Normal University, China).“Spectrophotometric studies on platinum - prochlorpera- zine - bismethanesulphonate complex,” A. Thimme Gowda (A. V. K. College for Women, Karnataka, India). “Spectrophotometric determination of cobalt with 5-(43- dimethyl-2-thiazolylazo)-2,4 ,-diaminotoluene ,” Zhang Guang, Zhang Xiao-Ling and Hu Yan-rong (Shaan Xi Normal University, China). Friday Molecular Spectroscopy Two dimensional NMR analysis of mixtures,” R. N. Ibbett and I. R. Herbert (Courtaulds Research, Coventry). “Trace analysis of NOx by laser induced fluorescence spectroscopy,” A. J. Yates, V. M. Young, M. R. S. McCoustra and J. Pfab (Heriot Watt University, Edinburgh). “Gas phase molecular absorption spectrometry diode array detection coupled to hydride generation: study of As, Sb, Se, Te, Bi, Ge and Sn,” J. Sanz, F. Gallarta, J. Galban and J. R. Castillo (University of Zaragosa, Spain). “Analysis of petroleum products by field ionisation mass spectrometry,” M. Kuras and L. Vodicka (Institute of Chem- ical Technology, Prague, Czechoslovakia). Friday General “Measuring the apparent dirtyness of surfaces by image analysis,” E. Mahers (Unilever Research, Port Sunlight, Cheshire). “Direct observation of surfactant micellar structures,” J. N. Ness and P. G. Cummins (Unilever Research, Port Sunlight Laboratory, Cheshire). “Fluorescent photobleaching techniques in the study of surface lateral diffusion,” J. Birmingham (Unilever Research, Port Sunlight Laboratory, Cheshire). “EXAFS investigation of the interaction between oxide abrasives and aqueous zinc species,” A. T. Steel (Unilever Research, Port Sunlight Laboratory, Cheshire). “Copper( 11) complexes with hydrozopyrazolone ligands,” Salah B. El-Maraghy, G. A. El-Znang, Kamal A. R. Salib and Shaker L. Stefen (Ain Shams University, Roxy, Cairo, Egypt). “Sulphitoamine complexes of cobalt(III),” Kamal A. R. Salib, Samy M. Abu El-Wafa, Salah B. El-Maraghy and Saied M. El-Sayed (Ain Shams University, Roxy, Cairo, Egypt). “Normal sulphites of metals,’. Kamal A. R. Salib, Salah B. El-Maraghy, Samy M. Abu El-Wafa and Saied M. El-Sayed (Ain Shams University, Roxy, Cairo, Egypt). Friday Environmental “Determination of releases in the application of polyester powder paints,” Jari Pukkila (University of Kuopio, Finland).

ISSN:0144-557X    

DOI:10.1039/AP9892600106

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS. MARCH 1989. VOL 26 113 Equipment News Spectrometers Two new versions of the 1700X series Fourier transform infrared spectrometers are announced: the near infrared version, covering the range 15 800-2700 cm-1, and the far infrared version, covering the range 720-30 cm-1. For each there is a choice of data systems, a dedicated spec- troscopy terminal or the 7000 Series professional computer. Perkin-Elmer Ltd., Post Office Lane, Beaconsfield, Buckinghamshire HP9 1QA. Spectrometers The new PU9800 Series Fourier Trans- form infrared spectrometers offer superb control and data manipulation facilities through an AT-compatible P3202 com- puter operating EAGLE IR software. The P3202 offers fast computing, high storage capability and access to standard IBM environment business software packages.Philips Scientific, Analytical Division, York Street, Cambridge CB1 2PX. Spectrometer An inductively coupled plasma atomic emission spectrometer, the Plasma 40 Wear Metals Analyser (P40 WMA), is optimised for the determination of wear metals in oil samples. It incorporates all the important features of the Plasma 40 ICP emission spectrometer. In addition, the sample introduction system is de- signed to withstand organic solvents such as xylene or kerosene. Perkin-Elmer Ltd., Post Office Lane, Beaconsfield, Buckinghamshire HP9 1QA. Direct Peaking Scanner for Spectrometers A programmable scanning channel with high precision, numerically controlled drive for the PV8606 series inductively coupled plasma optical emission spec- trometers allows direct peak positioning to be employed for fast measurement of non-routine elements.Philips Industrial and Electro-acoustic Systems Division, Building HKF, 5600 MD Eindhoven, The Netherlands. Electron Spin Resonance Spectrometers The first installation in the West of the RE series of ESR spectrometers has been completed at Royal Holloway and Bed- ford New College. Initial uses will include photosynthesis studies and the dating of geological materials to 0.5 x 106 years. Jeol UK Ltd., Jeol House, Grove Park, Colindale, London NW9 OJN. Spectroanalytical Systems Two series of integrated spectroanalytical systems, each including one (or more) monochromator, a detector (PMT and/or diode array), Spectralink electronics unit and PRISM software package, are an- nounced. Spectralink is built from a num- ber of modules, of which a wide range are available, including programmable HT power supply, photon counting data acquisition, lock-in amplifier/demodula- tor and drivers for choppers, mirrors and filter wheels.The PRISM software is con- figured to run on IBM-PCIAT, PS-2 and compatible computers. Instruments S.A. - EDT Ltd., 14 Trad- ing Estate Road, Park Royal, London NWlO 7LU. Gas Chromatography - Infrared Interface The Tracer capillary GC - FT-IR interface uses GC eluent trapping to achieve a 1-2 order of magnitude improvement in sensi- tivity over conventional GC - IR. The Tracer is designed as an accessory for the makers’ FT - IR systems. Bio-Rad Microscience Division, 53-63 Greenhill Crescent, Watford Business Park, Watford, Hertfordshire.Gas Chromatograph Designed to meet the needs of a busy analytical laboratory, the PU4400 is opti- mised for capillary analyses but also offers excellent performance on conventional packed column chromatography. Two new capillary injectors, one split - split- less, the other a programmable thermal vaporiser injector, offer outstanding per- formance with the most complex samples. Five types of detector are offered, and the PU4400 is available in five packages covering the vast majority of applications. Philips Scientific, Analytical Division, York Street, Cambridge CBl 2PX. Liquid Chromatograph The Model 338 gradient liquid chromato- graph links reliable pumps with pro- grammable ultraviolet - visible detectors and provides the advantages of single- point instrument control.The Model ll0B pump flow-rate range of 0.01-10 ml min-1 can be increased to 28 ml min-J with the addition of preparative pump- heads. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire. Modular HPLC Instrumentation At the heart of the new range of equip- ment is the PU4100M pump, available in isocratic, binary or quaternary versions and matchable with any detector from the makers’ range, thus allowing the analyst to configure a system to match his needs. An outstanding feature of the PU4100M is its upgradeability , allowing straightfor- ward conversions from isocratic to binary and quaternary systems. Philips Scientific, Analytical Division, York Street, Cambridge CB1 2PX. Modular Liquid Chromatography System Hewlett-Packard’s newly launched HP1050 Series modular range of liquid chromatography equipment is available for short-term rental.Users can either rent complete liquid chromatography systems configured to meet their require- ments, or individual components, such as detectors, pumps or autosamplers. Livingston Hire Ltd., Livingston House, 2-6 Queens Road, Teddington , Middlesex TW 11 OLB. HPLC Columns Part of the TosoH TSK-GEL family of HPLC columns, Progel-TSK resin-based and silica-based columns can separate or purify biological materials and organic solvent-soluble polymers by size-exclu- sion chromatography, hydrophobic inter- action chromatography and a variety of other specialised chromatographic mechanisms. Supelchem UK, Shire Hill, Saffron Walden, Essex CB 11 3AZ.Aldehyde Columns The HiPAC Aldehyde Column is an activated affinity column for the custom separation of antibodies, proteins, phar- maceuticals and biochemicals. It allows the user to immobilise his own ligand on a silica support, with only one pass of the ligand through the column. Chro:natoChem Inc., 2837 Fort Mis- soula Road, Missoula, MT 59801, USA. Diode Array Detection The Shimadzu SPD-M6A photodiode114 ANALYTICAL PROCEEDINGS. MARCH 1989, VOL 26 array ultraviolet - visible detectors incor- porate 512 elements and offer a resolution of 1 nm and an accuracy of fl nm over the wavelength range 195-670 nm. The SPD-M6A is controlled by an IBM PC or equivalent. Dyson Instruments Ltd., Hetton Lyons Industrial Estate, Hetton, Houghton le Spring, Tyne and Wear DH5 ORH.Analytical Columns Rapid, high resolution separations with high recovery of biomolecules are pos- sible with HRLC MA7 analytical col- umns. A full complement of MA7 ion exchangers in a 50 x 7.8 mm column format are available: a weak cation exchanger, carboxymethyl (MA7C); a weak anion exchanger, PEI (MA7P); a strong cation exchanger, sulphopropyl (MA7S); and a strong anion exchanger, quaternary amine (MA7Q). Recovery of proteins in the nanogram range (>98%) is possible with the HRLC MA7Q and MA7S columns. Bio-Rad Laboratories S.A., 19 Dreve De Senechal, B-1180 Brussels, Belgium. Conductivity Analyser The HRLC isocratic conductivity ana- lyser is based on a high performance detector giving p.p. b. sensitivity. Expen- sive suppressor columns are not required, as the patented design of the five-elec- trode flow cell and a built-in temperature control contribute to greatly reduced noise.Bio-Rad Laboratories S.A., 19 Dreve De Senechal, B-1180 Brussels, Belgium. Software for Thin-layer Chromatography CATS is the latest development in soft- ware for TLC from Camag. A clear windowing menu format keeps the user informed of where he is at all times. CATS allows rapid screening (20 mm s-1) and fast data processing. Pilot scans give fast method testing and files can be easily identified because they are named rather than number coded. Features include video integration, linear and non-linear calibration, spectral peak purity and iden- tity testing with statistical verification, statistics including CV and CI, and auto- matic peak window adjustment for poor chromatography.BDH Ltd., Apparatus Division, P.O. Box 8, Dagenham, Essex RM8 1RY. Ion Chromatography Components Ion chromatography columns and detec- tors are available in matched pairs, allow- ing HPLC users to add superior chemical suppressed ion chromatography or pulsed amperometric detection to their labora- tory’s capabilities without having to buy a complete system. Packages offered include a pulsed amperometric detector and columns for carbohydrate determina- tions, and a conductivity detector module and separator column with a MicroMem- brane chemical suppressor device for ion chromatography. Dionex (UK) Ltd., 4 Albany Court, Camberley, Surrey GU15 2PL. Oxygen Analyser The Model 311C is a p.p.m.oxygen analyser offering true portability intrinsic- ally safe to cenelec standards. Weighing just 2 kg, it offers a convenient way to spot-check gas phase p.p.m. oxygen in a wide variety of quality assurance and process monitoring applications. Teledyne Analytical Instruments, The Harlequin Centre, Southall Lane, South- all, Middlesex UB2 5NH. Oxygen Analyser The Model 306WAM on-line trace oxy- gen analyser guards against oxygen con- tamination in hydrogen, nitrogen, argon and other ultra-pure gases used in the manufacture of high density VLSI and VHSIC devices. It offers full scale analy- sis as low as G500 p.p.b. of oxygen with outstanding accuracy (k 1%) and low range sensitivity (1%). Teledyne Analytical Instruments, The Harlequin Centre, Southall Lane, South- all.Middlesex UB2 5NH. Combustion Efficiency Analyser The MAX portable combustion efficiency analyser measures four flue gas paramet- ers (oxygen, carbon monoxide, total com- bustibles and temperature) and then auto- matically calculates net combustion effi- ciency. A theoretical calculation of car- bon dioxide content is also provided. When connected to a printer the MAX provides a permanent record of stored data including a print-out of its operating instructions. Also featured are automatic calibration of the oxygen analysis and auto-zero for the carbon monoxide and combustibles measurements. Teledyne Analytical Instruments, The Harlequin Centre, Southall Lane, South- all, Middlesex UB2 5NH. Portable Flue Gas Oxygen Analyser The Model 320P incorporates a built-in sampling system with an integral push- button operated pump to educt sample gas without positive pressure.The 320P has three standard ranges and is linear from 0 to 100%. The sensing element is maintenance-free, specific to oxygen, insensitive to flow-rate and has 90% response in less than 7 s. Teledyne Analytical Instruments, The Harlequin Centre, Southall Lane, South- all, Middlesex UB2 5NH. Oil Contamination Monitor The LCM I1 oil contamination monitor is ideal for determining the level of particu- late contamination in lubricating oils and hydraulic fluids. Portable and fully auto- matic, it reports data conforming to ISO/ DIS 4406 cleanliness standard. Coulter Electronics Ltd., Northwell Drive, Luton, Bedfordshire LU3 3RH. Automatic Analyser The BT 950 BioStar is for continuous flow analyses of water and other liquid sam- ples. Chemically inert, electronically acti- vated microvalves are used in place of traditional pumps and manifolds, and reagent delivery is by positive nitrogen displacement.Detection limits for nitrite, nitrate and ammonium, for example, are 4 p.p.b., 0.03 p.p.m. and 5 p.p.b., respec- tively. BioStar is also fast; for nitrate analysis, for example, it can deliver up to 90 samples h-1. It is supplied complete with autosampler and data handling system. Biotech Instruments Ltd. , 183 Camford Way, Luton, Bedfordshire LU3 3AN. Automatic Sample Changer With the Model 960SC automatic sample changer the ORION 960 autochemistry system can perform repetitive titrations and ion analyses unattended.The sample changer can accommodate up to 20 sam- ples per tray, Orion Research UK, Freshfield House, Lewes Road, Forest Row, East Sussex RH18 5ES. Titrator The Model 682 controls up to four titrat- ing burettes automatically with up to 40 stored programs. A single button runs any sequence of stored programs from a library of 40 individual or linked proce- dures. With two burettes the Model 682 is a dedicated Karl Fischer and a poten- tiometric titrator in one, without the time and work of changing glassware.ANALYTICAL PROCEEDINGS. MARCH 1989, VOL 26 V. A. Howe and Co. Ltd., 12-14 St. Anne’s Crescent, London SW18 2LS. Chemical Oxygen Demand Analysis In chemical oxygen demand analysis it is necessary to decant the fluid from the tall narrow digestion tubes for titration of excess dichromate.As the ASP1 1000 combined redox electrode has an effective length of 175 mm and a diameter of only 9.5 mm it is now possible to titrate directly in the digestion tubes. Not only does this avoid decanting, but it increases precision the end.of.th-e processor. By rotation of the processor’s knurled knob, the plunger is slowly depressed and a gentle, con- trolled pressure is generated to force the solution dropwise through the SPE tube. Supelchem, London Road, Sawbridge- worth, Hertfordshire CM21 9JH. Distillation Systems A range of all-PTFE distillation systems and DURAN-glass distillation sets are supplied with outer threading on all joints, fitted with SAFELAB release and Radiometer D TS895 COD analyser system and minimises hazards.For single sam- ples a dedicated sample stand is recom- mended. Automated single titrations can be performed with the DTS812 multi- titration system. For ease of batch sam- pling there is the dedicated DTS895 COD analyser system. Radiometer Ltd., The Manor, Manor Royal, Crawley. West Sussex RHlO 2PY. Reagent Dispensing System Wellfill 5 is specifically designed as a single reagent dispenser with the capabil- ity of hands-off processing of up to 10 microplates in self-stacking format. It is able to deliver volumes infinitely variable from 25-400 ml per well determined by means of a program card system. It features an automatic stacking mechan- ism which will handle up to 10 microplates of any of the popular types, re-stacking them in the same sequence as provided.Denley Instruments Ltd., Natts Lane, Billingshurst, West Sussex RH14 9EY. Solid Phase Extraction Tube Processor The Visi-1 single, solid-phase extraction tube processor provides precise flow con- trol through a single SPE tube. An SPE tube is simply filled with the appropriate solution and attached to the adaptor at locking nuts. These patented devices, SAFELAB Stopper-loc-Nuts. make easy the assembly of the most complicated glass or PTFE distillation sets. A cata- logue is available. Safelab Systems Ltd., Bush House, 72 Prince Street, Bristol BS1 4HU. Inorganic Membrane Filters The ANOTOP PLUS range of disposable syringe filters incorporates a pre-filter to prevent clogging by removing extraneous matter prior to the filtration of smaller particles.In addition to the 0.2 and 0.02 pm pore sizes the ANOTOP range will now include a new pore size of 0.1 pm, ideal for the removal of mycoplasma. Anotec Separations Ltd. Thermometer The 2024-L hand-held thermometer has been designed for use with J-type thermo- couples. It has three switch-selectable temperature ranges of -30 to +199 or +6OO0C, and -30 to 1100°F. An impor- tant feature is the ability to memorise and display the highest temperature readings taken during a series of measurements. Lenton Thermal Designs Ltd., 12-14 Fairfield Road, Market Harborough, Leicestershire LE16 9 0 0 . 115 Peristaltic Pump The Clever peristaltic pump is a com- puterised dispensing filling machine. The operation program is entered through a computer included in the instrument, and all the operation stages are selected on the display.The selected cycle and the obtained data are printed. It is possible to select from 1 to 299 ml and four different programs: automatic, manual. filling and washing. Reproducibility is better than k0.2 ml. PBI International, Via Novara 89, 20153 Milano, Italy. Dispersion Units The Polytron homogeniser from Kine- matica, which uses the rotor - stator principle developed by Professor Wil- lems, is available in two sizes of the basic assembly: a 700-W motor handling vol- umes from 0.3 ml to 2 1, and a 1600-W motor which caters for volumes up to 25 1. Kinematica’s new dispersion units, the Polytron PT3000 and PT6000 and the Megatron 36-48, arriving shortly in the UK, attain peripheral speeds which can rapidly and repeatedly provide particle sizes down to 1 pm at a 50% lower noise level.WHM and Partners Ltd., Cathedral House, 5 Beacon Street, Lichfield, Staf- fordshire WS13 7AA. Mixing Equipment The Laboratory Series X10/20, the latest in a series of laboratory dispersing and mixing equipment from the German116 ANALYTICAL PROCEEDINGS, MARCH 1989, VOL 26 Ystral company, is designed for emulsify- ing, homogenising, dispersing, dissolving, suspending or aerating and allows vol- umes from 10 ml to 2 1 to be mixed at a complete range of speeds. A comprehen- sive range of accessories is available. The Scientific Instrument Centre Ltd., Unit 34D, Parham Drive, Boyatt Wood, Eastleigh, Hampshire SO5 4NU. Thermal Printers Three thermal printers offer high quality impressions with excellent bar code re- production.Each offers thermal transfer and thermal reactive processes and inter- faces with the makers’ Supaprint and Keyprint systems. The TP 255 produces labels of up to 255 mm maximum width, the TP 152 offers a maximum print width of 152 mm, and the TP 76 has a maximum print width of 76 mm. Map 80 Systems Ltd., Unit 2, Stoney- lands Road, Egham, Surrey TW20 9QR. Robotic System for Thermal Analysis A robotic system accessory has been introduced for use with the makers’ DELTA Series DSC 7 thermal analysis systems. It allows the automated testing of up to 48 samples without operator attention. Enhanced software options allow the use of an unlimited number of methods and the chaining of multiple methods for analysis of a single sample.Other features include automatic peak or glass transition analysis and printing of data and results, analysis of the data collected with the DELTA Series ad- vanced DSC software programs and the generation of hard capy sample file work- sheets. Perkin-Elmer Ltd., Post Office Lane, Beaconsfield, Buckinghamshire HP9 1QA. Computer Controlled Reactor The updated computer-controlled and automated reactor PC-Lab facilitates the running of most common laboratory processes, including the addition of reac- tants, temperature control for heating, cooling or isothermic conditions, reflux and distillation from vacuum to ambient pressure. Controlled addition of reactants can be determined by time, temperature or pH levels. Spectrum Computer Services plc, Spec- trum House, East Parade, Bradford, West Yorkshire BD1 5RJ.Information Data System for Testing Instruments The Moncal 10 system software, with an IBM personal computer, collects test results from the makers’ Rheometer, Mooney and Tensometer 10 instruments and offers the option of manually adding other test data. The system collects the results from as many as 10 instruments for display or printing and will compare specification limits of as many as 10000 compounds. The Moncal 10 system auto- matically displays a visual alarm and illuminates the failed light on the test instrument if a specification limit is vio- lated. Monsanto Instruments, Edison Road, Dorcan, Swindon, Wiltshire SN3 5HN. Laboratory Information Management System P-E Nelson’s Revision 1.1.6 of ACCESS- “LIMS offers a variety of additional functions.Results can be entered by operation as well as by methods and samples, and by chosen key word parameters. Samples may now be logged in as belonging to multi-tests and multi- studies, or as having no testing data at all, to meet the needs of laboratories with planned studies, i.e., toxicological or clin- ical protocols through to R and D and ad hoc type samples. Perkin-Elmer Ltd., Post Office Lane, Beaconsfield, Buckinghamshire HP9 1QA. Radioanalytic Imaging System From October lst, 1988, Automated Microbiology Systems Ltd. have assumed full responsibility for the sales and service of their AMBIS radioanalytic imaging system, which was previously handled by V. A. Howe and Co. Ltd. Automated Microbiology Systems Ltd., Grundy House, Somerset Road, Teddington, Middlesex TW11 8TD.Dual-laser Fibre Optic Test Set The Photodyne 2260XF is designed for use in the installation, maintenance and trouble-shooting of all fibre optic links operating at the standard wavelengths of 1300 and 1550 nm. The instrument oper- ates at either of these wavelengths or simultaneously at both. The transmitter section has two separate, electronically switched lasers, one for each wavelength; both remain energised continuously while the instrument is in use, thus avoiding repetitive warm-up times. Lambda Photometrics Ltd., Lambda House, Batford Mill, Harpenden, Hert- fordshire ALS SBZ. Literature A new applications data sheet outlines the use of primers, synthesised on a Beckman 200A automated DNA synthesiser, for sequencing various mRNA strands which encode mouse immunoglobulin heavy chains.The mRNA sequencing method and the synthesis of the four required dideoxynucleotides are described and results are presented by polyacrylamide gel electrophoresis. Information in this data sheet has been produced by the Department of Medical Biochemistry at the University of Geneva. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire. A brochure describes the FIP - Asarster bacteriological media preparation system. The instrument features alphanumerical display with friendly instructions for instrument - operator dialogue. The maxi- mum volume which can be processed per cycle is 10 1 and the minimum 2 1. Pool Bioanalysis Italiana, Via Novara 89, 20153 Milano, Italy.A new 289-page report, “Sensors and Monitoring Instruments for Fermentation Bioreactors in Europe,” takes a close look at the market for animal cell culture products. Analyses and forecasts are pro- vided by product type and application, end user industry and geographical region. Frost and Sullivan Ltd., Sullivan House, 4 Grosvenor Gardens, London SWlW ODH. A brochure outlines recent advances made by the Company in inductively coupled plasma mass spectrometry and introduces the PlasmaQuad PQ2, de- signed to meet the requirements of most routine analytical applications, and the PlasmaQuad PQ2 Plus, which features time resolved analysis and incorporates an extended dynamic range, giving detec- tion limits from p.p.t. to 100 p.p.m. VG Elemental Ltd., Ion Path, Road Three, Winsford, Cheshire CW7 3BX.OPUS 2000, an advanced mass spec- trometry data system, is the subject of a brochure. Based on the DEC VAXstation range of workstations and making use of the VMS operating system, OPUS 2000 provides a flexible software system cap- able of being operated either with menus and mouse or from the keyboard. Also announced is the AutoSpec mass spec- trometer, which features a friendly user interface and total computer control. VG Analytical Ltd., Floats Road, Wythenshawe M23 9LE. The 1988-89 “Ciba Corning World of Science” catalogue documents the full range of Ciba Corning analytical instru- ments, including the Delta I1 series of pH meters, Premium electrodes, Chroma col- orimeters, the 2800 Spectrascan ultra- violet - visible spectrophotometer, 965D carbon dioxide analyser and the 410 flame photometer.Ciba Corning Diagnostics Ltd., Hal- stead, Essex C 0 9 2DX. A brochure gives details of the DR/2000 spectrophotometer, which eliminates the task of calibration curve construction. Convenient, premeasured, unit-dme reagents minimise time spent on reagent and standard preparation. Camlab Ltd., Nuffield Road, Cam- bridge CB4 ITH. A Chromatography Supplies Catalogue presented as eight separate sections in theANALYTICAL PROCEEDINGS. MARCH 1989, VOL 26 117 form of individual booklets covers capil- lary columns, syringes, thermal desorp- tion, headspace, autosampling and ion trap detector consumables, recorders, printer - plotters, integrators and data storage consumables, ferrules, fittings and tubings, and miscellaneous consum- ables.Perkin-Elmer Ltd., Post Office Lane, Beaconsfield, Buckinghamshire HP9 1QA. A 70-page Capillary Gas Chromato- graphy Supplies Catalogue focuses on applications for acids, environmental analyses, flavours/fragrances, glycols, PCBs, pesticidesiherbicides and pet- roleum products. Product accessories are also included. Free technical literature is highlighted. Also available is the 82-page Environmental Chromatography Sup- plies Catalogue. which focuses on packed and capillary column gas chromato- graphy, HPLC, sample preparation and chemical standards. Supelchem, Shire Hill, Saffron Wal- den, Essex CBll 3AZ. A 24-page brochure, “High Performance Liquid Chromatography Products,” des- cribes the Accusphere columns and acces- sories for HPLC.It is illustrated with 38 chromatograms of samples analysed with Accusphere columns, including amino acids, drugs, toxins, insecticides, sugars, vitamins. fatty acids, antioxidants and alcohols. J and W Scientific, 91 Blue Ravine Road, Folsom, CA 95630. USA. A brochure describes the comprehensive range of modular components in the Shimadzu LC-6C HPLC system. Dyson Instruments Ltd., Hetton Lyons Industrial Estate, Hetton, Houghton le Spring, Tyne and Wear DH5 ORH. A brochure describes a range of auto- sampler vials, caps, septa and inserts. Of particular interest are very low prices for the Waters 48- and 96-tray samplers, Perkin-Elmer ISS 100 and the Gilson - Kontron - Spectra Physics Range. HPLC Technology Ltd., Wellington House, Waterloo Street West, Maccles- field, Cheshire SKll 6PJ. The Biogel range of electrophoresis equipment is described in a brochure. Included are the Biogel Easy dual vertical slab gel electrophoresis unit, the Biogel Submarine units for separation of nucleic acid samples in horizontal agarose gels, the Biogel Mini vertical system designed for use with mini polyacrylamide gels, the Biogel Flexi vertical sequencer, the Biogel drying frame and the Biogel blot- ter, as well as a range of power supplies.Biotech Instruments Ltd., 183 Camford Way, Luton, Bedfordshire LU3 3AN. A leaflet introduces a range of equipment for microdialysis: the CMAil00 microin- jection pump. the CMAi110 liquid switch, the CMAI130 in vitro stand, the CMA/140 microfraction collector, the CMAilO microdialysis probe and a complete range of documentation, including a com- prehensive manual on microdialysis in theory and practice, extensive biblio- graphy, application notes, etc.Biotech Instruments Ltd., 183 Camford Way, Luton, Bedfordshire LU3 3AN. Included in Volume 10, Number 2, of Analytical Bulletin are items on chromat- ography, microscopy, spectrophotometry and spectrometry. Philips Scientific, Analytical Depart- ment, York Street, Cambridge CB12PX. Issue number 10 of “Waters Column” contains items on Powerline HPLC, new HPLC detectors, enhanced networking systems, automated sample preparation, peptide separations, copolymer analysis and new chemical products. Millipore (UK) Ltd., Waters Chromat- ography Division, 11-15 Peterborough Road, Harrow, Middlesex HA1 2BR. A brochure presents the CMA/200 tem- perature controlled HPLC robot for autoinjection, fraction collection, pipet- ting and column switching. Biotech Instruments Ltd., 183 Camford Way, Luton, Bedfordshire LU3 3AN. Jun-Air, the quiet compressor people, have just brought out two new product brochures showing their oil-lubricated oil-less ranges of compressors. These range from 1/6 hp to 3 hp and have outputs of 17-350 1 min-1. All products are covered by a 2-year guarantee. Jun-Air (UK) Ltd., Bridge Street, Lin- wood, Paisley, Renfrewshire PA3 3DG. Issue number 8 of Laboratory Equipment Info gives details of equipment and con- sumables for spectrophotometry, chem- ical oxygen demand testing, viscometry, elemental X-ray analysis, pH measure- ment, chromatography and other applica- tions. Camlab Ltd., Trinity Hall Farm Indus- trial Estate, Nuffield Road, Cambridge CB4 1BR. A brochure catalogues a comprehensive range of plastic labware and deals with special printing and colours, custom moulding, special fabrication, the proper- ties of plastics, cleaning plastic labware, and bottle and aspirator specifications. Just Plastics Ltd., Cromwell House, Staffa Road, Leyton, London El0 7PY.

ISSN:0144-557X    

DOI:10.1039/AP9892600113

出版商:RSC    

年代:1989

数据来源: RSC