ISSN:0144-557X    

DOI:10.1039/AP98825FX021

出版商:RSC    

年代:1988

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June 1988 ANPRDI 25(6) 177-208 (1 988) Analytical Proceedings Proceedings of the Analytical Division of The Royal Society of Chemistry CONTENTS 177 Editorial 178 Analytical Viewpoint 'The Use of Robots for Automation in the Radiochemical Laboratory' by J. Huddleston 182 SUMMARIES OF PAPERS 182 The COSHH Regulations-the Challenge for the Analyst 182 'The Proposed Control of Substances Hazardous to Health Regulations: a Practical Approach to Assessment' by M. F. Curtis 'An Overview of Monitoring Methodologies' by B. Miller 184 1 84 'Industrial Hygiene Programme at an American Army Medical Centre in West Germany' by Mark B. Geiger 'Review of Atmosphere Analysis in the Process Industries' by J. R. P. Clarke 188 190 'Sensitive Portable Gas Chromatograph with Data Retrieval and Communications Capability for Remote Surveillance of Toxic Gases and Vapours in Plant' by Martin Adams and Mark Collins 'Quality Assurance in the Environment' by L.R. Pittwell 'The Relevance of Standards' by R. G. Collyer 'A Quality Assurance Viewpoint from Industry' by H. T. J. Chilton 'Laboratory Characteristics Affecting Quality Assurance Performance' by C. E. Wilde 'Information Management as a Quality Tool' by G. E. Martin 'Good Laboratory Practice and Computerisation in the Analytical Laboratory' by David L. M. Weller 192 Quality Assurance: Information and Its impact on Quality 192 194 195 195 197 199 GLP and Quality Assurance 199 201 Equipment News 204 Publications Received 205 Conferences and Meetings 206 Courses 206 University of Bologna Sigillum Magnum 208 Analytical Division Diary Typeset and printed by Black Bear Press Limited, Cambridge, England

ISSN:0144-557X    

DOI:10.1039/AP98825BX023

出版商:RSC    

年代:1988

数据来源: RSC

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177 ANALYTICAL PROCEEDINGS. JUNE 1988. VOL 25 Editorial Research Topics Twenty-five years ago, in April, 1963, an Ordinary Meeting of the Society for Analytical Chemistry was held at Chelsea College of Science and Technology, at which six short papers were presented by young research workers in Universities and Colleges of Advanced Technology. This was the first of a series of meetings held each year at centres with depart- ments of Analytical Chemistry all round the country. Papers for presentation are accepted by the Programmes Committee from young research workers who are completing their work for a postgraduate degree. After 1974, when the title of the meeting was changed to “Research and Develop- ment Topics in Analytical Chemistry,” equivalent research workers from industry and the public services were invited to participate.In 1974, Centenary Year, the meeting was held in Cambridge with the Society AGM and there were 16 papers. These meetings had become a regular feature in the annual calendar. They had evolved their own traditions. Each paper is allowed 20 minutes for presentation with 5 minutes for questions, and over-running the allotted time is frowned upon. In the discussions senior lecturers and profes- sors are encouraged to hold back, and the speaker from the “host” institution always gives the last paper of the meeting. A pleasant feature is that a small prize is given for the best presentation. An infor- mal dinner is held on one evening, and Walter Plinge generally manages to put in an appearance. Summaries of many of the papers appear in Analytical Proceedings while some are published in full in The Analyst.From 1980, the meetings have included the Divisional Silver Medal Lecture, when awarded, and from 1985 the Belcher Memorial Lecture has also been part of the Programme. From 1981 the oral lectures have been accompanied by ses- sions of posters. Over the years with some 320 papers and many posters every branch of analytical chemistry has been covered. This year the 26th meeting is being held at Plymouth Polytechnic and next year it goes over the water to the National Institute for Higher Education, Dublin. The programme of papers to be presen- ted at this year’s meeting at Plymouth, July 1&19th, is given inside the back cover of this issue. D. I. COOMBER EUROANALYSIS VII August 26th-31~t, 1990 Vienna, Austria This All-European Conference will emphasise methodological developments and especially the role of analytical chemistry for problem solving in major areas of science, such as clinical, pharmaceutical, forensic, food, agricultural and environmental chemistry, materials science, biotechnology, arts and archaeology.Additionally, special sessions discussing highly relevant topics, such as COBAC (Computer Based Analytical Chemistry), will be scheduled. Furthermore, a large exhibition of instruments, reagents and literature as well as an attractive social programme will be organised. The Conference Praesidium is: J. F. K. Huber, Vienna; E. Roth, Gif-sur-Yvette; D. T. Burns, Belfast; and L. Niinisto, Espoo. For registration and further information please contact the Secretary General, Prof. Dr. M. Grasserbauer, c/o Interconvention, Austria Centre Vienna, A-I450 Vienna, Austria (Phone: 43-222-2369/647; Telex: 11 18 03 lcos a; Cables: lntecon Wien; Fax: 43-222-2369/648),

ISSN:0144-557X    

DOI:10.1039/AP9882500177

出版商:RSC    

年代:1988

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178 ANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 Analyt ica I View point The following is a member of what is intended to be a continuing series of articles providing either a personal view of part of one discipline in anaytical 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 at 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 Use of Robots for Automation in the Radiochemical Laboratory J.Huddleston Instrumentation and Applied Physics Division, Harwell Laboratory, Oxfordshire OX1 I ORA After a rather hesitant start, the use of robotics as a means of automation for laboratory analysis is becoming considerably more of a routine exercise than a major development pro- gramme. Pioneers in the field of applying robots to chemistry generally accepted the implementation of this style of system as a learning exercise and most had a significant development programme before their applications were used routinely. However, the equipment manufacturers have responded to the needs of the scientist and now it is possible to develop applications in days rather than months. System developers have several choices to satisfy their requirements. Solutions can be implemented based around a robotic arm, such as those produced by Zymark or Perkin-Elmer. An alternative is to develop a system based around a self-contained unit, such as the Waters Millilab (Fig.1). There may be grounds for producing a specific, custom built mechanism and there is always the intermediate solution, where an application is constructed from a mix of commercial and custom constituents. Table 1. Common reasons for introducing robotic systems Improvements in sample throughput Improvement in sample analysis reproducibility Release of qualified staff for more interesting work Use of lower grades of staff Flexibility of equipment in changing procedures Removal of staff from hazardous chemicals or environments Experience in laboratories at Harwell indicates that there are wide extremes of requirements in radiochemical applica- tions.At one end, where a glovebox is essential for contain- ment, the working area is so compact that a human operator is the only practical solution. At the other extreme, in applica- tions with a high throughput of samples, the equipment requirements and financial justifications are such that a specific mechanism is appropriate. The mid-ground is currently covered by some form of fixed automation, usually a sample changer of some description. Advantages of Robotic Systems Table 1 is extracted from a brief survey of some of the published literature on laboratory robotics, and lists in roughly decreasing frequency the more common reasons quoted for the introduction of robotics. Sample throughput is usually achieved by the operation of the equipment overnight or at weekends rather than by improvements in the cycle time of the analysis.Gains in sample reproducibility result from the mechanically precise and consistent application of the analysis procedure, which is difficult to expect of even the most diligent of human operators. The list could be extended further to include factors such as financial benefits and the prospect of undertaking analyses in environments not possible with human operators, such as in special atmospheres or lighting condi- tions. Constraints of Robots The negative features of robotic systems stem from the limitations of the mechanical design and of the computer control. Table 2 lists some potential limitations of robotic solutions.It is an awesome and instructive task to program a robot to undertake the basic operations of a simple exercise. It is analogous to working with your hand in a boxing glove and your head covered with an opaque padded bag! The eyes, ears, and touch of a human operator provide a degree of sensitivity and control that will not be achieved for some years in automation. An application involving a robot has therefore to be engineered to reduce or eliminate dependence on these factors. The dexterity of the human arm and hand is difficult to reproduce mechanically. This can result in mechanisms which occupy a larger working area than would be expected for a human operator. Obviously, solutions to many of these problems can be found in specific instances, but the general solution needs considerable research and development.There are major development programmes in universities and com- panies all over the world in this field. Table 2. Limitations of robots Robot systems lack sensors and intelligence Most general purpose robots require large working areas One malfunction in a complex set-up can disable the entire system Hardware requires specialist back-up Systems operate sequentially yielding a long cycle time Special safety precautions are needed Requirements for Radiochemistry There are many areas of research where radiation measure- ments are required. In some research departments, large numbers of samples can be generated for measurement, using techniques such as liquid scintillation counting. The method is usually well defined and sizes of samples are fixed.It is therefore perfectly feasible to build specific machinery to undertake the measurement and instrument manufacturers areANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 179 producing increasingly sophisticated products to meet the demand. At the Harwell Laboratory, the range of applications is diverse and the number of samples often small and so specific equipment is not always cost effective. Fig. 1. Waters Millilab system [photograph by Millipore (UK) Ltd.] Of the advantages of robotics listed in Table 1, the first entry, that of improving sample throughput, is currently the most significant. Radiation is measured by counting the number of interactions of the emitted species with an approp- riate detector. The details can be obtained from the literature’ and are not relevant here except to note that the accuracy of the measurement is related to the number of events measured.The standard deviation of the measurement is the square root of the number of counts. In most applications, specific activity levels are very low and therefore measurement times are long. It is not unusual to count the radiation from a sample for 10 min and recent measurements at Harwell of samples resulting from the Chernobyl disaster have had to be counted for 4 h in order to obtain a reliable answer. By operating the measurement apparatus outside working hours, the sample throughput can clearly be doubled or tripled if some form of automatic sample changing apparatus can be utilised. Low levels of activity in the sample require that the effects of background radiation are kept as low as possible.Depending on the laboratory, shielding may be required to isolate the detector from natural radiation or from adjacent radiation sources. In an automatic sample changer it is often useful to keep the distance between the sample storage area and the detector as large as possible. Typical shielding may consist of a wall of 4-in thick lead bricks with an automatic door or lid to permit access. The range of movements required by a robot to satisfy these requirements can be extreme. In the past automation has been achieved by specific mechanisms based on slides or carousels. Recently, intermediate solutions have been adopted where a standard robotic arm selects samples from a rack and transfers them to a more specialised transport mechanism to present the sample to the detector for measure- ment.Particular care must be taken to ensure that the packing of the radioactive sample is not damaged. If a vial of liquid were to be broken in the detector by the malfunction of the manipulator, the background radiation level of the detector would be raised. This would reduce the quality of the measurement and could necessitate decontamination of the apparatus. Many radiochemists prefer to use a mechanism which moves samples by sliding them from one position to the next, rather than picking them up. The problem of breakage can be alleviated by adding “touch” sensors to the end effectors of the robots and ensuring the arm remains static in the event of power failure.One requirement when working with elements such as plutonium is that the work can only be undertaken within an enclosure to provide physical containment. The radiological hazard may not be significant. The normal method of containment is to use a glove box which restricts the working volume available and limits access. The overheads associated with a glove box are high and it is usual to make the box serve as many functions as possible. In a situation where there is a range of diverse samples and analyses required, apparatus is moved from the more accessible front parts of the box to the rear if it is not required at that time. Robotics is difficult to apply under these circumstances. A human operator is considered to be the most effective solution at present, for reasons of dexterity and adaptability. Another problem associated with glove boxes is that the access ports are generally small, typically less than 8-in diameter, and once a component has been introduced into the box it becomes contaminated.It may not be feasible or economic to remove and repair it. This then adds further constraints on the size and reliability of the components used in automation. Other practical aspects, such as the necessity for gas-tight bulkhead connectors to allow the transfer of electrical power and signals, need to be considered. Solutions to these requirements are usually available, but they may entail modifications to proprietary equipment. While the previous paragraph suggests that robotics is impractical, there may be circumstances when it may be essential.If samples are being used where there is a chance of a high radiation dose to the operator, then some solution must be adopted to allow work to continue. Permitted levels of radiation are always under review and changes in legislation that called for reduction in dose levels might significantly alter current working practices. The incentive would then be present to find solutions to the problems indicated. It is anticipated that any robotic mechanism would have to be designed into a glove box from the start, as retrospective installation would be considerably more difficult. The methods of implementing robotic solutions are discussed later, but it seems likely that custom designed mechanisms will be more appropriate than standard devices in these instances.Robot-based systems can offer flexibility in two ways. Provided that the physical layout and facilities of the work area have been prepared carefully, it is possible to change the analytical method by loading a new instruction file into the robot control computer. Hardware running one method during the day could easily perform a different analysis overnight. The other aspect of flexibility is that the mechanism can cope with variations in position or sample form: for example, a robot can select test-tubes from any position in a rack. A further illustration can be taken from the nuclear industry, where it is common practice to monitor airborne radiation by sucking a representative volume of air through a filter-paper.Subse- quently, the radiation from particulates deposited on the paper is measured. There is a variety of collection devices available and a range of possible paper sizes. These are often unmounted glass-fibre filter-papers, but increasingly papers are being used which are supported by a cardboard surround. At least three different types of card mounted papers exist. A large establish- ment may have the throughput of samples to justify a mechanism for each type of paper, but a robot-based mechan- ism has the potential to adapt to each type of paper as required and so may reduce equipment requirements. Other instances of variations in sample size have been solved in the past by making a carrier to suit the largest sample and providing inserts to cope with smaller samples.The advantage of a robot gripper1x0 ANALYTICAL PROCEEDINGS. JUNE 1988. VOL 25 with a touch sensor is obvious in such instances, provided that the centre of the sample is placed at the centre of the storage location. However, there are limits to the flexibility of these systems. The measurement of radiation levels in foodstuffs requires large sample sizes as well as long counting times. A human operator can easily manipulate samples ranging from millilitres to litres and tens of grams to one or two kilograms. A robot of this capacity may well need a light industrial system to cope with this variation in range and may not be a realistic solution. Similarly, in other areas at Harwell, the range of activities between batches of samples may vary between bequerels and megabequerels of activity which require variations in technique not readily automated. These analyses are currently handled manually.Towards a Solution Before a robotic solution to an analytical problem is embarked on, it is important to consider two further points. The first is whether the desired analytical result can be achieved by another, simpler, route. Denton2 refers to an example where a wet-chemical method was completely eliminated by the use of a suitable nebuliser on an atomic absorption spectrometer. A degree of lateral thinking can be very worthwhile before a commitment is made. The second point, which is not considered in any detail here, is to consider the justification and resources needed to embark on a programme of robot based instrumentation.The purchase may have to be based on a comprehensive financial case, which would include depreciation and maintenance costs. Personnel resources must also be considered. Robotic systems usually imply some familiarity with computers and, to a lesser extent, electronics and mechanics. Staff who have this background, or are willing to learn it, must be available. The future of any personnel displaced by a robot system must also be considered. Methods of Implementation The implementation stage must commence with a market survey. The scientific instrument manufacturers have usually identified the areas where it is profitable for them to manufacture equipment of specific function. Such equipment usually provides the most economic and effective solution, as no development with be required by the customer.Once the decision to employ robotics has been taken, the constraints of the problem and the local environment can be assessed to form a specification, against which the routes forward can be evaluated. Of major importance are the complexity of the movements required and the space available. The five standard geometries used in robotic systems are Cartesian, cylindrical, polar, anthropomorphic and SCARA. Each arrangement has advantages and disadvantages and are discussed in reference 3 and text-books on the subject of robotics. Other forms, such as long articulated arms or “snake-like” flexible arms, are unlikely to be relevant in the laboratory and have usually been developed for particularly difficult problems, such as reactor core maintenance.For the scientist wishing to automate a method, there are two basic routes forward. A system can be purchased com- pletely from a manufacturer, such as Waters, Zymark or Perkin-Elmer, or it can be developed in-house. In the instance where a system is purchased from a manufacturer, two further classes can be identified: systems using a flexible manipulator and devices incorporating a dedicated motion system serving a fixed operating area. The solution offered by the laboratory robot manufacturers is to offer a flexible manipulator, which is surrounded by a variety of peripherals such as balances, dispensing stations, mixers, etc. These can be specifically designed components, such as those in the Zymark PyTechnology system, which permit rapid system configuration, or any other commercial Fig.2. Elmer Ltd.) Perkin-Elmer Masterlab robot system (photograph by Perkin- product that is capable of being interfaced to the system control computer. A typical system based on the Perkin-Elmer Masterlab system is shown in Fig. 2. The manufacturers can also offer a design, configuration and commissioning service and are constantly improving their products to reduce demands on the user. An alternative packaged approach is to use a product such as the Waters Millilab system or the Gilson Model 212B sample handling system. These products are Cartesian systems of a compact nature and lack the flexibility of a discrete robot system. If this style of device can fulfil the task required, it represents an effective solution as the bulk of the design and programming has already been developed in the basic product and only specific method instructions are required.However, these advantages are soon lost if the device is forced beyond its capabilities and the user attempts in-house “enhancements.” “In-house” developments, where the entire system is de- signed from scratch, should be avoided if at all possible. Such projects are frequently over budget, overdue and incomplete. Once the system is operational, the final stages of tidying up and documentation are rarely completed and there is often an unhealthy dependence on one or two of the scientists who developed the system. This can result in great difficulties maintaining such a system in the future. However, as was indicated earlier, there are occasions when an “in-house” development is the only appropriate solution, such as facilities which operate in a glovebox or involve a harsh environment.Also, in laboratories where radiation is involved, it may not be feasible to allow the manufacturer access to the work area for maintenance or repair. The scientists involved in the analysis will have to undertake this work and the experience gained developing the system will ensure that the maintenance and repair can be undertaken without undue difficulty. The situation is also not quite as bleak as indicated in the previous paragraph, provided that good use of commercial components is made wherever possible. There is a considerable range of actuators and drive systems available on the market from which a manipulator system can be constructed.Several manufacturers offer modular electronic systems, which allow the user to control motors and relays from a standard personal computer. The system designer has the choice of control computer and language system used for programming. Factors in his choice can be to utilise existing expertise and to make use of commercial or private software packages. The programmer can optimise critical parts of his own software rather than decoding and modifying supplied software. Digital and ana- logue inputs from the apparatus can also be simply included. There are sufficient products on the market that an alternative component can be selected if the original module becomes unavailable, especially if this is considered at the time of initial selection.The user can therefore ensure the long-termANALYTICAL PROCEEDINGS. JUNE 1988. VOL 25 181 maintenance and availability of his system. Commercial units, such as shakers and autochangers, should be incorporated if possible to minimise special developments. The bespoke solution ensures that the specification can be fully achieved, or that compromises are dictated by the “customer” not the manufacturer. Conclusions Currently the techniques employed by radiochemists fall into two main groups: those involving large numbers of samples, which can be addressed by special purpose mechanisms, and those which are more efficiently undertaken manually a.t present. The requirements of handling radioactive materials impose certain constraints, which are not easily satisfied by current robot systems.If there is a strong requirement for automatic operation, such as overnight operation or radiation hazard, robotic methods offer an attractive route foward where there are no suitable specific instruments. The success of a robot based analysis system is very dependent on the ingenuity and enthusiasm of the scientist or engineer who is developing the system and the flexibility of the user to accept a novel solution to his automation problem. The number of successful robot installations being reported in recent literature is most encouraging. The author thanks his colleagues in the Chemistry and Environmental and Medical Sciences Divisions at Harwell for sharing their opinions on instrumentation with him.The author’s work in this area is undertaken as part of the Underlying Research programme of the UKAEA. 1. 2. 3. References Wang, C. H., Willis, D. L., and Loveland, W. D., “Radiotracer Methodology in the Biological, Environmental and Physical Sciences,” Prentice-Hall, Englewood Cliffs, NJ, 1975. Denton, M. B., Analyst, 1987, 112, 347. Huddleston, J., 1. Phys. E , 1985, 18, 891. Analytical Applications of Spectroscopy Edited by C.S.Creaser, University of East Anglk and A.M.C. Davies, Institute of Food Research, Nomich This new book provides a ‘State-of-the-Art’ review of the applications of the major spectroscopic techniques and will prove invaluable to researchers involved in this form of analysis. The book provides wide-ranging coverage of recent developments in analytical spectroscopy, and in particular the common themes of chromatography - spectroscopy combinations, Fourier transform methods and data handling techniques. Each section includes a review of key areas of current research, written by spectroscopists who have made major contributions in their respective disciplines, as well as short reports of new developments in these fields. These common themes have played an increasingly important part in recent advances in spectroscopic techniques and emphasise the multidisciplinary approach of present research. 502 pages ISBN 0 85186 383 3 Price $47.50 ($99.00) ROYAL SOCIETY OF CHEMISTRY ~ Information Services To order or for further information, please write to: Royal Sodety of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 IHN, UK, or telephone (0462) 672555 quoting your credit card details. We 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, 30 Russell Square, London WClB 5DT, UK.

ISSN:0144-557X    

DOI:10.1039/AP9882500178

出版商:RSC    

年代:1988

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182 ANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 The COSHH Regulations-the Challenge for the Analyst The following are summaries of five of the papers presented at a Joint Meeting of the Automatic Methods and Special Techniques Groups and the South East Region held on December 10th-I Ith, 1986, in the Scientific Societies Lecture Theatre, London W1. The Proposed Control of Substances Kazardous to Health Regulations: a Practical Approach to Assessment M. F. Curtis Cabinet Office, Civil Service Occupational Health Service, Tilbury House, Petty France, London S WIH 9EU Although the final details of the proposed COSHH Regula- tions are not yet known, we can say with certainty that the regulation dealing with “assessment” will place an obligation on employers to carry out an assessment of the health risk from work activities that are liable to expose people at work to substances hazardous to health.An important part of this assessment will be to decide what systems have to be applied to ensure that exposure is prevented or adequately controlled. In this paper I shall focus on what this really means in practical terms and in the process of so doing I hope to allay some of the fears and misapprehension that seems to be growing about the extent of this particular duty. I have intentionally not said new duty, because although the detail proposed in COSHH is new, I hope and believe that most people are already carrying out a basic assessment in order to comply with the requirements of Section 2 of the Health and Safety at Work Act (HSWA).Some will also be making assessments under the 1980 Lead Regulations. The draft Code of Practice contained in the Consultative Document on COSHH said: “An assessment can be considered adequate when an informed judgement has been made of the risks to health arising from exposure to a substance hazar- dous to health and the means of controlling that risk have been determined. The risk is a function of the nature of the substance and of the nature and degree of exposure. The person carrying out the assessment should be competent for that purpose.” The above statement encapsulates the essential features involved. When it is analysed, it can be broken down into three stages based on the “passwords” of occupational hygiene: recognition, evaluation and control. Assessment is more about the first two of these but an understanding of effective control options is also required.Before going into detail I shall try to bring the subject more into focus by reference to an every-day example. Consider how you would go about safeguarding your own health when using a pesticide in a greenhouse. Most would read the precautionary label and any leaflet supplied. This should determine whether the material is right for the job, the hazards involved and therefore the precautions to be taken. The precautions depend on whether the material is likely to be used as a spray, or simply as a dilute liquid applied by pouring. The protective clothing to be worn would depend on whether the label indicated an inhalation risk or a risk from skin contact; ventilation of the greenhouse will depend on the degree of airborne contamina- tion.One might go through this process almost without thinking, but in fact this is just the sort of process that needs to be gone through in the case of any assessment. Returning to the workplace, an assessment will follow the same pattern. The approach needs to be structured, following a logical sequence of steps if it is to be done properly. Those involved must have the necessary information available to them and those making decisions must be sufficiently well informed to enable valid decisions to be reached. The early stages are likely to benefit from involvement at shop-floor level; later stages may need specialist input except in straight- forward cases. A first practical step is to decide the basis on which to make the assessment-by substance, by process or by work area.A number of factors will determine which is best. Dealing with items one by one may be easier than trying to do it all at once. To discuss assessment in more detail I shall use six steps, as follows. Recognition i. What are the materials, impurities, by-products and other contaminants that need to be considered? Evaluation ii. What hazards do they present-acute, chronic, inhalation, ingestion, skin absorption, corrosives, etc? iii. Identify systems of work, process factors, safeguards or any other factors relevant to any risk. iv. How does the exposure compare with any relevant exposure limits? If no published limit exists, what in-house standard ought to be applied? Control v.What immediate action is needed to correct faults? Will existing controls remain effective? Are on-going checks and monitoring in place? Conclusion vi. Have I now made a confident assessment, sure in the knowledge that relevant facts have been established? Do I need to seek further specialist advice before I can be confident? From the above outline, it can be seen that the requirements of an assessment cover the principles of occupational hygiene. The complexity will vary from one situation to another. In some instances the task will be straightforward, requiring little more than general awareness knowledge. At the other extreme the assessment of a complex process with hazardous materialsANALYTICAL PROCEEDINGS. JUNE 1988, VOL 25 183 will require a substantial input of specialist knowledge. Where a competent hygienist is available he or she may be able to do the bulk of the work with little assistance, but even so it is likely that a useful input can be made by those who actually carry out the process and are aware of problems that arise, e.g., during plant malfunction.In other instances a team approach with an input from in-house specialists and external advisors will be the norm. The important point is not who does the work but whether it can stand up to critical scrutiny. Substances Liable to Present a Risk to Health The most obvious substances to consider are the raw materials. Include any impurities they may contain as these may pose a special risk, e.g. , dioxins in chlorophenols. Identify interme- diates and products.Intermediates must be considered even in closed systems, as exposure may occur during breakdown maintenance. Consider fumes and contaminants liable to be present in the workplace, e.g., thermal degradation products, exhaust fumes from vehicles and unflued heaters or asbestos from sprayed-on insulation. Although there is no legal requirement to prepare a written statement, it will certainly help to make the job much easier and less liable to errors and omissions if it is written down. The next review will also be much easier if records are held. Identifying Hazards Having identified the materials, we must now consider whether they pose any significant hazards. Judgments have to be made on the basis of knowledge and information gathered. There are many sources of data.Obvious sources are the labels on containers and data sheets available from suppliers. Do not forget that the supplier has a duty under Section 6 (HSWA) to give guidance on safety in use. Other sources include text books, journals, advisory leaflets, Guidance Notes from the HSE, manufacturers’ handbooks, trade association data, trade union literature and the experience of specialist staff within the organisation. If these sources are inadequate then specialist advice needs to be sought. Identification of hazards will be incomplete unless consider- ation has been given to both acute and chronic hazards, including the special problems of sensitisation, corrosives and asphyxiants. Inhalation, ingestion and skin contact must be considered. The Process and Systems of Work None of the hazards comes into play until a material is used or exposure occurs.The way in which the work is carried out and the interaction between man and process must be evaluated. If it has not been done before it is necessary now to see the situation and to carry out a detailed walk-through assessment of operational factors. It cannot be properly done from a desk. Consider scale and frequency of use, and whether there is a likelihood of contact with the skin or the generation of airborne contamination. High-risk activities include spray application, hot processes, pressurised systems, confined spaces and all processes that rely on solvent evaporation, as for paints, adhesives, etc. Cleanliness, fugitive emissions, eating and drinking in the workplace are also relevant.On the other side it is necessary to consider the containment systems and protective systems in use, such as fume cupboards, total enclosures, personal protection, respiratory protection and process controls. When all factors are considered it may be found that a “harmful” material used in large amounts presents a more significant risk than a “very toxic” material used in a small amount. Exposure Levels By this stage the number of substances and processes liable to represent a health risk will have been reduced. Assessment of exposure then becomes less onerous. For the purposes of “assessment ,” as opposed to ensuring compliance with occupa- tional exposure limits (OELs), fairly simple tests applied to processes that are liable to give peak/highest levels of personal exposure may be adequate.The assessment is a process in which the potential for health risks and the adequacy of precautionary systems are evaluated. Deciding how to resolve special problems is another matter, but a review of the assessment may be required when this has been done. Carrying out exposure measurements against OELs is a specialist activity and is the most likely part of an assessment to require external assistance. The HSE Guidance Note EHI40 will be a necessary reference source for current UK exposure limits and general guidance on their application. Other Guidance Notes will be helpful for specific substances or processes. A particular pitfall to be avoided in exposure assessment is the variability that may arise from day to day, from one season to another, from batch to batch where ingredients vary and from person to person.If external advisers are used to evaluate exposure it is necessary to ensure that they are competent. Formal qualifications in occupational hygiene, e.g. , BERBOH registration, participation in quality assurance schemes or similar indicators will give a degree of assurance on this point, but there are no specific statutory provisions. Corrective Action It is likely that close scrutiny of work activities for assessment will bring to light improvements that need to be made. These should be put in hand as a separate issue and that part of the “assessment” will need to be reviewed when corrective action is complete. Ongoing Monitoring Some aspects of the assessment will clearly indicate the need for regular monitoring to ensure that conditions do not deteriorate.This point will be covered by specific provisions in COSHH. Again, requirements that are identified should be put in place while they are fresh in the mind. Completion of Assessment Before the assessment can be regarded as complete it is necessary to check back over the whole process to ensure that all aspects have been covered and that the decisions that were made along the way are well founded and, therefore, that there can be confidence in the final outcome. Ideally, an assessment package is written up and signed off by the person responsible for it and a date set for a first review if process changes do not provide an earlier need. Conclusion As indicated earlier, the process of assessment may be carried out by one person or by a team.This will depend very much on the scale and complexity of the work place and the availability of the appropriate expertise. Even if specialist advisers are involved a major contribution can come from shop floor level in a cooperative effort. The main role of specialists may be just to audit what others have done. It is expected that the HSE will publish illustrative guidance on assessments and also on the factors that might need to be taken into account in deciding on the level of competence needed. It is intended that these shall be available by the time the COSHH Regulations come into force.184 ANALYTICAL PROCEEDINGS, JUNE 1988. VOL 25 An Overview of Monitoring Methodologies B. Miller” ICl plc, Mond Division, P.O.Box 8, The Heath, Runcorn, Cheshire WA7 4QD During the past 50 years or so various laws have been introduced to help protect people from exposure to toxic substances and there has been increasing activity in measuring potential exposure. Relevant Acts have been the Factories Act 1961 and the Health and Safety at Work Act 1974. Current official recommendations regarding the highest concentrations of airborne materials to which people should be exposed are listed in the Health and Safety Executive (HSE) Guidance Note EH40/86, “Occupational Exposure Limits.” The COSHH regulations (and proposals from ACTS) are aimed at improving the Health and Safety Commission’s current policy on occupational exposure. Regulations 6 and 10 of COSHH relate to the assessment of risk created by work activities and monitoring exposure at the work place, so a range of monitoring methods will be required to ensure compliance with the Regulations.Gases and Vapours Methods of monitoring gases and vapours can be divided into seven groups, outlined below. The range of instruments and methods discussed is in no way complete as new instruments and methods are becoming available fairly frequently and it is impossible to gain experience of all of them. However, most of the instruments and methods discussed are ones with which the author is familiar. Short-term or spot tests can be made using a variety of methods, including detector tubes, test papers and a range of portable continuous analysers.Samples can also be taken in the field using a range of collection devices such as bags, syringes, diffusion bottles, bubblers/impingers, evacuated flasks, gas burettes and solid adsorbents and returned to the laboratory for analysis by, for example, spectrophotometric methods, gas chromatography, infrared analysis or high- performance liquid chromatography. Continuous or rapid repetitive measurements can be made using a range of instruments such as paper-tape analysers, infrared analysers, ultraviolet analysers, photoionisation analysers and portable gas chromatographs. Personal monitors provide the best means of measuring the air that a person breathes and can generally be divided into three groups: (a) commercially available instruments; (b) active or pumped systems based on adsorption or colour production; and (c) diffusive systems based on adsorption or colour production.* Present address: 22 Ashbourne Avenue, Runcorn, Cheshire WA7 4YD. Leak seekers are used for looking for small leaks on pipelines, etc., and typical devices include detector tubes and the range of portable instruments already mentioned in 2. Fixed installations which usually take the form of multi- point monitoring systems must be tailored to meet the measurement geography of a particular plant or area. They are expensive, will generate a lot of data and can be operated using instruments such as paper tapes, gas chromatographs, infrared or ultraviolet spectrometers and mass spectrometers. Biological methods, which are being increasingly used to compare dose to exposure (using personal monitors), include urine, blood and breath analysis.Emission monitors are usually used to measure levels in stacks or plumes with techniques such as infrared, electro- chemical, gas chromatography and UV analysers. A fav- oured, but expensive, method is to monitor the plume using a laser-based technique. Dusts and Fumes Generally personal sampling is carried out using gravimetric methods (MDHS 14) and a range of pumps, filters, holders and cyclones. The system used will depend on the measurement, ie., total or respirable, mass only or mass and analysis for individual components. An instrument, the Miniram, now available for personal monitoring of total dust based on the light-scattering principle, gives a direct readout of concentration, time elapsed, TWA concentration and shift average.The PDS-1 personal dust sensor, also based on light scattering, has a built-in alarm, continuous display and can be linked to a dosimetry system to give time - concentration profiles. There are several direct-reading instruments available for dust such as the Simslin, again based on light scattering, which measures respirable dust giving a direct readout, an over-all TWA concentration and, via a memory unit, a time - concen- tration profile. Also available is the PCD-1 Sibata respirable dust monitor, which is microprocessor based, thus allowing the user to adapt the instrument to a particular monitoring application. All instruments need to be calibrated for measurement of a particular dust and it is desirable for the particle size range to be known.Industrial Hygiene Programme at an American Army Medical Centre in West Germany Mark B. Geiger US Army Second General Hospital, 6790 Landstuhl-Pfalz, FRG Background Logistics and Geography American Army in Europe. Its geographical location makes the area one of the crucial European centres for military The Second General Hospital in Landstuhl, West Germany, is the largest of ten regional medical centres supporting the supply, transport, depot level maintenance, medical support and billeting of reserve forces.ANALYTICAL PROCEEDINGS. JUNE 1988, VOL 25 185 Table 1. Key operations and exposures Type of operation Embalming . . . . . . . . Ethylene oxide steriliser . . . . Cast room . . . . . . . . . . Radioisotopework .. . . . . Aviationmaintenance . . . . Optical shops . . . . . . . . Pesticide work . . . . . . . . Air conditioning and refrigeration Metal treating . . . . . . . . Chemical analysis and preparation Paint booth . . . . . . . . Dentallaboratory . . . . . . Carpentry shop . . . . . . . . Pathological and biological work . . Welding shops . . . . . . . . Ordnance . . . . . . . . . . Electrical shoDs . . . . . . . . X-rayandfilmprocessing . . . . Shippingheceiving . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Vehicle maintenance (above unit level) Unitvehiclemaintenance . . . . . Small-arms repair . . . . . . . Total . . . . . . . . . * See Table 2. Estimated Key work task exposure* No. LOHHI no. of personnel . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Formaldehyde ETO, N N, D R N, P, s N, s Pesticides W (Cd ?), S (Freon) S, Apr, N, acid, caustic S (limited), acid Rad, possible sensitisers p, Apr, N Hg, N N, D Bio N, CO w, Apr N, P, Apr, A , S N, Ph W, P, S (limit), CO N, CO s, N 1 1 1 1 3 4 4 6 8 8 8 10 11 14 18 21 26 27 31 125 264 - 10 592 5 8 5 150 88 52 27 34 80 80 37 100 14 200 96 292 181 216 395 677 1431 96 4336 General scope - 5 major military communities - 118 separate installations - Military and civilian worker population approximately - 60000 square mile area 100 000 Core areas of concern 8000 persons in 800 work locations Depot level maintenance of vehicles, equipment, ammunition Facilities maintenance and construction activities Medical and laboratory operations Preliminary Survey and Analysis An initial industrial hygiene inventory of hazardous work locations within the Army facilities in Europe was completed by military environmental health technicians with limited specialised training during 1982 to 1984.The effort required six man years in the Landstuhl area alone and documented a total of 592 work places. (“Non-hazardous” locations such as administrative areas were not evaluated.) The data were coded and transcribed for central computer analysis but were not readily usable at the local level at the initial stages. Subsequent inventories and evaluations have indicated significant undercounting and widespread scatter in individual worksite evaluations but have not altered the general conclu- sions derived from review of this data.Results of Preliminary Industrial Hygiene Survey Key operations and exposures are given in Table 1, and key work tasks and exposures with the number of personnel exposed in Table 2. Conclusions from Review of Initial Data A review of the initial inventory data and limited on-site evaluation by an experienced hygienist provided the following conclusions: 1. 2. 3. 4. 5. 6. High numbers of similar shops and work operations. Few locations appeared complex, exotic or individually differ- ent to evaluate. Most exposures could be further categorised into a limited number of common operations and related processes (see Table 3). The inventory of hazards was relatively complete but did not indicate the degree of risk of frequency of exposure. Where special evaluations had been conducted significant exposures were often documented.A high proportion of work places lacked effective control measures with major deficiencies in ventilation, protec- tive equipment (especially respirators) and worker train- ing. More frequent and prolonged exposures to given physical and chemical agents were sustained by specialised work- ers at higher level maintenance facilities, typically local nationals. Table 2. Key work tasks/exposures and number of personnel exposed N=noise . . . . . . . . . . . . . . . . . . 3436 W = welding (primary weld shop + vehicle maintenance shop) . . . . . . . . . . 400 S = solvent cleaning (except acetone) . . . . . . . . 658 CO = carbon monoxide . . . . . . . .. . . . 2400 Apr = abrasive paint removal, lead, chromium, noise . . . . . . . . . . 577 P = paint (chrome lead solvents) . . . . . . . . . . 404 Bio = biological hazards . . . . . . . . . . . . 96 D = low-toxicity dust (TLVS1 mgm-’) . . . . . . 200 Rad = ionising radiation . . . . . . . . . . . . 150 A = acetone . . . . . . . . . . . . . . . . 152 Hg . . . . . . . . . . . . . . . . . . . . 14 Woodworking . . . . . . . . . . . . . . . . 200 ETO = ethylene oxide . . . . . . . . . . . . . . Formaldehyde . . . . . . . . . . . . . . . . 5-10 80186 ANALYTICAL PROCEEDINGS, JUNE 1988. VOL 25 Table 3. Key hazardous operations in Landstuhl Army Regional Medical Centre determined from local occupational health hazard inventory L .c c 0.05 0.03 a, C E! 0.01 -0 m 3 0.005 Type of operation Spray painting - US OSHA lead standard - 0 0.US OSHA action level lead exposure 0 - o# 0 - 0 Welding/brazing : SMAW (stick) on mild steel (E6013 electrode) MIG (wire-fed gun) on A1 (A1 wire, Ar shield gas) Torch brazing on copper and steel (rods vary) Torch cutting (often on painted surfaces) Abrasive paint removal Solvent cleaning (excluding acetone) Acetone cleaning Carbon monoxide (from vehicle operation) Woodworking Surgery Anaesthesia equipment calibration/maintenance Principle exposures Metals: Pb, Cr, Mo, Zn. Various solvents. Noise (paint booth and adjacent operations) 03, Mn, Fe, welding fumes not otherwise classified, noise 03, Al, fumes not otherwise classified, NO2, noise NO2, Ag, Cu, Ph, Zn, Sn, Cd (?) Pb, Cr, NO2, Zn Pb, Cr, noise, Zn, Mo Chlorinated and aliphatic hydrocarbons HC (PD-680, Stoddard solvent), noise, some aromatic hydrocarbons Acetone , noise, paint pigments (Ph, Cr, Mo) CO, noise, NO,, aldehydes Noise, wood dust (oak, pine) Anaesthetic gases (nitrous oxide) (halogenated agents) Biological hazards Remarks Estimated personnel exposed Most operations 404 (principal job) involved camouflage paints containing lead and chromium pigments 406 (principal job) Limited number of abrasive 577 blasters but many locations grinding paint with pneumatic sanders Listing only for those who have this as major job element 687 Mostly at Meisau Ordnance workers 292 warehouse workers, 677 vehicle paint (above unit level), 1431 motor pool Good ventilation control in main hospital operating suites Typically poor ventilation and high exposures in eight dental, veterinary and special procedures areas (22 surgical locations) 152 2400 (1986 estimated to be “unprotected”) 200 100 100 50 30 20 10 5 2.5 D E 0 .- +- F E 1.0 a, 0.50 - co a, ” 0.15 > a, I 2 0.1 0.05 0.03 0.01 0.005 L L L C LL LL c LLL c CCC C CC LL LtFc German lead standard c c (0.15 mg/m3) US OSHA lead standard (0.05 rng/m3) US ACGIH TLV for Or VI L L L c L C L L cc US OSHA action level for C L lead exposure L 2 51016305070 84 909598 Percentage of measurements less than indicated value Fig.1. paint removal Lead (L) and chromium (C) exposures generated in abrasive Analysis The number of detailed work-place evaluations required by regulations and good practice far exceeded available staff resources (two or three persons).Additional limited evalua- tions in a broad number of work areas would have been of limited value. Measurements of exposures in a relatively circumscribed number of work places with use of statistical evaluation to project (estimate) exposures of larger popula- tions was indicated. 0.5 t 0 German lead standard 0 0 0 2 510163050 70 909598 Percentage of measurements less than indicated value Lead exposures in general repair welding operations 0.001 Fig. 2.ANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 L LL 187 0 I , , , I , I , , , 10 m t 0 0 m .- w I Percentage of measurements less than indicated value Fig. 3. Solvent exposure from spray painting Prioritisation and Action for Work Place Process Evaluation Evaluations are prioritised on the basis of the following: (1) regulatory requirements (example codes relates to noise and lead exposures; (2) estimated severity of the health effect using standard risk assessment code; (3) frequency/extent of ex- posures to this specific agent/process of concern; and (4) extent of cooperation provided by the unit being served in assisting and implement corrective action. Details are given in Table 4.1 .o 0 5 0.1 m 0.05 E 0.03 ? ?? O.O1 r” c. C ! 0.005 m 0.001 0.0005 OSHAlead c“hc standard c l L OSHA action 1 level for lead LL /LL 1-c / I LY CLL L c, ccc L c c c/ L L L / / 1 1 1 , I I I I , , , 2 5 101630 507084909598 Percentage of measurements less than indicated value Fig. 4. painting Lead (L) and chromium (C) exposures generated in spray Statistical Evaluation of Key Exposures Environmental samples show a wide dispersion that can be “normalised” toward a gaussian distribution by using the logarithm of concentration.The frequency curve can be linearised by plotting the logarithm of the cumulative percen- tage against logarithm of concentration. Examples are shown in Figs. 1-4. Using guidelines of the National Institute for Occupational Safety and Health (NIOSH), estimates of population ex- posures may be made from limited numbers of data points. Table 4. Prioritisation for work place evaluation Agents Primary exposures Regulatory requirements Initial findings and actions Noise . . . . . . . . 400+ work locations, OSHA hearing conservation 1. Many units lack effective most “industrial” workers amendment. programmes. exposed Army guidelines require 2.Extensive training programmes protective equipment. Training medical monitoring for 85 dBA implemented by health nurses. 3. Rapid survey report format used. Lead . . . . . . Chromium(V1) . . . . Waste anaesthetic gases . . Primarily related to painting, grinding and welding with and around lead-based paints. 577 “grinders” (mostly welders or painters, ca. 400 welders, ca. 400 painters) Similar to lead as constituent of pigments (lead chromates and zinc chromate) in paint. Very limited stainless steel welding 100 exposed in 22 surgical, dental and veterinary operating suites OSHA lead standard (0.05 mg m-3) 1. Statistical sampling of those operations with most significant potential exposures (welding, painting and grinding). 2.Uniform technical guidelines for 1 control measures developed for abrasive paint removal and ventilation of welding operations. 3. Engineering study of major painting operations conducted and guidance for corrective action provided. Army regulations (treated as suspect carcinogen) (TLV 0.05 mg m-3) Similar to lead (above). Army regulations Ongoing evaluations (required quarterly) find significant lack of ventilation controls and related high exposures in many clinics. Efforts focused on providing a report for action to the medical centre Commander. Detailed technical consultation provided.188 ANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 Table 5. Summary of key occupational exposures. US OSHA Lead Standard. Chromium calculated as chromium(V1) contained in lead chromate and zinc chromate paint pigments.ACGIH TLV (for 1985-86) is 0.05 mg m-3. Calculated fraction of allowable exposure to mixed solvents using criteria of ACGIH TLV for 1985-86 Process Occupational exposure Geometric Standard Contaminant n criteria/mg m-3 mean/mg m--3 deviatiodmg m-3 Abrasive paint removal (pneumatic sanding) . . Lead Chrome 30 0.05 1.14 0.94 30 0.05 0.345 2.61 Spray painting . . . . . . . . . . . . Lead 21 0.05 0.013 0.137 Chrome 21 0.05 0.010 0.31 Mixed solvents 28 1.0 0.15 0.45 General repair welding adhesive application . . Lead 20 0.05 0.032 Mixed solvents 11 1 .0 0.20 0.46 This technique has been applied to estimate the (geometric) mean and standard deviation exposure of persons conducting key common hazardous operations. A summary of key occupational exposures is given in Table 5.Conclusions A review of preliminary survey data indicated that a high proportion of chemical exposures generated within US Army work places in Germany could be attributed to a limited number of key processes and operations. Data obtained in evaluations of these operations were combined to develop estimates of personnel exposures. Standard formats for data collection, reporting and uniform guidance for corrective action were developed concurrently. The most significant common exposures were found to be heavy metals in abrasive paint removal, followed by metal exposures in mixed welding and spray painting. Review of Atmosphere Analysis in the Process Industries J. R. P. Clarke ICI Engineering Department, Winnington, Northwich, Cheshire Industry’s aim is to maximise profit; this aim is counter- balanced by the need to act within socially acceptable or legally enforceable limits.A successful, responsible approach to the processing of materials has sound process engineering and careful operation as the basic means of preventing leakage of noxious materials. Careful analytical monitoring of legitimate ducts and the surrounding area is an additional major feature. Vent Monitors UK legislation has tended to favour chemical analysis at legitimate exit points such as vents or stacks. Sampling problems often make it difficult to obtain measurements that are representative of the analyte in an enclosed vent ,1 but this is easier than monitoring for leakages that may occur anywhere across the plant area.A large number of analytical methods are continually under development and a good knowledge of the operating condi- tions and all chemical species or debris is essential to ensure that the systems can be adequately designed. As each application usually has several possible analytical methods, each with its own sampling requirements, plant managers or designers would be prudent to consult specialists. Plant Area Monitoring It can generally be argued that if industrial hygiene, local to a plant, is well maintained, then the exposure to neighbours outside the boundary fence will be at a lower level. Apart from cases of extreme immediate hazard, where it may be necessary to box-in a whole area, it is increasingly common to place gas monitors or sampling points across a plant site according to the probability of a leak and human presence at a particular place and the direction of the prevailing wind.An array of pumped or diffusively operated traps or “long-term” Draeger tubes can be a useful initial survey procedure. Variations in the general direction of air movements make it impossible for fixed-point area monitors to guarantee an instantaneous response to any unplanned vapour emission and normal local air turbulances give very rapid variations in the concentrations even directly downwind of a steady release of vapour. Several strategies may be used to pipe samples to a central analyser: 1. A fixed sampling pattern; only lines about to be sampled and actually being examined are pumped at any one time.2. Several (n) independent lines may be sampled at once (this dilutes the gaseous effluent in any one line up to n-fold). An intelligent system, having noted an emission, will assess groups of sample lines to home-in on the offending area. 3. Biasing sampling to be downstream of the current wind direction reduces the mean time before leak detection. 4. A parallel cluster of centrally placed traps enhances the analyser’s sensitivity and uses the time when a sample line is not being directly examined-method 1. 5. Several ( n ) tubes feeding one trap overcome diluting a positive result by up to n-fold-method 2. It is essential to make practical trials to assess the effects of polar samples being “lost,” even with optimum materials and tube construction. Even though all sample lines give some smoothing to naturally occurring concentration pulses, there is a good chance that the instantaneous snap action of a conventional process gas chromatograph sampling valve will not obtain a fair representation of the mean effluent concentra- tion.The modern mass spectrometer, with continuous operation, high speed of response, sensitivity and selectivity, is increas- ingly replacing the gas chromatograph for monitoring organic vapours. Similar comments, in principle, apply to spectropho- tometers, but large sample cells give a concentration smooth- ing, so reducing effective sensitivity and speed of response. Sample timing problems apart, a photoacoustic spectrometer which periodically seals a small sample cell by means of a pairANALYTICAL PROCEEDINGS.JUNE 1988, VOL 25 189 of valves, would be a sensitive alternative to conventional spectrophotometers. Integrating Systems Some analysers, perhaps akin to the mechanisms in physiology, trap the signal over a period of time. The analytical chemist has developed thousands of colour tests. The application of these on tapes or packing, with flowing streams of reagents or to fibre-optic probes, opens up many possibilities. The develop- ment of UV chromophores offers further opportunities with automated viewing. Hirschfeld2 claimed to have developed 24 types of fibre-optic sensors based on fluorescent reagents. The principle of entrapment could generally be applied to conventional process analysers and has been well established for the automated desorption of personal diffusive sampling tubes into gas chromatographs. The criteria for traps for higher boiling materials could be met by the use of commercially available quartz wide-bore (0.53 mm) capilliaries.Infrared Flammable Gas Sensors “Sampling in a line” can be achieved most simply by using a detector remote from the infrared source, but mirror systems allow source and detector to be mounted adjacent to each other. More sophisticated steerable laser systems3 can monitor flammable levels of hydrocarbons by reflecting radiation from normal plant items or p.p.m. levels of other vapours using retro-reflectors. Alternative systems have demonstrated p.p. b. measurements at kilometre ranges.4 All these systems use a reference beam to compensate for absorption by dust, rain or changes in the reflectivity.Leak Seeking The chance of a major leak going undetected is small. This may not be the case for minor leaks likely from a gland or flange, even when a point area monitoring system has been installed. Given favourable air currents, area monitors are still unlikely to be able to pin-point the precise position of an emission. This needs sensitive, rapidly responding, portable, leak-seeking equipment to nose down to the source of the vapour plume. Such equipment must never constitute an electrical hazard in the presence of flammable vapours and will often need to be certified as intrinsically safe. Even without an area monitoring array, the regular applica- tion of leak-seeking equipment to joint seals allows manage- ment to monitor minor emissions and maintain a sound plant.Portable hydrogen flame-ionisation detectors, shielded behind a flame trap, are generally suitable for tracing organic vapours. Interference from naturally occurring methane may be overcome by use of a UV photoionisation leak seeker. Katharometers, lacking great sensitivity, may be used to pin-point leaks at very close range. Although slower in response, portable infrared equipment responds to volatile dipolar molecules. Electron-capture seekers are sensitive to most halocarbons, and UV detectors, developed for mercury, also respond to aromatic hydrocarbons. Electrochemical sen- sors will continue to give good value in seeking inorganic vapours. There should be no insuperable problems to the develop- ment of a hand-held quadrupole mass spectrometer.Avoiding the vacuum necessary for a true mass spectrometer, Graseby Dynamics have developed security systems based on differ- ences in ion mobility between charged electrodes when opposed by a steady air current. Personal Monitors The human nose has evolved to give warning of poor-quality food. Ideally sited as a sampling device, it is by no means useless for detecting many toxic vapours.5 The senses of sight and hearing should not be ignored in the context of gaseous emissions, especially when used with intelligence. The principle of combining the ratio of responses from a series of sensors is the principle on which the nose, and all other human sensors, have been evolved. Following some success with a pair of otherwise fairly unselective Taguchi solid-state sensors, Persaud and Dodds are trying to mimic the human nose.As any change in the breathable atmosphere is usually bad for humans, selectivity is not necessarily of overwhelming importance, whereas reliability and consistent performance are critical factors. Hence, one may be content with sensors that respond to class types rather than to individual chemicals, for example, with “chlorine” sensors which respond to oxidants. Worn close to the breathing zone and not conveniently out of the way, as with portable or fixed-array transducers, personal monitors are nearly ideal sampling systems. However, these monitors must be convenient or they will often be used incorrectly or even wilfully damaged. The psychology of their application and the release of their analytical results needs careful consideration for each situation. A monitor’s size/mass factors are greatly dependent on the intrinsically safe batteries needed to operate throughout a shift, for example, in personal sampling pumps used to trap toxic vapours for subsequent laboratory analysis.’ Colour chemistry has now been married to these personal sampling pumps by means of the long-term Draeger tube.The need for a robust case and energy requirements thwarted an automated personal paper tape analyser. A 1.1-kg prototype ended up as the 2-kg portable, unwearable, Draeger Toxiwarn system, despite a low-energy system of impacting rather than, as is normal, sucking sample through the tape thickness.* The problem of wearer acceptability becomes acute where multiple hazards exist, for example, in drains.The development of combined instrumentation for oxygen deficiency, hydrogen sulphide and flammable gas detection is a step forward for the water industry. The severe limits on the analytical techniques that can be incorporated into a personal monitor are frequently avoided by using traps, followed by laboratory assessment,g e . g . , as in the Perkin-Elmer ATD-50 system of tubular traps. Worn for a shift, these are automatically thermally desorbed into a laboratory gas chromatograph. Many successful personal monitors use naturally occurring gaseous diffusion to bring the sample to the analyser, followed by transducers with low energy requirements. Compur sensors rely on diffusion and electrochemical principles and a small battery to initiate an audible alarm.With less ergonomic convenience, this system may be worn with a microprocessor to record the transducer’s output. On playback, the shift time- weighted average concentration may be assessed. Non-toxic asphixiant gases such as nitrogen may also be guarded against by means of diffusively sampling, electrochemical oxygen deficiency monitors. Some diffusive traps or badges generate coloured stains. One may look forward to energy-efficient, automated viewing and alarm systems. Much work has been carried out on piezoelectric sensors.1() The absorption of mercury vapour by a gold layer is a felicitious example as it does not share the problem common to most other piezoelectric systems of the absorption of water vapour from an atmosphere of varying humidity.The answer to this may lie either in differential measurements to gain selectivity, or in the removal of water vapour by a suitable membrane sampling technique. Portable Monitors It is not possible to provide wearable monitors for every application but portable equipment placed close to the worker still offers additional protection. Conversely, personal moni- tors may be of value as portable equipment, for example, by the insertion of an oxygen deficiency monitor into a vessel prior to entry. Placing of portable equipment relative to a potential leak190 and to the worker may often be far from improved sampling and wind direction certainly enhance staff‘s protection. optimal. Training, monitoring would Biological Monitoring Healthy communities of plants, animals or microorganisms are indicative of good living conditions, so the monitoring of naturally occurring biological specimens can provide evidence of the long-term environmental impact of a plant.Following this argument led to monitoring the traditional canary or other biological material to sense or trap possible effluents. Conclusion The future will call for enhancements in the miniaturisation, precision, speed, selectivity, convenience, reliability and lower cost of effluent measurements. The application of sampling systems and the use of microcomputers should transform what are often relatively useless transducers into viable measure- ment systems trusted by their owners. In-house development can never meet more than a fraction of a company’s needs, so it is vital that contacts are maintained ANALYTICAL PROCEEDINGS, JUNE 1988.VOL 25 with academic and government laboratories, instrument sup- pliers and brother users. 1. 2. 3. 4. 5 . 6. 7. 8. 9. 10. References Cornish, D. C., Jepson, G., and Smurthwaite, M. J . , “Sam- pling Systems for Process Analysers,” Butterworths, London, 1981. Hirschfeld, T., paper presented at Anatech 86, International Symposium on Applications of Analytical Chemical Tech- niques to Industrial Process Control, Noordwij kerhout, 22-24 April 1986. Cramp, J. H. W., Eur. Pat., 59 593, 1981. Krigman, A., Zntech, 1985, 32 (12), 9. Amoore, J. E., and Hautala, E., J. Appl. Toxicol., 1983, 3, 272. Persaud, K., and Dodd, G. , Nature (London), 1982,299,352.Wagg, R. M., Coker, D. T., Clarke, J. R. P., Lee, G., Leinster, P., Miller, B., and Piney, M., in Ogden, T. L., Editor, “The Selection and Use of Personal Sampling Pumps,” British Occupational Hygiene Society, Technical Guide No. 5 , Science Reviews, Northwood, 1985. Clarke, J. R. P., and Tortoishell, G., Br. Pat., 1 496 684,197.5. Melcher, R. G., and Langhorst, M. L., Anal. Chem., 1985,57, 238R. Alder, J. F., and McCallum, J. J., Analyst, 1983, 108, 1169. Sensitive Portable Gas Chromatograph with Data Retrieval and Communications Capability for Remote Surveillance of Toxic Gases and Vapours in Plant Martin Adams Centronic Sales Ltd., Cro ydon, Surrey Mark Collins Photovac Inc., Ontario, Canada Many industries use highly toxic gases and solvents in process operations and severe health implications including blood disorders, cytogenetic damage and various forms of cancer have been associated with inhalation of these chemicals in occupational situations.The new COSHH regulations will call for regular monitoring of these vapours with very strict limits being imposed for exposure levels. The ability of conventional instrumentation to measure these substances, often to low parts per billion levels, is limited by lack of sensitivity or selectivity, resulting in the need for slow and cumbersome pre-concentration techniques. Field portable instrumentation must be capable of multi- component analysis, giving a high degree of sensitivity under varying conditions of field use. The possibility of misidentifica- tion must be minimised.The instrument must be fully self-contained and perform self-calibration during unattended operation. All these performance capabilities are incorporated in the Photovac 10s series of photoionisation gas chromato- graphs described here. Instrument Features The photoionisation detector can operate at room temperature using air as the carrier gas, and it exhibits unprecedented sensitivity to a large number of gases and solvent vapours (benzene can be measured at levels below 0.1 p.p.b. in air). The carrier gas is contained in an easily refilled internal tank; power is provided by a series of internal re-chargeable batteries. The entire system is contained in a briefcase-sized aluminium case weighing about 20 kg. There are several models available; the 10S70 communications model will be described in detail.An internal pump draws in sample through a loop and hence on to two columns in series. The columns are housed in an insulated enclosure. The 10S70 computer compensates for base-line drift, and a built-in source gives regular calibration. The columns are in series for about 40 s, then the configuration changes to the back-flush mode to prevent contamination of the analytical column by heavier materials. All these operations occur automatically by using six PTFE electrically operated miniature valves. Data Handling The 10S70 computer incorporates its own four-colour printer - plotter and 32-character alphanumeric keyboard with liquid crystal display. There are four library files, each capable of storing up to 25 components by name.When the pie-deter- mined threshold value is exceeded an alarm will sound, and the result is printed in red. The calendar and 24-h clock will indicate the precise time of an incident. The computer can provide time-weighted averages (TWA) and maximum con- centrations. An RS232 interface is provided, which can be connected to a remote terminal or specially programmed computer. All functions that can be performed on the keyboard can also be performed on a remote terminal or computer. A modem is also available, which can be used on internal telephone systems. Applications The photoionisation detector used in this instrument is able to detect most organic vapours and various other hazardous substances such as hydrogen sulphide, arsine and phosphine.As indicated before, the 10s system can identify individual compounds, calculate the threshold levels and indicate TWA and maximum concentrations during a pre-determined period. The new COSHH proposals call for this measurement to be carried out on a number of substances in Groups 1 and 2. AllANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 191 the organic vapours and carbon sulphide in Group 1 can be measured at levels well below the stated exposure levels and in Table 1. Minimum detectable levels and exposure levels Maximum exposure limit, Compound MDL, p.p.m. p.p.m. Acrylonitrile . . . . . . Ethyleneoxide . . . . . . Carbondisulphide . . . . Formaldehyde . . . . . . Dichloromethane . . . . . . Ethyleneglycol . . . . . . Styrene . . . . . . . . 2-Ethyl methoxyacetate .. Trichloroethane . . . . . . Trichloroethylene . . . . Vinylidinechloride . . . . Vinyl chloride monomer . . 0.25 0.01 0.01 1 0.1 0.05 0.01 0.05 0.01 0.01 0.001 0.001 2 5 10 2 100 5 100 5 350 100 10 3 some instances with a minimum detectable level (MDL) of less than one hundredth of current exposure levels. The limits of detection and exposure levels of each of the compounds are given in Table 1. Other key applications for the 10s series are benzene, toluene and hydrogen sulphide (all to 0.001 p.p.m.), arsine, phosphine and ethylene (to below 0.005 p.p.m.) and a wide variety of organic solvents such as aldehydes, ketones, ethers, acetates and chlorinated and unsaturated hydrocarbons to well below the parts per million level. Conclusion The 10S70, with its capability to communicate and be remotely controlled, leads to considerable time savings for the industrial hygienist. This instrument is an important tool for the analyst whose workload will be increased significantly by the new COSHH regulations. 1 An Introduction to Applications of Light Microscopy in Analysis i I By D. Simpson and W.D. Simpson, Analysis for Indusfry, Thorp-le-Soken Light Microscopy is one of the oldest techniques at the disposal of the analyst and is unfortunately greatly undervalued and underused in the analytical laboratory. It is, in fact, a conventional economical technique which should not be overlooked and can be of great value in the analysis of foods, pharmaceuticals, metals, plastics, water, agrochemicals, textiles and much more. In this book the authors draw upon their considerable experience in industry and consulting practice, to provide examples of the many and varied uses of light microscopy in analysis. They describe in detail its capabilities and seek to encourage its wider use in actual practice, reminding analysts of its qualities and applications. They also advocate good practice in its use. Microscopists, analysts and students alike will gain much from the authors’ enthusiasm and as a result may assist in extending the utility of the instrument into the future. Due Summer 1988 Price g29.50 ($63.00) ISBN 0 85186 987 4. Hardcover approx. 200pp ROYAL SOCIETY OF CHEMISTRY ~~ information Services To order or for further information, please write to: Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 IHN, UK,or telephone (0462) 672555 quoting your credit card details. We now accept Access/Visa/MasterCard/EuroCard. RSC Members are entitled to a discount on most RSCpublications and should write to: Membership Manager, Royal Society of Chemistry, 30 Russell Square, London WClB 5DT, UK.

ISSN:0144-557X    

DOI:10.1039/AP9882500182

出版商:RSC    

年代:1988

数据来源: RSC

摘要:

192 ANALYTICAL PROCEEDINGS. JUNE 1988. VOL 25 Quality Assurance: Information and Its Impact on Quality The following are summaries of five of the papers presented at a Meeting of the Automatic Methods Group held on May 5th-6th, 1987, in the De Vere Hotel, Coventry. Quality Assurance in the Environment L. R. Pittwell Department of the Environment, Romney House, 43 Marsham Street, London SWlP 3PY This paper discusses the quality of analyses used to monitor and control the environment. The problems analysts face are world-wide; governments have been concerned about the quality of the environment for a very long time, prompted, of course, by the regard people have for their own well being. The 1898 Royal Commission on Sewage Disposal found discrepancies in their data and set up a committee to investigate the accuracy of the analytical methods used. They issued a series of recommended methods.The committee’s successors continue to this day. In the 1960s, there was a need to determine the loads of various substances carried to the sea by British rivers. Unfortunately, there were discrepencies in analysis even for chloride. To improve the quality of analysis, the Department started the Harmonised Monitoring Analytical Quality Control project, operated by the Water Research Centre. Samples were circulated and analysed by various laboratories. Problems were discovered and solved by those taking part. The findings have been published in The Analyst. The WRC Aquacheck project continues this effort. There are far too many possible substances for it to cover every determinand.A similar scheme is being developed by the Public Health Laboratory Service for microbial analysis, which is open to Water Authority participa- tion. The Standing Committee of Analysts was set up by the Secretary of State in 1972 to issue recommended tested methods for monitoring the quality of water, sewage and associated land and sediments. These methods, which are examined and selected by interested experts in the various fields, drawn from the water industry, from universities, public analysts, and all other interested bodies, always include performance characteristics and test data. The Nature Conservancy Council has estimated the number of different unpolluted river types in Great Britain to be 56. To these must be added marine and groundwaters, effluents and the associated materials that affect water or are affected by sewage disposal.Because of the variety of samples, the variations in work load and the mix of samples dealt with, it has been found necessary to recommend more than one method per determi- nand, to include variations and issue reviews of special techniques. Although some determinands remain to be covered, work has started on the revision of the earlier booklets and additional booklets on multi-determinand tech- niques. Over 100 booklets have been issued. As one of the charges to the Standing Committee of Analysts is to keep the compendium up to date, work continues. The ever changing pesticide market and parameters such as Kjeldahl nitrogen, complexed cyanide and total sulphur create analytical difficul- ties requiring new methods.In the past the accuracy of a method has been the prime concern. However, in these days when there are many calls on available money, and the number of samples is increasing, although accuracy of analysis is important it is not the only criterion necessary for a satisfactory analysis and a satisfied customer. A single figure result is of more value if supplied before the water has been drunk or the food eaten than a result with several-figure accuracy that arrives too late. Speed is important, and cost, equipment availability and efficient laboratory operation need to be considered. When searching for an accurate and efficient analytical procedure one should investigate possible methods, equipment used, reagent purity, staff competence, materials and sample reliability.It is impossible to study these in isolation. This means studying the performance characteristics of the method under various conditions. The nomenclature of performance characteristics varies, but the fundamental concepts remain the same: Limit of detection or criterion of detection is that concentra- tion at which there is certainty that the determinand is present even if it cannot be quantified. Limit of quantification , sometimes called limit of detection , is that concentration at which the determinand can be quantified to a given accuracy with an agreed degree of confidence. Repeatability or precision is the ability to repeat the results regardless of accuracy. Accuracy or trueness is a measure of the ability to determine what the truth really is.Bias is used in some countries as a synonym for total error, but in English bias means a tendency to go to one side (and there is a need for such a term). Systematic error is probably a better term. Standard deviation is a measure of the repeatability of results. There are several varieties. Relative standard deviation is most useful; it relates the variability to the range. Degrees offreedom is a measure of how thoroughly a method has been tested. The larger the number, the more testing has been done; however, the concept becomes difficult to handle when many laboratories test a method. It becomes simpler just to tabulate what was done. When evaluating a method, there are many snags for the unwary.Interference effects are among the commonest. When an analytical technique appears it is often lauded as being interference free. Problems appear later. Some of the latest methods are highly instrument dependent; some of the recent methods issued by the SCA, whilst giving the customary typical test data, warn users to check the method and interference effects with their own equipment before using it. Band spectra, overlapping lines and matrix effects areANALYTICAL PROCEEDINGS, JUNE 1988. VOL 25 193 becoming as much a problem in EAAS and ICP-AES as they were with emission spectroscopy. Similar problems plague chromatography, as the concentration of ions in a sample can shift peaks and peaks of different substances overlap. These problems are often solvable by change in eluent or column or the use of a different detector.Interference effects can be checked by additions of suspected interferents to synthetic samples at various concentrations of both determinand and suspect interferent. Even here, there can be snags. Complex interference effects, in which one substance alters the interference effect for a second substance on the determination of a third, are known. These double interference effects can be turned to advantage, as in matrix suppression or matrix modification when large amounts of an easily ionised metal are added to reduce the effects of another metal. In spectrophotometry beryllium suppresses fluoride in the determination of iron(II1). Sometimes in both spectro- scopy and gravimetry, it is important to specify the acid used to bring the sample to the correct pH.Methods are first evaluated on synthetic standard samples, but need to be tested on real samples to be sure that there are no unsuspected interference effects. However, reliable real samples of known composition are difficult to acquire. In order to approach their own samples as close as possible, analysts use samples to which known amounts of determinand have been added. If the determinand added to a sample or standard is not in the same form as in the sample it may react differently. Cyanocobalamin (vitamin BIZ) is a complex cobalt cyanide, but it gives very few of the reactions of either cyanide or cobalt. The same can occur with many compounds in the environment. Some errors are caused by not thinking.Many errors are caused by taking untested short cuts in the method, such as comparing the sample with standards that have not been treated in the same way as the sample, without making allowance for the difference. Impurities in the reagents, the water used or leaching from apparatus or resins used, steam, volatile trace compounds, organic pollutants in tap water and vapours wafting in from adjacent rooms present problems. Sometimes it is impossible to treat the blank and samples identically and it may be necessary to analyse the reagents separately and derive a theoretical reagent blank. Occasionally the sample itself is purer than anything else and a multiple standard additions procedure may be needed. Some determinands are so reactive that it is not practicable to use a standard sample for calibration, quality control or inter-laboratory comparative tests.Disinfecting agents for drinking water are good examples. The SCA showed that the same decay curve was obtained repeatedly in all participating laboratories and calculated the precision from the scatter of points along this curve. In such methods reagents are standar- dised with a recognised primary standard substance. Automation can sometimes help to reduce errors; thus the turbidimetric determination of sulphate in water tends to have poor reproducibility, but the automated flow injection method can be made reliable for sulphate concentrations of over 2 mg 1-1. It is impossible to have a reliable analysis if the sample is not representative of the whole.The environment varies mark- edly. Temperature, density effects, flow and turbulence or absence of turbulence cause variations. Rivers may have very complicated variations in their composition. Air can become segregated. The sampling of land and other solid materials is even more difficult. Water and air composition can vary with time of day and season of the year but, once known, for water the pattern stays fairly constant. Hence it may be worth investigating the pattern including variation over day and season. Rain can present problems when sampling large bodies of water. It may produce layers differing in composition. Density may make rivers channel through a lake or reservoir without mixing. Even with piped supplies the sampling regime must be carefully worked out.Would a first draw sample or a flushed sample be best? In areas of mixed age building there may be private supplies, statutory supplies and even several mains in one street. Ring mains with flow direction dependent on demand cause sampling problems. The British Geological Survey and others are still studying the problem of sampling groundwater. Many determinands are potentially unstable. Materials may deposit or adsorb on to bottle walls, gases are lost or may diffuse. Bacteria and similar organisms can feed on a wide variety of substrates and slow chemical reactions occur. Stabilisers are often used but these can cause false results. It pays to pre-check the sample bottles by testing a few with standards stored in them for several weeks. Some sewage and microbiological samples must be analysed almost immediately if reliable results are to be obtained.The SCA are preparing supplements on sampling techniques to go with their own existing booklets and IS0 5667. For reliable analysis it is necessary to check for errors. The simplest method is by use of regular control samples and re-analysis of stable samples, together with use of control charts. Customers have been known to check laboratories in this way. Methods which do not give normal distribution error curves require careful study. By use of matrix conversion techniques (by carrier precipitation), production line operation and regular analytical quality control procedures, two-figure accuracy can be arrived at routinely, using a method some workers rate as, at best, semi-quantitative. Animals, plants, algae, diatoms, aquatic animals and fish vary in their reaction to different environmental stresses.The SCA is issuing methods for monitoring macroinvertebrates , macrophytes and fish. The Department is funding the study of a method which may prove almost impossible to deceive. Using a combination of biological methods, especially those for macrophytes, water authorities have detected hitherto unsus- pected discharges of harmful wastes. The National Test Laboratory Accreditation Scheme (NATLAS) has been extended into the environmental field. A technical expertise assessment scheme has been suggested to back this up. There are those who think that the best way to ensure comparable results between laboratories and nations is to have all the samples analysed by the same method.This sounds to be sensible, but it is not. It might be, were all the samples the same; but they are not. A very wide variety of samples are sent for environmental analysis. Mandatory methods suffer from numerous problems. It is difficult to allow for variable interference effects without making the methods unduly complicated and wasteful. The optimum method for reliable and efficient laboratory opera- tion varies, depending on the workload and types of sample analysed. There are also personal and instrumental errors. Thus mandatory methods may lead to an uneconomic use of manpower and other resources. Inter-laboratory tests by the European Commission showed that technicians obtained the best results when they used the method with which they were most familiar.Improved methods should not be used until they are officially approved; pressure groups urging the adoption of unproven methods must be resisted. Legal problems can occur when an analysis by a mandatory method gives a result that is scientifically wrong. If mandatory provisions are necessary, the obvious require- ment would be that the analyst should provide results with adequate accuracy allowing for the type of sample, the determinand and the reason for the analysis. That places the responsibility where it should be. It follows that when planning a programme of analysis, the analyst should: (1) ensure that the proper samples are taken and the right determinands have been requested;194 ANALYTICAL PROCEEDINGS.JUNE 1988. VOL 25 (ii) ascertain how accurate the results must be, how soon variables; decide on the method; check how representa- tive the sample is; and (iii) evaluate methods with the equipment that will be used; (v) include quality assurance samples, and occasional (iv) investigate possible interference effects and the effects of re-analysis. required and consequences of delay; The Relevance of Standards R. G. Collyer Quality Assurance Services, British Standards Institution, Linford Wood, Milton Keynes, Buckinghamshire The British Standards Institution (BSI) is the body which is charged with the preparation of standards in the UK and its activities cover an enormous range of products and services. The Institution also co-ordinates the UK input into inter- national standards organisations.It was set up in 1901 and the first standards produced covered the rails for locomotives and tramways. The Institution is a unique organisation which operates as an independent body whose objectives are set out in the Royal Charter which was granted in 1929. The Institution’s main function is to draw up voluntary standards reaching the agreement of all interested parties and encourage the adoption and use of these standards in the UK. Although BSI is supported by the Government and obtains some of its funds from a direct grant, the majority of its income comes from the sale of standards and from voluntary subscrip- tions. The Government grant is based pound for pound on the subscription income which the Institution obtains.The other activities of the Institution are concerned with product testing, certification and the advisory services such as the Technical Help for Exporters. These are separately financed and receive no Government funding. The Institution combines three main activities. These are the BSI Standards Division, which is based in London and Manchester and provides secretaries for the various technical committees and assistance with the editing and drafting of standards. Draft British Standards are based on a consensus and are therefore subject to agreement by the entire committee. Once a draft has been prepared it is circulated for public comment. All comments are considered by the technical committee responsible before a standard is finalised and sent for publication.The BSI Testing Services Division is based at Heme1 Hempstead and offers a fast, confidential and consistent service to its clients from its well equipped laboratories which are organised in four main product areas-electrical, electron- ics, mechanical and physics. Each group contains separate facilities for specialised testing. However, some of the special- ised testing is carried out using outside test houses. Conse- quently to ensure consistency, all test centres used by BSI are NAMAS or NATLAS Accredited. What relevance do standards have today? There is no doubt that companies are becoming increasingly aware of quality and the consistency with which a product meets its specification. The purpose of a British Standard, or any other standard, is clearly a defined set of minimum requirements that can be used to form the basis of a product certification.They can be a code of practice, which defines minimum safety requirements or they may define a testing method. There are currently about 8000 standards, which cover every conceivable technology. In the chemical industry our standards should do more than just define simple specifications, stating the requirements for any important properties of the substance. Nearly all of the current standards include a classification for the types of grade, often giving an indication of the application for which they are intended. Other standards are associated with laboratory equipment and again define test methods, grades, etc. The third type of standard is the code of practice, which gives guidance on the safety use of various equipment types.There is an increasing demand for manufacturers of chemical products to show how their product consistently meets the requirements of customer specifications. This can often involve companies seeking registration within the requirements of the IS0 9000 BS 5750, the international quality standard, which sets out a basic framework for a quality management system. As customers become more and more quality aware, they will place increasing importance on the manufacturer’s ability to meet consistently the requirements of the specification. It is likely, therefore, that where national or international stan- dards exist these will be called up. The importance of quality management systems based on BS 5750 and I S 0 9000 will continue to grow because using one of those standards one can assure the customer that the product that is manufactured will consistently meet the specification.Linked to those standards will be the increasing demand for standard test methods so that both the manufacturer and the customer are using the same technique to verify the product quality. The use of standards then will make the job simpler because there will be standard test methods. People will all be using the same specification. A simpler job means that it will be done faster and will hopefully result in less off-specification material being produced. Standardisation will mean that a producer will be able to put a greater reliance on the products that are received from the suppliers.Again, this means that the producer will inevitably do less testing because it will be possible to have more faith in the supplier’s ability to manufacture to an agreed specification. When one specifies a product, material or service to a British Standard, then one can rely on the inbuilt assurance of that product’s fitness for its intended purpose. Using a material to a standard specification will mean that one is able to obtain it faster with the result that there will be an increased efficiency of manufacture. The importance of standardisation is growing and we obviously hope that the Institution will be able to continue to write standards that are relevant to industry. Better standards will mean a better quality of British products will hopefully enable the UK to regain its position in world markets.ANALYTICAL PROCEEDINGS.JUNE 1988. VOL 25 A Quality Assurance Viewpoint from Industry H. T. J. Chilton Monsanto plc, Ruabon, Clwyd The Ruabon plant is one of the main manufacturing sites of Monsanto Europe/Africa. It is a continuqus process operation making a range of rubber, fine and speciality chemicals which are exported to over 95 countries. A Quality Programme-Why? Our quality programme arose in response to independent studies showing the high cost of (poor) quality, because of quality competition on a world market and because of customer demand. A step change in quality from defect levels at the percentage level to the parts per million (or even parts per billion) level was required to meet this need. Conventional approaches to quality assurance would not meet this need so we resolved to use the total quality concept.This makes quality the responsibility of everyone in the organisation, not just the Quality Assurance Department. Total Quality Programme-Key Stages Our programme resolved into four key stages: policy, aware- ness, total quality system and training. Policy A quality policy was prepared and is permanently displayed in all parts of the plant. It made clear the organisation’s commitment to a policy of total quality in order to increase customer satisfaction and competitiveness. Quality improve- ment was to be a never ending process. Quality Awareness To attract people’s attention and make them aware of our intentions, a quality awareness programme was undertaken using the usual promotional features of talks, posters, competi- tions and hand-outs.The programme was not high-key as this was not a once-off campaign but is ongoing. Total Quality System To achieve our objective of total quality we needed a system 195 that would make this happen. The system which we have largely put in place contains the following elements: computer process control; statistical process control; quality assurance (conventional); product quality index; despatch quality index; quality improvement plans; quality improvement projects; quality circles; and internal audit. The system is organised so that it conforms to the requirements of BS 5750/ISO 9000. The total quality system we have set up is in effect a quality assurance system, but quality assurance as it is conventionally understood only forms one element out of nine.Training To achieve the necessary step change in quality we realised that a large training programme was necessary to change attitudes and provide required skills. As total quality requires a contribution from everyone, we set up a very large training programme which covered everyone of the 500+ people on site. In a period of 1 year each person received between seven and ten days’ full-time classroom quality training in topics tailored to be relevant to each specific job. The programme has been judged to be successful and was well received by participants. This was the largest programme ever undertaken on-site. It was executed by a team of line managers as part of their normal job and met timing and budget commitments. Con c I u s i o n Most of the elements of our quality system are now in place and we are actively working on the remainder.Currently we have a further training programme in specialist subjects for certain target groups and we expect this to continue. Our programme is now well under way and we are starting to see some of the benefits of our approach. Quality assurance is now a part of everyone’s job and, combined with quality improvement, we believe it is a vital element of continued success in a competitive international business. Laboratory Characteristics Affecting Quality Assurance Performance C. E. Wilde Department of Clinical Chemistry, Royal Infirmary, Doncaster The general external quality assessment programme (EQAS) for clinical chemistry has been operating in the UK since 1969.This general scheme and some of the more recently introduced specialised schemes are organised in Birmingham and have been directed by Prof. T. P. Whitehead for many years. The general scheme initially included 15 analyses but this has since been extended to cover 22 and well over 50 analyses are now covered in all UK EQAS clinical chemistry schemes. A method of scoring performance based on a variance index score (VZS) has been in use since the start. The variance index (VZ) for each participating laboratory is calculated from the difference between the result obtained for a given analysis and the calculated method mean (x,), expressed as a percentage of the method mean and divided by a chosen coefficient of variation (CCV) for that analysis.These CCVs were chosen on the basis of the average laboratory performance at that time. Thus x - x x , V=- x 100 X vzs = - x 100 ccv The MVZS is the mean for all analytical results at any one time and the ROMVZS is the running overall mean VZS for the last 40 results submitted. The smaller the VZS and the ROMVZS the better is the performance. Anonymity is maintained by the use of laboratory code numbers. Considerable general improvement in laboratory perform-196 ANALYTICAL PROCEEDINGS, JUNE 1988. VOL 25 ance has been demonstrated since the inception of the schemes and the introduction of each new analysis into the programme has usually quickly been followed by an improvement in the over-all performance of that analysis, although there has sometimes been a lag phase whilst the participants gained confidence in the scheme and realised that their performance was not as good as they thought.Despite the over-all improvement, there has always been a wide variation between individual laboratories with some showing consistently good and some consistently poorer performance. Some years ago a study’ way undertaken, supported by the Nuffield Provincial Hospital Trust, to attempt to define the factors which contributed to good performance. The Nuffield Study A team of nine people was assembled representing the professions practising in clinical chemistry and 70 laboratories were chosen randomly by computer to give a representative range of size, of geographical distribution and of performance in the NEQAS scheme.A number of subjective and objective criteria were assessed in each laboratory with the help of a questionnaire and a visit by members of the team. The anonymity of the schemes was respected and the performance of each participating laboratory was unknown to the survey team at the time of assessment. Table 1. Correlation between performance (ROMVZS) and some laboratory characteristics - r Quality assurance awareness (subjective) . . 0.48 Number of staff . . . . . . . . . . . . 0.42 Cost of calibration serum . . . . . . . . 0.40 Cost of equipment . . . . . . . . . . 0.39 Workload . . . . . . . . . . . . . . 0.37 Laboratory organisation (subjective) . . . . 0.24 Workload per member of staff . . . . . . 0.03 P <0.001 <0.001 <0.001 <0.01 <0.01 <0.05 NS Nine main objective criteria relating to features of the laboratory were used.These included number of staff, workload, cost of equipment and expenditure on calibration and control materials. Six derived factors including number of requests per member of staff and the number of requests related to equipment investment were calculated and three subjective “scores” were awarded by the team on their visit for quality assurance awareness, laboratory organisation and management, the last judged by the morale of staff and the attitude and interest of senior members in the work of the laboratory and welfare and training of their staff. Statistical Approaches Statistical approaches were employed for the analysis of the quantitative data to determine the relationship, if any, between scores for the various criteria and the performance of the laboratory.The correlation between the various laboratory characteristics and performance was investigated by linear regression using product moment and Spearman rank methods. Multiple regression analysis was also performed to determine if the correlation could be improved using combina- tions of factors. A second approach was to study the characteristics in relation to three equally sized groups of laboratories, those with the best, intermediate and worst performance figures. This approach involved a multiple discriminant function analysis. The third type of analysis involved grouping laboratories according to particular charac- teristics, e.g., size, workload and cost of equipment, and determining any differences in performance between these groups.In addition, the contribution to performance by particular factors such as type of equipment, staff structure and use of quality assurance and calibration was studied in greater depth. Results of Analyses (Tables 1-3) All types of analyses showed that the size of laboratory was strongly related to performance. Whichever way the data were analysed there was a significant relationship between perform- ance and workload, staff numbers, equipment costs, labora- tory area and cost of quality assurance material. These all showed a strong association with each other and the results show that the larger laboratories, however defined, tend to have the best performance.Table 2. Multivariate analysis of relationship of performance with laboratory characteristics t values Quality assurance Cost of calibration serum . . 2.25 awareness(subjective) . . 3.35 3.07 3.48 3.02 Costofequipment . . . . . 1.31 Numberofrequests . . . . 1.53 Numberofstaff . . . . . . 1.30 Correlation with ROMVZS r = 0.52 0.49 0.48 0.48 p = <0.001 Using the derived factors, e.g., individual staff workload and workload per unit of equipment cost, there was no significant correlation with performance. Indeed, the mean size/workload ratios were similar for the groups of laboratories with different grades of performance. It appears that whilst the cost of facilities (e.g., staff, equipment) related to workload were similar in all laboratories, the smaller laboratories suffered and may require greater expenditure per analytical request to attain desirable levels of performance.In addition to using quality assurance serum, clinical chemistry laboratories often use serum-based calibration material, rather than aqueous standard solutions, to compen- sate for matrix effects when analysing serum derived from patient’s blood. The degree of use of both these materials showed a particularly strong association with performance. The use of quality assurance material for internal quality control would be expected to improve performance. The use of serum-based calibration material may correlate with perform- ance because the matrix effect inaccuracies are eliminated, or because this material is extensively used on automated analysers and the correlation may result from better precision of such analysers rather than the use of calibration material per se or it may be because of the way values are assigned to the calibration material, sometimes to accord with consensus values in EQA schemes, a practice which is not recommended as it may perpetuate or accumulate problems of bias.Another group of factors which proved to be related to performance was the visitor’s subjective scores for quality assurance awareness, general laboratory organisation and laboratory management. It is perhaps not surprising that such features should contribute to good laboratory performance, but it is interesting that experienced laboratory workers can generally judge if a laboratory is likely to perform well even from a cursory impression of analytical capability, attitudes and morale of staff, awareness of quality assurance techniques and the contribution of senior members of staff to general organisation and management and to the welfare of their staff.The score for quality assurance awareness proved to be highly significantly related to performance by all statistical methods of analysis and when linked by multivariate analysis to characteristics of laboratory size even greater correlation with performance was achieved (Table 2). Some clinical chemistry laboratories are administratively independent, others are part of a pathology department encompassing other departments of clinical laboratory medi-ANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 197 cine. The latter may not have a full-time administrative head and may not have a chemist in charge.In the survey analysis the majority of laboratories in the two best performing groups were run by a full-time chemist or chemical pathologist and conversely the number of part-time administrative heads was significantly greater in the group of laboratories with the worst performance. Table 3. Discriminant function analyses ( a ) The factors which best dijyerentiated the group of laboratories with the best performance from the remainder of laboratories: Quality assurance awareness Equipment costs . . . . . . . . 0.81 3.06 <0.01 Costcalibrationmaterial . . . . 0.72 2.71 <0.01 n t P (subjective) . . . . . . . . 1.04 3.91 <0.001 Workload . . . . . . . . . . 0.81 3.04 <0.01 Number of staff .. . . . . . . 0.71 2.66 <0.01 ( b ) The factors which best differentiated the group of laboratories with the worst performance from the remainder of laboratories: Quality assurance awareness (subjective) . . . . . . . . 1.10 4.29 <0.001 Management (subjective) . . . . 0.94 3.56 <0.001 Workload . . . . . . . . . . 0.79 3.00 <0.01 n t P Number of staff . . . . . , . . 0.92 3.50 <0.001 Equipment costs . . . . . . . . 0.82 3.13 <0.01 Costcalibrationmaterial . . . . 0.73 0.27 <0.01 Laboratory Instrumentation Although estimates of equipment value were requested on the questionnaire prior to the visits, it was apparent at the visits that some of the estimates given were grossly inaccurate. The replacement values of major items of equipment were there- fore calculated in a uniform manner.Lists of equipment were compiled at the time of the visit and current prices were obtained for different equipment categories. Equipment with similar facilities was allotted an average figure for the cost of replacement. Using these figures the replacement cost of the equipment in each laboratory was calculated. The major items of equipment were the automated analysers and at the time of the survey these were single-channel continuous flow auto- analysers, multi-channel continuous flow analysers and three main types of discrete multi-channel analyser. As has already been stated, the total equipment cost was related to performance by all the statistical analyses. A breakdown of the data also showed that the use of the continuous flow multi-channel analysers was three times more widespread in the group of laboratories with the best perform- ance than in those with the worst.Conversely, laboratories in the latter group performed twice as many analyses by manual methods. Conclusions Although the survey was conducted some years ago, its conclusions are no less likely to be relevant today. There has been considerable development in the automation of labora- tory procedures in recent years and few traditional manual techniques are now used in clinical chemistry. From this point of view the survey was timely in that it was able to compare laboratories with different degrees of mechanisation and automation, an aspect of the study which would be far more difficult to investigate today.The conclusions of the survey are based mainly on statistical analyses and by the nature of such methods and the diversity of laboratories there will be exceptions to these generalisations. For instance, one very small laboratory was placed in the group with the best performance. The analyses, particularly multiple discriminant function, shows that it is easier to predict which laboratories will perform well. Thus, the poor performers include very few laboratories with a high throughput of requests, a high capital investment in mechanised or auto- mated equipment, substantial use of calibration sera, an awareness of quality assurance techniques and a full-time chemist or chemical pathologist as head of laboratory. Other factors such as attitudes to organisation and management and leadership and morale and training of staff do appear to be detectable and to play an important part in determining the level of performance in the clinical chemistry laboratory.Reference 1. McLagan, N. C., Kind, P. R. N., Daly, J . F., Kenny, A. P., King, J., McSwiney, R. R., Stevens, J . F., Tomlinson, K., and Wilde, C. E., “Factors Affecting Analytical Performance in Clinical Chemistry Laboratories,” Report of a Working Party sponsored by The Nuffield Provincial Hospital Trust, 1980. Information Management as a Quality Tool G. E. Martin ICI Chemicals and Polymers Limited, Billingham, Teesside This paper seeks to demonstrate the relevance and value of applying information management techniques in laboratories that support manufacturing operations. There is currently a surge of interest in quality issues and the adoption of quality systems that permeate entire organisations is becoming a key element of corporate strategy in an increasing number of manufacturing businesses. This trend has been stimulated largely by the quest for competitive advantage or by competitor or customer pressure.It is accompanied, however, by a growing recognition that optimum quality coincides with optimum cost effectiveness in the business taken as a whole and that judicious investment in the prevention of quality problems is well rewarded by reducing the costs associated with curing those problems. In the language of quality systems, businesses are recognising the need to strike an optimum balance between the costs involved in conforming to a quality standard acceptable in the market, and the costs incurred as a result of non-conformance to that standard.The total amount of money involved, the sum of these two costs, is very significant. Typical figures for manufacturing industry are in the range 10-30% of sales turnover. Quality and Analytical Information The highest returns on investments in quality improvement will be obtained when such improvements are directed at the major cost items attributable to non-conformance to the optimum standard. These will vary from business to business, but in general the first priority in controlling the quality of manufac- tured products is to secure and maintain control over the full manufacturing process. In this context it is necessary to distinguish between process control and product appraisal.Product appraisal alone is not usually a cost-effective approach to quality control. It represents action after the event and can198 ANALYTICAL PROCEEDINGS. JUNE 1988. VOL 25 do no more than help identify sub-standard product. It is rarely exhaustive and it does nothing to reduce the cost of scrap material or rework. It is normally more effective to monitor the process as a whole, including incoming raw materials and intermediates, and to apply statistical techniques to the data collected in order to yield information which enables the process to be kept constantly under control. Much has been published on the subject of statistical process control and this will not be enlarged upon here. An essential prerequisite to this approach, however, is the collection and processing of valid data.Depending on the nature of the production process, many of these data may be generated in the analytical laboratory. In such instances it is clearly vital that the information, which is the sole “product” of the laboratory, is consistently produced to an appropriate standard of quality. There is little point in establishing powerful systems for the control of manufacturing processes if the data on which such systems depend are derived from a process which itself is out of control and whose results may be utterly misleading. The standard of quality that is appropriate for analytical informa- tion is that which leads to the minimum total quality cost in the business as a whole.It is important, therefore, to judge potential quality initiatives that may be taken in the laboratory in relation to their effects in the business at large and not to confine attention to consideration of cost effectiveness in the laboratory in isolation. A variety of parameters is involved in determining the quality, and hence the value, of the information produced by the analytical laboratory. Pre-eminent among these is correct- ness, as other considerations cease to hold much significance if the information reported is wrong. Correctness, and the assurance of correctness, of analytical information is a fairly complex issue. It encompasses sampling procedures, reagent preparation procedures, storage of samples and reagents, maintenance of test equipment, maintenance of valid analy- tical methods, use of the correct methods for the materials and tests concerned, corroboration that the methods remained within control limits on each application, avoidance of tran- scription and reporting errors and ensuring that data collected are attributed to the method and sample to which they apply.Other quality parameters for analytical information include its availability for a range of different applications, its delivery on time in a format that is suitable for the intended use, the time and cost involved in producing it and the consistency of its production. To provide a consistent standard of analytical service the laboratory needs to employ a systematic approach to its data and information handling tasks. Such systems should be reliable and to some extent automatic, as good intentions alone will not ensure that all the procedures, checks and reviews that are necessary actually happen and are documen- ted.Laboratory managers also need facilities to monitor the laboratory’s workload and performance in order to detect trends that may compromise the quality of service unless corrective action is taken. This management information should also reveal where improvements are taking place so that the manager can promptly reward and reinforce the behaviour that brought them about. Although the factors mentioned above contribute to the control of quality of analytical information, a further layer of procedures and documentation is introduced when the labora- tory is obliged to assure internal clients and external agencies that it has consistently generated information of proven and known quality.Quality assurance involves the generation of dependable evidence that quality control operations are, in fact, being performed as specified. It requires that reasonable steps be taken to ensure the accountability, traceability and integrity of reported information and its related data. Role of Information Management In view of the trends discussed above it is hardly surprising that there is at present a very high level of interest in laboratory information management systems (LIMS). These are com- puter software systems which, in general, are designed to aid analytical laboratories with many of their data and information handling tasks. The extent to which a LIMS will contribute to the control and assurance of quality in analytical information, and hence the value of such a system to the corporation as a whole, will depend on the detailed design of the particular system. A LIMS that is designed to optimise the quality of analytical information should satisfy all of the following criteria.It should employ computer hardware and software that permits integra- tion of the laboratory system with other corporate computing systems, because laboratory information is only of value when used for decision-taking purposes and this normally involves combination with information from other sources. It should be highly reliable; many laboratories that support production operate 24 h a day, every day of the year. The system should be flexible because the organisation, instrumentation and methodology of laboratories are subject to frequent change, and yet it must be properly supportable, which means that the flexibility should be achieved by data configuration rather than custom programming.It should actively support laboratory management in performing and documenting the reviews and checks that comprise the laboratory’s quality assurance proce- dures. The system should be easy for laboratory staff to use and should be well documented. There should be adequate provision for security of access to system functions and data and for selectively archiving data on to long-term storage media such as magnetic tape. Above all, the system should contribute positively to reducing the risk of error in the generation and reporting of analytical information. The criteria discussed above were prominent among the considerations built into the design of the LIMS which has been developed in ICI Chemicals and Polymers Limited. This system, known as “ACCOMPLIS,” runs on a distributed network of VAX and microVAX computers, which support a complete department of analytical laboratories that may be physically distributed over a large manufacturing site. It makes extensive and novel use of bar-code technology to eliminate repetitive keyboard operations, which otherwise can be significant sources of error. The system software provides very extensive LIMS functions which include a wide range of features dedicated to the control and assurance of quality in analytical information. The data gathered and processed by the system are securely stored in the ACCOMPLIS data base from where a variety of different reports are generated and automatically delivered to customers of the analytical service. One of the current areas of development is concerned with automatic data exchange between ACCOMPLIS and a similar system which has been developed by ICI for real-time monitoring and control of manufacturing plant. The implementation of a well designed LIMS can undoubt- edly contribute to increased productivity in the laboratory, liberating analysts from much of their clerical and routine calculation workload. This, however, is not the primary area of benefit to be derived from the application of this technology. If the LIMS has been designed for this purpose, the most significant advantages accrue from the enhancement of the over-all quality of the sole product of the analytical laboratory -its information. This contributes directly to the quality of products and services offered to end customers by the organisation as a whole, and this issue is now widely recognised as being central to the long-term health and survival of the business.

ISSN:0144-557X    

DOI:10.1039/AP9882500192

出版商:RSC    

年代:1988

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS, JUNE 1988. VOL 25 199 GLP and Quality Assurance The following is a summary of one of the papers presented at a Meeting of the East Anglia Region held on February loth, 1987, in Warren Spring Laboratory, Stevenage, Hertfordshire. Good Laboratory Practice and Computerisation in the Analytical Laboratory David L. M. Weller” Quality Assurance, Life Science Research Limited, Eye, Suffolk IP23 7PX Substantial changes to many laboratory working practices have been made by the introduction of computers, and therefore we need to be aware of the requirements of good laboratory practice and our subsequent responsibilities in using existing or introducing new computer systems. For consideration are: firstly, Good Laboratory Practice regulations, “the letter and the spirit ,” and their relationship with computerisation; secondly, the need for a management policy on computerisation; and thirdly, procedures to be adopted for each system under this policy, including specifica- tion of hardware and software, definition of raw data and archive media, physical and procedural system security, hardware and software maintenance, personnel training and clearance to perform specific tasks, system validation and certification and standard operating procedure (SOP) prepara- tion; and finally, the role of the quality assurance unit.Good Laboratory Regulations There never has been and there never will be any argument for poor laboratory practice. It should never have been necessary for governments to set up good laboratory practice as law. However, in the field of safety testing of chemicals, because of the betrayal of trust by some scientists, that is now the situation.Even though Good Laboratory Practice (with capital letters) is now law, we should remember that the principles of good laboratory practice (GLP) have not been significantly changed by becoming law. Legal GLP documents, regardless of governmental source, will not tell one in detail how to run an analytical laboratory and will certainly not tell one how to computerise it. The earliest GLP legislation does mention computers fleetingly and the most recently published GLPs make more references to computers, but still fall a long way short of being a blueprint for computerisation. It is important then, when using computers in the laboratory, to apply both the spirit and the “letter” of GLP.If experimental work is conducted in compliance with GLP, with or without the aid of computers, it should be possible for an inspector, maybe 4 or 5 years hence, to look at the records of the work and determine easily why, how and by whom the work was done, who was in control (the Study Director), what equipment was used, the results obtained, any problems that were encountered and how they were overcome. The introduc- tion of computers into the laboratory does not alter these basic requirements in any way. However, the level of compliance with the principles of good laboratory practice needs to be upheld. Various groups have been applying their minds to com- puterisation and compliance with good laboratory (and good * On behalf of the Computer Auditing Working Party of the Quality Assurance Group (UK) .manufacturing) practice regulations both in USA and the UK. Reports available of comments and findings from regulatory inspections (particularly those in the USA) show a high and increasing level of interest in computerisation on the part of inspectors. Inspections in the UK performed by the DHSS have, to date, shown little in-depth computing content, although the inspectorate has indicated that they will tackle computerisation in the future. We now have an opportunity, by solid thought and action on computer operations, to pre-empt governmental GLP require- ments and ensure that, with due care and liberal common sense, procedures are of the highest integrity.So what should we be doing in practical terms? The first job must to be evaluate the position of one’s laboratory, both in terms of present or planned systems and in terms of compliance with GLP. The second concerns manage- ment, who may or may not be familiar with computers. Management need to be aware of the position, consult system users, computer and QA staff, and produce a policy on computerisation, to define strategy and systems through which they can exercise control. The policy should cover the following aspects: Organisation and staff responsibilities . . Acquisition . . . . Project control and organisation . . . . Records and documentation . . Operational code of practice . . . . . . Including systems management, communication, decision-making , control of software.Purchasing of hardware and software; writing software. Progress monitoring, validation criteria, personnel involved, acceptance. Record type, raw data definitions, archiving, writing of standard operating procedures (SOPS). Security, training, assessment. The discipline of such a policy offers the potential to work in an organised manner and from a position of strength. Each system or application should be the subject of a formal plan, with intentions and criteria being clearly stated, and it should apply equally to in-house and commercially purchased soft- ware packages, for the latter paying particular attention to defining who takes responsibility for validation (supplier, purchaser or both). The imposition of such a policy may not be universally welcomed, particularly as the disciplined approach it aims for may slow down system implementation, but this very process200 ANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 allows time for thought and effective action, resulting in a more useful and reliable final product. All systems and application-specific procedures should be fully documented and the documents filed.System-Specific Procedures Specifications for Hardware and Software These are basic but important and require definition, in complete detail, of the task to be carried out and constraints on it, to enable suppliers to produce an adequate specification upheld by equipment and software. Definition of Raw Data and Archive Material This seems very simple, but may prove difficult, particularly where analysers are linked to computers.The facilities this gives for screen review of original data, selection of data or removal of interference, etc., may indicate the possibility of editing original data and overwriting it in the memory, so the system needs to be designed so that files are not overwritten, but edited, leaving a full audit trail of the analyst’s interven- tion. When it comes to choosing and defining a medium for archiving the management policy should give firm guidance. The choice of medium used, e.g., floppy disc, paper printout or tape, is not easy to make but it must be made and proper provision made for secure archiving and for any necessary maintenance of stored material. System Security-Physical and Procedural To ensure that neither software nor data are corrupted by unauthorised access, steps must be taken to secure the system.Sign-on and sign-off procedures serve to keep unauthorised people out and identify bona fide users. Good computing practice should ensure that backup copies of software are kept and that backup copies of data are made at regular intervals and stored securely in more than one location. Maintenance of Hardware and Software Computer hardware should be treated like any other equip- ment operated to GLP standards. There should be planned routine maintenance, breakdowns and faults should be logged, and all maintenance and repair activity documented. Software maintenance should follow similar procedures. Personnel Training and Clearance to Perform Specific Tasks GLP requires that personnel should have education, experience and training appropriate to the tasks they have to perform.This applies equally to computerisation as to every other aspect of laboratory work. Only trained staff should be given access to computer systems and then only to those functions within the system where they have responsibilities. “Edit capability” should be severely restricted, so that data can only be altered with the knowledge and under the supervision of a senior member of staff. System Validation and Certification System validation exercises should be organised like GLP compliant studies. Someone should be identified as being in charge who should not be the author of the software. Each validation exercise should have a plan (protocol), which is formally approved, and changes should be docu- mented.The nature and scope of the validation programme will vary with the system but should provide assurance that the whole system (including personnel) (a) meets specification, (b) produces correct results under normal operating conditions and (c) responds in a reasonable way under stress. Consideration should be given to periodic revalidation, mainly to ensure that software has not become corrupted, but also following system enhancement or “bug fixing. ” In every instance records should be maintained and archived of why, when, how and by whom. Standard Operating Procedures To permit reconstruction and repetition of experiments, the methods used should be fully documented. Standard pro- cedures require writing up as SOPs, which should be prepared and available early in the life of a new system. SOPs are best written by the person who knows most about the system but should be reviewed by someone at least one step removed from the system and more able to take a broader view.They should be approved by management. Quality Assurance Quality assurance personnel should become involved in monitoring all aspects of computerisation. They should estab- lish procedures that enable them to assure management that their policy on computerisation is being adhered to, that the system-specific procedures described are in place and that SOPs are being followed. In conclusion, although GLP regulations on computerisation are not specific, they have certain requirements for the selection of suitable equipment, maintenance and calibration of that equipment, accountability of data, archiving of data, staff training, education and experience, and quality assur- ance. To comply with these requirements and to ensure planned and controlled use of a valuable resource, manage- ments should formulate a policy on computerisation, system- specific procedures should be developed and documented, and quality assurance should perform a monitoring function. If this resource is not controlled, quality will suffer.

ISSN:0144-557X    

DOI:10.1039/AP9882500199

出版商:RSC    

年代:1988

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS. JUNE 1988. VOL 25 201 Equipment News Atomic Absorption Spectrometers The PU9100 Series complements the makers’ PU9200 an PU9400 Series, launched in 1987. The new range super- sedes the SP9 and is designed to meet the elemental analysis needs of every labora- tory. Ideal entry-level instruments, they are modular in design, so that upgrading can be carried out easily. Control and data manipulation facilities are offered via an IBM-compatible Philips analytical each with its own microprocessor and command instruction set. A wide range of modules are available, including pro- grammable HT power supply, photon counting data acquisition, lock-in ampli- fier/demodulator and drivers for chop- pers, mirrors and filter wheels. The Prism software package is configured to run on IBM-PC/AT and compatible computers.All the data acquisition functions, includ- ing those of a JY multi-channel detector, Philips Analytical PU9100 Series atomic absorption spectrometer data station. Also featured are high- energy, single-beam optics and a totally inert fluoroplastic spray chamber with high solids burner for improved sample handling. A comprehensive range of accessories is available. Philips Analytical, York Street, Cam- bridge CB12PX. Infrared Analyser The Compscan 7000s near-infared stand- alone analyser is designed to provide fast, accurate, quantitative analysis on up to 100 products. It is simple to use. The operator selects the product and up to six calibrations are then displayed simul- taneously. Once the sample cell is loaded into the sample transport module analysis results are displayed in seconds. Results can be obtained as hard copy through the external line printer and data can be transmitted alternatively to IBM PC or PC compatible using NSAS-PC software.A multiplex of up to six units at different locations, controlled through one PC, is possible. The wide variety of sampling cells available includes a high fat/high moisture, slurry/paste cell, large granular cells, textile cells, reflectance cells and cuvettes. Pacific Scientific, 4 First Avenue, Mar- low, Buckinghamshire SL7 1YA. Spectrometer Controller, Data Acquisition System and Software The Spectralink is an electronic control centre built from a number of modules, are integrated with a complement of data manipulation routines. Operation can be made fully automatic once the operator has selected the desired spectral region.The Spectralink - Prism combination operates with the complete range of JY monochromators and spectrographs, with focal lengths ranging from 10 cm to 10 m and with both single and multi-channel detectors. Instruments SA - EDT Ltd., 14 Trading Estate Road, Park Royal, London NWlO 7LU. Spectrophotometers Two scanning ultraviolet - visible spectro- photometers from Cecil Instruments have a wavelength range of 190-800 nm (optionally 900 nm) and an extensive range of accessories (including a high resolution graphic plotter) which peak labels and tabulates all operating parameters, and sequences and lists all peaks by both height and wavelength. The instruments are the 5000 and the 6000 Series and they use a symmetrical double beam optical system and have as standard features automatic wavelength calibra- tion, RS232C bi-directional computer interface and Talkback display.The 6000, when used in conjunction with the Super- scan graphic plotter, has full overlay capability and 1st to 4th derivative spectra as standard features. Scientific and Medical Products Ltd., Shirley Institute, Didsbury, Manchester M20 8RX. Data Handling Package New features have been added to PECCS, the general purpose ultraviolet - visible and ultraviolet - visible - near infrared data handling package for the Lambda series of instruments and the IBM PC. The new software permits the use of a colour monitor, via the EGA graphics card, in addition to the Hercules mono- chrome card, and data can be stored on disk in ASCII using one of the two JCAMP formats for easy incorporation into other programs and databases.Plot- ing routines for the HP 8-pen plotter are also included. Perkin-Elmer Ltd., Post Office Lane, Beaconsfield, Buckinghamshire HP9 1QA. Colorimeter A new model of the Tristimulus col- orimeter, the CR-231, allows absolute colour or colour difference to be measured on the basis of any of four colour systems: Vxy, L*a*b, L*C*Ho or Munsell. Either CIE Illuminant C or D65 can be selected and reflection density can also be measured. The CR-231’s memory provides space for 20 calibration stan- dards, 20 target colours for colour differ- ence measurements and 300 sets of colour measurement values.A built-in alarm can be used to warn users when the colour difference is outside pre-set limits. Minolta (UK) Ltd., 1-3 Tanners Drive, Blakelands North, Milton Keynes MK14 5BU. Data System and Controller for Chromatography An IBM compatible multi-tasking data system and controller for HPLC and GC, the Axxiom Model 747, allows the user to enter and edit programs for one system while two others are running and collect- ing data. It can be configured to control three binary and two ternary HPLC systems, with independent starting and stopping. User interaction is via a key- board with special function keys that remove the need for mnemonics or codes. All the information needed to run, inte- grate, analyse, archive and print data is contained on just four screens. For quick and easy file entry a simple “fill in the blanks” style of programming is used.Ciba Corning Diagnostics Ltd., Hal- stead, Essex C 0 9 2DX. Automatic Set-Up of User Defined Analyses for Gas Chromatography Shimadzu GC-l4A, 15A and 16A gas chromatographs, equipped with a current loop interface, can be automatically set up for user defined analyses simply by insert-202 ing an IC card into the associated C-R5A Chromatopac integrator. The integrator then loads the stored program and com- municates with the chromatograph on selected parameters such as injector, col- umn and detector temperatures, flow- rate, amplifier settings, etc. Data routines within the integrator are also set up by the IC card. Dyson Instruments Ltd., Hetton Lyons Industrial Estate, Hetton, Houghton le Spring DH5 ORH.Aluminium Clad Capillary Columns The extended range of ALSIL columns are available in 0.53, 0.32 and 0.22 mm internal diameter. They incorporate improved low bleed bonded phases and are designed to achieve excellent perfor- mance when used in all chromatography systems, particularly where the user is operating a GC - MS system. A new high temperature HT5 bonded phase capable of continuous operation at temperatures of 460 "C and temperature programming to 480°C has been developed. Scientific Glass Engineering (UK) Ltd., Potters Lane, Kiln Farm, Milton Keynes MKll 3LA. Column Oven for Chrtjmatography The Model 505 oven offers temperatures of 10 "C above ambient to 99 "C with 0.02 "C stability and 1 .O "C repeatability. It can accommodate an injector, guard column and both analytical and prepara- tive columns up to 1 in for precise control of temperature conditions. Scientific Glass Engineering (UK) Ltd., Potters Lane, Kiln Farm, Milton Keynes MKll 3 LA.Chromatography Software The latest upgrade to the operating soft- ware for the makers' HPLC ChemStation can double the productivity of the HP 1090 liquid chromatography system. Offering full foreground - background operation, data evaluation and reporting can be effected on-screen at the same time as data from another run are being collected. Optional gel permeation chro- matography software is also available. Hewlett-Packard Ltd., Miller House, The Ring, Bracknell, Berkshire RG12 1XN. Ion Chromatography System The Shimadzu HIC 6A system is based on a new and superior design, non-suppres- sor type conductivity meter and delivers high precision and stability, as the detec- tor has built-in microprocessor control and three stage temperature control.Although designed for use with the Shi- madzu LC-6A pump, the HIC 6A can be configured with any good quality HPLC pump incorporating a pulse damper. The Shimadzu modular approach allows a simple HIC 6A system to be easily upgraded for full automation, and an ANALYTICAL PROCEEDINGS, JUNE 1988. VOL 25 existing LC can be converted for ion chromatography work. Dyson Instruments Ltd., Hetton Lyons Industrial Estate, Hetton, Houghton le Spring DH5 ORH. DNA-Grade Hydroxylapatite Bio-Gel, a DNA-grade hydroxylapatite, can be obtained for the quantitative analysis of nucleic acids, particularly hybrid species.Bio-Rad Laboratories Ltd., Caxton Way, Watford Business Park, Watford, Hertfordshire WD1 8RP. Chromatography Column for Purification of Antibodies Formulated specifically for the purifica- tion of antibodies and monoclonal anti- bodies in biotechnology and pharmacol- ogy, the HiPAC Protein A column uses the makers' HiPAC silica support, mak- ing the column highly pressure and pH tolerant, while cutting purification time from several hours to 10 min. ChromatoChem Inc., 2837 Fort Mis- soula Road, Missoula, MT59801, USA. Amino Acid Analysis The System Gold Personal Chromato- graph is now available in a special con- figuration for amino acid analysis. Ion- exchange chromatography can be used with this system and there is a choice of the makers' Spherogel ion-exchange col- umns for separating either physiological fluids or hydrolysates.For results unaffec- ted by sample matrix or derivative stabil- ity during separation, the system uses cation exchange with ninhydrin post-col- umn derivatisation and detection at 500 nm. This method separates all amino acids in a single process. The system can be easily configured for high sensitivity binary gradient analysis of PTH, PTC and OPA derivatives using the makers' Ultra- sphere columns. Beckman Ltd., Progress Road, Sands Industrial Estate, High Wycombe, Buck- inghamshire. Automatic Set-up for Gel Permeation Chromatography All parameters necessary for reliable data handling in gel permeation chromato- graphy can now be set up automatically using 3; in disk based software for the Shimadzu C-R4A Chromatopac integra- tor.Dyson Instruments Ltd., Hetton Lyons Industrial Estate, Hetton, Houghton le Spring, DH5 ORH. Gel Dryers Among the features of the Model 543 and Model 583 gel dryers are the ability to select pre-set programmed cycles for opti- mised drying of a variety of gels, a quick seal track for instantaneous gasket sealing and selectable temperature settings from 50 to 90°C. For sequencing gels, the pre-set cycle speeds up drying by eliminat- ing pre-heating requirements. The pre-set cycle for gradient and PAGE gels elimi- nates the stress of rapid temperature changes, which can cause cracking of these gels. Bio-Rad Laboratories Ltd., Caxton Way, Watford Business Park, Watford, Hertfordshire WD1 8RP. Electrophoresis System for DNA GeneLine is an electrophoresis system which offers a novel and reliable method for the separation of megabase fragments of DNA.A transverse alternating field electrophoresis system, GeneLine makes use of pulsed field electrophoresis, but with a unique difference which allows simple separation of DNA fragments from 2 kb to more than 9000 kb in size. It also separates whole chromosomes as large as nine million base pairs in straight, high resolution lanes. Beckman Ltd., Progress Road, Sands Industrial Estate, High Wycombe, Buck- inghamshire. Combustion Gas Analyser The 700B instrument features a new design of probe assembly coupled to the makers' microprocessor controller. The 700B is available with oxygen and carbon monoxide measurements or with oxygen only.Combustion gas temperatures as high as 1800 "C can be handled. The stack mounted sensor uses a low demand aspir- ator to produce a positive sample flow, thus offering a 90% response for a 0.5 m ceramic probe of typically 7.2 s. Servomex Ltd., Crowborough, Sussex TN6 3DU. Moisture Analyser The ERH 100 has been specifically de- signed to meet the food industry's requirement for high accuracy, repeat- ability, quick response and ease of opera-ANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 203 tion. It offers single or multi-station Sam- pling units, which allow the analyser to be used for a variety of roles from simple spot checks of manufacturing processes to analytical batch sampling and the genera- tion of moisture sorption isotherms.The operating range of the sensor is 5-100% ERH (equilibrium relative humidity) and the accuracy is better than +1% between 5 and 90% ERH and better than +2% above 90% ERH. Michell Instruments Ltd., Unit 9, Nuf- field Close, Nuffield Road, Cambridge CB4 1SS. Dew-point Meter The makers of the new instrument have filed a British patent application for a device that overcomes the problems inherent in the determination of the dew-point of gases. The new development involves the interposing of a heat pipe between the heat pump and heat sink, thus allowing the use of a small heat sink which can be situated sufficiently far from the mirror surface so that neither has any adverse effect on the other. Moreover, the heat pipe enables the mirror surface temperature to be reduced by the heat pump to a level unattainable in traditional instruments.Consequently the dew-point meter has a significantly wider opera- tional range. Michell Instruments Ltd., Unit 9, Nuf- field Close, Nuffield Road, Cambridge CB4 1SS. Titroprocessor The third generation instrument from Metrohm allows the user to plan the sequence of a method including all auxi- liary functions, such as the addition of solutions with pumps or dosimats, before or within a titration procedure. Both dynamic titrations with variable volume steps and monotonic titrations with con- stant volume steps can be performed. Complex titrations containing up to four different procedures in a single method are also possible. V.A. Howe and Co. Ltd., 12-14 St. Ann’s Crescent, London SW18 2LS.Sample Changer for Automatic Titration The Mettler ST20 sample changer, in combination with any one of the makers’ latest titrators, saves time by extensively automating sample preparation and analysis routines both during and outside normal working hours. The titrator accepts up to 40 sample weights from a balance, stores them and after every titration reconciles the consumption to produce the required result. The standard sample turntable can accommodate 20 samples of up to 100 ml; an alternative turntable accepts 14 samples of up to 250 ml. MSE Scientific Instruments Ltd. , Sus- sex Manor Park, Gatwick Road, Crawley, West Sussex RHlO 2QQ. Diagnostic System The Easy St diagnostic analyser is a benchtop unit which carries out fast, accurate and economic diagnoses of serum, plasma and urine in individual wards, ~linics and in general medical pm.All contact parts of the filter can be sterilised either individually by autoclave or as a complete unit by in-line steam sterilisation. The high performance filter tube used to remove bacteria can also be sterilised in an autoclave and will tolerate temperatures up to 150 “C in dry gas. The filters comply with the requirements of the FDA. Balston Ltd. , Monckton’s Lane, Maid- stone, Kent ME14 2QB. Laboratory Information Management System LIMS 2000VX is an enhanced version of LIMS 2000. It is compatible with Digital Equipment Corporation’s VAX com- puter series as well as Concurrent Com- puter Corporation’s 3200 series of mini- computers. Perkin-Elmer Ltd. , Post Office Lane, BDH Diagnostics Easy St diagnostic analyser practices.Capable of carrying out more than 40 diagnostic tests, it provides results of selected tests in 2-6 min. BDH Diagnostics Division, Broom Road, Poole BH12 4”. pH Electrodes for Use in Fermentation A range of steam sterilisable pH and Redox electrodes have been designed for use with laboratory, pilot-plant and pro- duction fermenters. Demonstrating an average electrical resistance of 100-200 MQ, they give a fast response to pH change. Russell pH Ltd., Station Road, Auch- termuchty, Fife KY14 7DP. Sterile Air Filtration Unit A new filtration unit provides clean, dry, sterile air from oily, wet, dirty com- pressed air. Its multi-stage filter removes over 99.9999% of all particles down to 0.1 Beaconsfield, Buckinghamshire HP9 1QA.Ultraviolet Dryer The Minicure is a benchtop ultraviolet dryer suitable for laboratory, test and quality control work. Designed for use with ink, paint and surface coating Sam- ples or in any other application involving the use of ultraviolet-curable inks and varnishes, it is able to simulate production conditions. Its conveyer speed can be varied, and the unit can be fitted with a tachometer. There are sizes from 150 to 360 mm wide and the unit can be supplied with one or two air-cooled medium-pres- sure mercury-arc lamps in ratings of 80, 100 or 120 W cm-1. Other models have combination systems incorporating infrared, ultraviolet drying and nitrogen purging. Primarc Ltd., 121 Loverock Road, Reading, Berkshire RG3 1DZ.204 ANALYTICAL PROCEEDINGS, JUNE 1988.VOL 25 Muffle Furnace A new compact design incorporates four ranges with eleven models and chamber sizes varying from 1.8 to 9 1. It is available in three temperature ranges, maximum temperatures 1000, 1100 and 1200 “C. All models feature cool exterior cases, asbes- tos-free low thermal mass insulation, top grade wire wound elements, up and over door with self locating position lock, overtemperature protection, fully remov- able control console and various control options. Thermo-Active Ltd., Unit lC, Carlisle House, 99 Carlisle Street East, Sheffield S4 7QN. Detergent Enzyme Lipolase is the first industrial enzyme product to be produced for the world market by genetic engineering and the first fat-splitting detergent enzyme ever. Novo Industri A h , Novo Allk, 2880 Bagsvaerd, Denmark.Lasers Three new He : Ne lasers are to be offered at reduced prices until June 30th, 1988. All units meet the German VDE specifi- cation. The PL-605 has a red power output of 0.5 mW at a wavelength of 632.8 nm. The PL-610 gives a red output over 2 mW at 632.8 nm. The PL-405GR gives a green output over 0.5 mW at 543 nm. Lambda Photometrics Ltd., Lambda House, Batford Mill, Harpenden, Hert- fordshire AL5 5BZ. Literature A twelve-page catalogue describes the makers’ range of optical emission spec- trometers using the arc - spark technique, plasma instrumentation including the DCP and ICP excitation techniques, X-ray fluorescence sim and seq spec- trometers and the SMS-100 and SMS-200 automatic sample manipulation systems. Leaflets are also available for these last robotic systems.“ICP Applications,’’ a series of method sheets giving details of the analysis of real samples, provides information on sample and standard pre- paration, instrument conditions and spread notes about areas requiring special attention. ARL Applied Research Laboratories SA, En Vallaire, 1024 Ecublens, Switzer- land. Literature describes the 6250 and the Composcan 7000 series near-infrared spectrophotometer range. Pacific Scientific, 4 First Avenue, Globe Park, Marlow SL7 1YA. A brochure gives details of the Axxiom 747 PC-based, multi-channel, multi-task- ing data system and controller for HPLC and GC. The System can monitor one to six chromatograms and control three binary or two ternary HPLC systems simultaneously. Quadrant Scientific Ltd., 36 Brunswick Road, Gloucester GL1 1JJ. A new, up-to-date and comprehensive applications bibliography for sample preparation lists over 500 articles and procedures which cite the use of Analyti- chem’s solid-phase extraction products in the extraction and purification of a wide variety of chemical compounds found in biomedical, clinical, environmental, food and general applications. Analytichem International, P.O. Box 234, Cambridge CB2 1PE. The formation of a GC Users Group has been announced. Offering regular updates on new equipment, technical application notes outlining specific analy- sis procedures and a GC Users Group Newsletter, it will enable members to be kept to date with the latest developments in gas chromatography. Analytical Measuring Systems, Shire- hill Industrial Estate, Shirehill, Saffron Walden, Essex CBll 3AQ.

ISSN:0144-557X    

DOI:10.1039/AP9882500201

出版商:RSC    

年代:1988

数据来源: RSC

摘要:

204 ANALYTICAL PROCEEDINGS, JUNE 1988. VOL 25 Publications Received Chromatographic Separations. Peter A. Sewell and Brian Clarke. Ana- lytical Chemistry by Open Learning. Pp. xx + 335. Wiley. 1987. Price E13.95 (softback); E36.50; $77.50 (hardback). ISBN 0 471 913715 (softback); 0 471 913707 7 (hardback). Scientists in Conference. The Conference Organizer’s Handbook. The Congress Visitor’s Companion. Volker Neuhoff. Pp. xix + 223. VCH. 1987. Price DM58. ISBN 3 527 26579 1 (VCH Verlagsgesellschaft); 0 89573 591 1 (VCH Publishers). Modelling of Structure and Properties of Molecules. Z. B. Maksid. Pp. xviii + 360. Ellis Horwood. Price f38.50. ISBN 0 7458 0168 4 (Ellis Horwood); 0 470 21010 9 (Halsted Press). Reagent Chemicals. Seventh Edition. American Chemical Society Specifica- tions.Official from January 1, 1987. Pp. xiv + 713. American Chemical Society. 1986. Price $89.95 (US and Canada); $107.95 (Export). ISBN 0 8412 0991 X. A Protocol for Analytical Quality Assur- ance in Public Analysts’ Laboratories. Pp. 40. Association of Public Analysts. 1987. Price E12.50. Guide to Safe Practices in Chemical Lab- oratories. Pp. 48. Royal Society of Chemistry. 1986. Price f10; $18. ISBN 0 85186 479 1. Laser Optoacoustic Spectroscopy. Springer Series in Optical Sciences, Vol- ume 37. Pp. x + 327. Springer-Verlag. 1986. Price DM149. ISBN 3 540 11795 4; 0 387 11795 4. Organo-chlorine Solvents. Health Risks to Workers . Commission of the European Communi- ties. Pp. xvi + 254. Royal Society of Chemistry. 1986. Price 550; $90. ISBN 0 85186 078 8. The Analysis of Agricultural Materials.Third Edition. Ministry of Agriculture, Fisheries and Food. Reference Book 427. Pp. x + 248. HM Stationery Office. 1986. Price f13. ISBN 0 11 242762 6. Organo-chlorine Solvents. Health Risks to Workers. Commission of the European Communi- ties. Pp. xiv + 254. Royal Society of Chemistry. 1986. Price 550; $90. ISBN 0 851186 078 8. Sample Preparation and Isolation Using Bonded Silicas. Proceedings of the Third Annual International Symposium, May 5-6, 1986, Sheraton Poste Inn, Cherry Hill, NJ. Pp. 327. Analytichem International. 1987. Price E23. Available from Jones Chromatography, Hengoed, Mid-Glam- organ. Food Additives-The Professional and Scientific Approach. Pp. iv + 20. Institute of Food Science and Technology (UK).1986. ISBN 0 905367 01 4. Recent Developments in Ion Exchange. Edited by P. A. Williams and M. J. Hudson. Pp. xii + 423. Elsevier Applied Science. 1987. Price 245. ISBN 185166 101 8.ANALYTICAL PROCEEDINGS. JUNE 1988. VOL 25 205 Advances in Non-Linear Spectroscopy. Edited by R. J. H. Clark and R. E. Hester. Pp. xvi + 363. Wiley. 1988. Price f70. ISBN 0 471 91652 8. Analytical Chemistry. Principles and Techniques. Larry G. Hargis. Pp. xvi + 672. Prentice- Hall. 1988. Price 217.95 (softback). ISBN 0 13 033564 9. Biosensors International Workshop 1987. Edited by R. D. Schmid. GBF Mono- graphs, Volume 10. Pp. xx + 346. VCH. 1987. Price DM128. ISBN 3 527 26801 4 (VCH Verlagsgesellschaft); 0 89573 6837 (VCH Publishers). Statistics for Analytical Chemistry. Second Edition.J. C. Miller and J. N. Miller. Pp. 227. Ellis Horwood. 1988. Price f26.50; $59.90 (hardback); f9.95 (softback). ISBN 0 7458 0271 0 (hardback); 0 7458 0292 3 (softback); 0470 20902 X (Halsted Press). Detection and Data Analysis in Size Exclu- sion Chromatography. Edited by Theodore Provder. ACS Symposium Series 352. Pp. x + 307. American Chemical Society. 1987. Price $69.95 (USA and Canada); $83.95 (rest of the world). ISBN 0 8412 1429 8. Klinisch-toxikologische Analytik. Gengen- wartiger Stand und Forderungen fur die Zukunft. Pp. viii + 92. VCH. 1987. Price DM38. ISBN 3 527 27405 7. Toxicological Evaluation of Certain Food Additives and Contaminants. Prepared by The 29th Meeting of the Joint FAO/WHO Expert Committee on Food Additives. WHO Food Additives Series 20.Pp. viii + 286. Cambridge University Press. 1987. Price f19.50; $24.95. ISBN 0 521 34347 X. Laboratory Information Management Systems-Concepts, Integration and Implementation. Edited by R. D. McDowall. Pp. xvi + 383. Sigma Press. 1987. Price €24.95. ISBN 1 85058 083 9 (Sigma Press); 0 470 20947 X (Halsted Press). Macmillan Dictionary of Chemistry. D. B. Hibbert and A. M. James. Pp. viii + 532. Macmillan Press. 1987. Price €45 (hardback); E14.95 (softback). ISBN 0 333 39081 4 (hardback); 0 333 43471 4 (softback). Methods for the Examination of Water and Associated Materials. Standing Committee of Analysts (to review Standard Methods for Quality Control of the Water Cycle); Department of the Environment, National Water Council. Acid Soluble Aluminium in Marine, Raw and Potable Waters (Second Edition). 1987. Pp. 58. 1988. Price &3. ISBN 011 752040 3. The Determination of 6 Specific Poly- nuclear Aromatic Hydrocarbons in Wat- ers (with Notes on the Determination of other PAH) 1985. Pp. 44. 1988. Price 54.30. ISBN 0 11 752032 2. Determination of Acrylamide Monomer in Waters and Polymers. 1987. Pp. 17. 1988. Price €2.80. ISBN 0 11 752039 X. Examination Biological Filters, Toxicity to Aerobic Bacteria, Effect of SRT and Temperature 1985-6. Pp. 46. Price f4.30. ISBN 0 11 752037 3. Comprehensive Organometallic Analysis. T. R. Crompton. Pp. xxvi + 883. Plenum Press. 1987. Price $129.50. ISBN 0 306 42593 9. Chemometrics: a Textbook. D. L. Massart, B. G. M. Vandeginste, S. N. Deming, Y. Michotte and L. Kauf- man. Data Handling in Science and Tech- nology, Volume 2. Pp. xii + 488. Elsevier. 1988. Price $85.25; Dfl175. ISBN 0 444 42660 4 (Volume 2); 0 444 42408 3 (Series).

ISSN:0144-557X    

DOI:10.1039/AP9882500204

出版商:RSC    

年代:1988

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS. JUNE 1988. VOL 25 205 Conferences and Meetings Electrochemistry Graduate Students Meeting June 20, 1988, London This meeting will be held in the Chemistry Department of Imperial College. It will be a Joint Meeting of the Electroanaly- tical and Electrochemistry Groups of the RSC and the Electrotechnology Group of the SCI. Details of registration are available from Dr. G. H. Kelsall, Royal School of Mines, Imperial College, Lon- don SW7 2BP. (Tel. 01-589-5111.) Nuclear and Radiochemistry July 11-15, 1988, Brighton The second international conference on this subject will be held in the Brighton Metropole Hotel, and will form part of the twenty-first anniversary celebrations of the formation of the Radiochemical Methods Group of the Analytical Divi- sion of the RSC.The invited lecturers will be Dr. D. C. Hoffman, Dr. D. Comar, Dr. J. Silvester, Professor E. A. Scheikert, Dr. C. Allen, Professor B. F. Myasoedov, Dr. E. I. Hamilton, Dr. K. Roessler and Dr. A. Dyer. The pro- gramme will consist of sessions on Nuclear Reactions, Radioanalytical Chemistry, Radionuclide Production and Labelling, Radioactive Nuclides in the Environment, Chemistry of the Nuclear Fuel Cycle and Cosmo- and Geo- chemistry. For further information contact the Secretary, Analytical Division, The Royal Society of Chemistry, Burlington House, Piccadilly, London W1V OBN. 18th International Symposium on En- vironmental Analytical Chemistry and 4th International Congress on Analytical Techniques in Environmental Chemistry September 5-8, 1988, Barcelona, Spain These combined symposia will be held under the sponsorship of Expoquimia and the Catalan Chemical Society.The speak- ers on Instrumentation Techniques will be J. L. Anderson, J. Arpino, D. Barcelo, C. M. G. van den Berg, U. A. Th. Brinkman, H. A. Das, R. W. Frei, R. van Grieken, G. G. Guilbault, J. A. Haseth, D. M. Hercules, G. Knapp, J. F. Law- rence, J. C. van Loon, G. Mille, G. Ramis, S. Straja, J. D. R. Thomas and M. Valcarcel. Other sessions will be on Inorganic Pollutants, Organic Pollutants, Aquatic Environment and Atmospheric Environment. For information write to the Palau de Congressos, Departament de Conven- cions, Av. Reina Ma. Cristina, s/n.-08004 Barcelona, Spain. 2nd International Symposium on New Trends in Chemistry-the Role of Analy- tical Chemistry to National Development January 2-7, 1989, Cairo, Egypt Based on the success of the first event in 1984, which was attended by more than 250 participants from 10 different coun- tries, a second symposium is to be organ- ised at Cairo University, Giza.The cen- tral theme of the conference, which is supported by the Working Parties on Analytical Chemistry and Food Che- mistry of the Federation of European Chemical Societies, will be the contribu- tion of Analytical Chemistry to national development, focusing on agricultural, food, health and environmental che- mistry, as well as life and materials science. Analytical chemists from indus- trialised countries are particularly invited to present their developments and share206 ANALYTICAL PROCEEDINGS, JUNE 1988, VOL 25 their experience and knowledge.Cairo, being the centre of the Arabic world, is one of the most fascinating cities in the world. Pharaohic Egypt provides some of the greatest wonders of histroy. Pre- or post-conference programmes will be offered on personal request. Comfort- able, budget priced, accommodation will be available near the university. For further information and registra- tion of a contribution or participation at the symposium please write to Professor M. Khater, Chemistry Department, Cairo University, Giza, Egypt, or Profes- sor M. Grasserbauer, Technical Univer- sity, Getreidemarkt 9, A-1060 Vienna, Austria. Second Karlsruhe International Confer- ence on Analytical Chemistry in Nuclear Technology June 5-9, 1989, Karlsruhe, FRG This conference will be held in the Kern- forschungszentrum, Karlsruhe.The ses- sions will be: New Developments in Analytical Methods, Automated Analy- sis, In-line and Non-Destructive Analysis, Uranium and Plutonium Analysis, Specif- ications, Quality Control and Standards and Safeguards, Surface Analysis, Trace Analysis of Radionuclides in the Environ- ment, Analysis of Conventional Impuri- ties and Organic Degradation Corn- pounds, and General Session. The dead- line for abstracts is February 15, 1989. For further details contact Professor Dr. Hans J. Ache, Kernforschungszen- trum Karlsruhe, Institut fur Radio- chemie, Postfach 3640, D-7500 Karlsruhe 1, Federal Republic of Germany. Transducers '89 June 25-30, 1989, Montreux, Switzerland The fifth in this series of conferences will be held in Montreux.Papers on the following topics will be considered. General: physical and chemical effects, basic concepts, standards, calibration and application areas. Sensor technology: thin and thick film deposition, silicon process- ing, micromachining , glass fibre technol- ogy and ceramics. Interface electronics: low-noise amplification, offset correction, A/D conversion, multiplexing, frequency output, bus systems and microprocessors. Radiation sensors: photodiodes, photo- conductors, CCDs, nuclear radiation and X-ray sensors and IR detectors. Mechan- ical sensors: pressure sensors, accelero- meters, force sensors, angle sensors and position sensors. Temperature sensors: thermistors, thermocouples, temperature sensitive diodes, transistors and circuits, thermopiles and pyroelectric devices. Magnetic field sensors: Hall-effect dev- ices, superconducting devices, magneto- resistors, magnetodiodes, magneto- transistors, SQUIDS and MAGFETs. Chemical sensors: ion sensors, gas sen- sors, humidity sensors, CHEMFETs, SAW chemosensors and biosensors. Actuators: piezoelectric devices, mag- netic recording heads, thermal print heads, micromechanical devices, micro- motors, microvalves and micropumps. For further information contact Trans- ducers '89, Secretariat, COMST S.A., P.O. Box 415, 1001 Lausanne 1, Switzer- land.

ISSN:0144-557X    

DOI:10.1039/AP9882500205

出版商:RSC    

年代:1988

数据来源: RSC