摘要:

of the Analytical Division ofThe Chemical SocietyCONTENTS295 Summaries of Papers295 Annual Chemical Congress: 'Analysisin the Energy Industries'31 0 'Sampling-Problems and Solutions'312 Equipment News31 5 Chemical Society Library31 6 Portable Oxygen Monitors320 Obituaries320 Revision of British Standardson pH, pHMeters and GlassElectrodes320 Conferences and Courses321 Publications Received324 Analytical Division DiaryVolume 13 No 10 Pages 295-324 October 197PADSDZ 13(10)295-324(1976)ISSN 0306-1 396October 1976PROCEEDINGSOF THEANALYTICAL DIVISION OF THE CHEMICAL SOCIETYOfficers of the Analytical Divisionof the Chemical SocietyPresidentD. W. WilsonHon. SecretaryP. G. W. CobbSecretaryMiss P. E. HutchinsonHon. Treasurer Hon.Assistant SecretariesJ. K. Foreman D. I. Coomber, O.B.E.; D. C. M. Squirrel1Editor, ProceedingsP. C. WestonProceedings is published by The Chemical Society.Editorial: The Director of Publications, The Chemical Society, Burlington House, London, W1 V OBN.Telephone 01 -734 9864. Telex 268001.Subscriptions (non-members): The Chemical Society, Publications Sales Office, Blackhorse Road, Letch-worth, Herts., SG6 IHN.Non-members can only be supplied with Proceedings as part of a combined subscription with The Analystand Analytical Abstracts,0 The Chemical Society 1976Off i ci a 1,Standardised andRecommendedMethods of AnalysisSECOND EDITION (1 973)Compiled and Edited forTHE ANALYTICAL METHODS COMMITTEEofb yThe Society for Analytical ChemistryN. W. Hanson, BSc, PhD, FRICPp. xxiv + 897 €17.00; U.S. $42.50ISBN 0 85990 704 XObtainable from The Publications Sales Officer,The Chemical Society, Blackhorse Road, Letchworth, Herts., SG6 1 HNMembers of the Chemical Society are entitled to buy one copy fortheir own personal use at the special price of f14.50 ( U S $36.50)provided they order direct and enclose remittance

ISSN:0306-1396    

DOI:10.1039/AD97613FX034

出版商:RSC    

年代:1976

数据来源: RSC

摘要:

Octobev, I976 ANALYTICAL DIVISION DIARY 323in the Protection of the Environment.” €3€’ Refinery, Grangemouth.Analytical Division Diary, continuedNovember, continued“Analytical Isotachophoresis-A NewApproach to Analytical Problems,” byH. D. Fairley.“lsotachophoretic Analysis of Muscle Ex-tracts,” by R. C. Woledge and I). Gower.Scientific Societies Lecture Theatre, 23 SavileRow, London, W.l.Thursday, 18th, 6.30 p.m.: KirkbyNorth West Region, jointly with the Liverpooland District Section of the CS.“The Chemical Control of Colour Photo-graphic Processes,” by G. I. P. Levenson.Kodak Ltd., Kirkby, nr. Liverpool.Thursday, 18th, 6.30 p.m.: LondonBiological Methods Group : Annual General“Rabies,” by G. S . Turner.New Savoy Tavern, Savoy Street, London,w.c.2.Thursday, 18th, 10.00 a.m.: Milton KeynesMeeting.Radzochemical Methods Group : AnnualGeneral Meeting and meeting on “Design andSafety in the Radiochemical Laboratory.”Welcome by Ilr. J . L). Coombes, ResearchDirector, Hoechst Pharmaceutical ResearchLaboratories.“Experiences in 12adiochemical LaboratoryDesign,” by D. Hughes.“Design of Animal Houses for RadioactiveWork,” by T. E. I;. Carr.“Safety of Workers in Radioactive Areas,” byH. D. Evans.“l,egislative Attitudes,” by S. Luxon.“Safety Considerations in the Production ofTiadiopharmaceuticals,” by K. Friihauf.“Design Features in the Hoechst Laboratories,Milton Keynes,” by R. Andrews.The meeting will include a tour of theLzboratories.Hoeclist Pharmaceutical Iiesearcli Labora-tories, Walton Manor, Walton, MiltonKeynes, Bucks.Friday, 19th, 6.30 p.m.: ChepstowWestevn Region.Discussion on “Industrial Hygiene andAnalytical Chemistry because of theHealth and Safety Act,” to be introducedby N . Pearce.Miye Room, George Hotel, Chepstow.TIzevvnal Methods Group : Annual GeneralMeeting and meeting on “Thermal MethodsFriday, 19th, 10 a.m.: BathSpeakers to include: J . P. liedfern, A. A.Hodgson, L. S. Bark and C. J . Keattch.University of Bath, Claverton Down, Bath.Midlands Regzon : Annual General Meeting,followed by a Joint Meeting with theBiological Methods Group.“Alternatives to liadioimmunoassay,” byJ . Bridges.Lecture Theatre, The Boots Co. Ltd., Penny-foot Street, Nottingham.Tuesday, 23rd, 6.15 p.m.: NottinghamThursday, 25th, 2.15 p.m.: CambridgeEast Anglza Region : Annual General Meeting,followed by a meeting on “Analysis forPlant Breeding.”“Quality Components of Some AgriculturalCrops,” by E.T. Whitmore.“Analytical Techniques in Wheat Assess-ment,” by Miss E. M. Nicholas.“Quality Assessment in Sugar Beet,’’ byW. Woodwark.Research and Technology Centre, SpillersI,td., Station Road, Cambridge.Tuesday, 30th, 2.15 p.m.: LondonA tomic Spectvoscopy and Particle Size Anal~IsisGroups : Annual General Meetings, followedby a Joint Meeting on “Sampling.”“The Sampling of Heterogeneous HulkSolids,” by R . Smith.“Powder Sampling in the Laboratory,’’ byM. W. G. Burt.“Sampling, Grinding and Particle Size Effectsin Analysis,” by A.E. Smith.“Atmospheric Sampling in the IJrban En-vironment,” by D. J . Ball.Lecture Theatre, Geological Society, Burling-ton House, Piccadilly, London, ‘j7v. 1.Tuesday, 30th, 10.30 a.m. : GrangemouthChvovnatography and Electvophovesis GvouP :Annual General Meeting and Joint Meetingwith the Scottish Region and the Chroma-tography Discussion Group on “Ga.;Chromatography in the Oil Industry.”“Measuring Men’s Exposure to PetroleumVapours During Processing and Trans-portation,” by D. T. Coker.“The Use of Molecular Sieves for Analysis ofPetroleum,” by N. G. McTaggart.“Quantitative Analysis of Petroleum f’ro-ducts by Gas Chromatography,” by A. G.Butlin.“A Baseline Study of Hydrocarbons in SeaWater,” by P.John.“Some Aspects of Gas Chromatography inPetroleum Prospecting,” by A. G. I>ouglasAnalytical Division DiaryOCTOBERThursday, 21st, 2.30 p.m.: LondonBiological Methods Group on “Replacement ofthe Therapeutic Substances Regulations :Compendium on Biological Substances.”This meeting has been postponed.Thursday, 21st, 2 p.m.: LondonJoint Phavmaceutical Analysis GvouP on“New Techniques in Thin-layer Chromato-graph y . ”“The Latroscan TH 1 0-An Advance inQuantitative TLC,” by A. Stafford.“The Application of Mass Spectrometry in theIdentification of Drug Impurities Resolvedby TLC,” by B. Millard.“The Technique and Application of Thin-layer Gel Filtration,” by E. A. Hill.The Hall, Pharmaceutical Society of GreatBritain, 1 Lambeth High Street, London,SEl 7JN.Friday, 22nd, 5 p.m.: ExeterWestevn Region, jointly with the PeninsulaSection of the CS.“Carbon Furnace Atomic-absorption and-emission Spectrometry,” by J.M. Ottaway.Newman Building, The University, Exeter.Thursday, 28th, 10 a.m. : MiddlesbroughNovth East Region and Atomic SpectvoscopyGvouP on “Sources for Emission Spectro-scopy.”Introduction by A. A. Smales.Plenavy I<ectuve : “Is Optical Emission Spec-trometry Being Tailorcd to the Require-ments and Budgets of a Large Variety ofUsers?” by P. W. J. M. Boumans.“Fast Optical Emission Analysis of Metals-Two Points of View,” by K. Slickers.“Improving the Performance and Speed ofAnalysis by Triggered Capacitor Dis-charges,” by N.Kemp.“Some Aspects of Spectroscopy with Induc-tively Coupled Plasmas,” by S. Greenfield.“Some Recent Studies with a MicrowavePlasma Source of Multi-element DetectionSystems,” by G. F. Kirkbright.“Development of Glow Discharge EmissionSpectroscopy for Application in the SteelIndustry,” by A. Butterworth.Cleveland Scientific Institute, CorporationRoad, Middlesbrough.Thursday, 28th, 10.30 a.m.: LeatherheadSouth East Region on “Chemistry in thePackaging Industry.”“The Role of PIRA and the Facilities andServices it Offers to Industry,” by F. A.Paine.“Matching the Packaging to the Product,” byH. Adcock.“The Determination of Traces of VinylChloride in Various Media,” by J . T. Davies.“Some Aspects of Chemistry in PrintedPackaging Manufacture,” by E.W.Peacock.Research Association for the Paper andBoard, Printing and Packaging Industries(PIRA), Randalls Road, Leatherhead,Surrey.NOVEMBERThursday, 4th, 6.30 p.m.: LondonMicvochemical Methods and ElectvoanalyticalGroups.Discussion on “The Practical Use of Ion-selective Electrodes,” to be introduced byA. G. Fogg.The Savoy Tavern, Savoy Street, London,w.c.2.Friday, 5th, 5 p.m.: GlasgowScottish Region : Annual General Meeting.“British Contributions to Atomic Spectro-scopy in the Last 250 Years,” by ProfessorT. S. West.Thomas Graham Building, University ofStrathclyde, Cathedral Street, Glasgow.Analytical Division on “Isotachophoresis andLecture on “Isoelectric Focusing,” byWednesday, loth, 10.15 a.m. : LondonIsoelectric Focusing.”J . S. Fawcett.Postev Pvesentations“Detection of Soya Protein by IsoelectricFocusing,” by J. W. Llewellyn.“The Use of Isoelectric Focusing in a System-atic Strategy for Protein Purification,” byH. D. Leaback.“Analysis by Isoelectric Focusing of Phospho-glucoseisomerases in Schistosoma Speciesand their Snail Hosts,” by G. C. Ross.“Some Comparisons Between Different Typesof pH Gradients used for IsoelectricFocusing,” and “Continuous Flow Iso-electric Focusing,” by J . S. Fawcett.Lecture on “Some Remarks on AnalyticalIsotachophoresis,” by F. M. Everaerts.“The Use of the Antimony Electrode forDetermination of Isoelectric Points,” by J . A.[continued inside back coverPostev PvesentationsBeeley .Printed by Heffers Printers Ltd Cambridge Englan

ISSN:0306-1396    

DOI:10.1039/AD97613BX036

出版商:RSC    

年代:1976

数据来源: RSC

摘要:

Proceedings of the Analytical Division of the Chemical Society ANNUAL CHEMICAL CONGRESS The Annual Chemical Congress of The Chemical Society and Royal Institute of Chemistry was held at the University of Glasgow from April 5th to 9th, 1976. Two Symposia were organised by the Analytical Division and summaries of the papers given at Symposium B, Analysis in the Energy Industries, are presented below.Summaries of some of the papers given at Symposium A, Developments in Analytical Atomic Spectrometry, appeared in the September issue of Proceedings (p. 258) and the Fifth Tlieophilus Redwood Txcture by Professor R. Belcher was published in full in the June issue (€1. 153). Analysis in the Energy Industries The following are summaries of seven of the papers presented at the Annual C,hemical Congress on April Sth, 1976.Analytical Developments in the Nuclear Industry V. M. Sinclair Dounveay Experimental Reactov Establzshment, United Kingdom Atomzc Enevgy Aidhovify, Thwso, Caithness The nuclear energy industry in the UK is concerned with the manufacture and re-processing of nuclear fuels for power reactors, the development of nuclear systems for power production ie.g., the steam generating heavy water reactor (SGHWR) and the liquid metal cooled fast breeder reactor] and the underlying research in nuclear energy. In all of these fieldsthe analytical chemist is playing a vital role, using his professional skill and developing tecliniques to ensure the efficient, effective and economic application of the optimum analytical procedures to the problems that are encountered.In the fuel fabrication and re-processing fields, the major developments in analysis have been directed to improving and increasing on-line instrumentation and to the computerisation of laboratory instruments. I t has been noticeable that the on-line instrunientation has tended to involve simple but robust techniques such as y-absorptiometers, ion-selective electrodes and attenuation of ultrasonics, to monitor the performance of intermediate sections of the plant rather than the use of complex instrumentation to determine chemical species in a waste or final product stream.Automatic analysers in the laboratories have had only a limited application in these fields. The development of the fast reactor system for power production has necessi- tated improvements in methods of analysis for plutoniuni in process streams of both fuel fabrication and re-processing plants.The application of on-line methods has proved to be more difficult in this area because of the greater complexity of plutonium processing and because consideration of criticality has limited the size and dictated the shape of processing equipment.On-line analysers have played a major role in the control of the chemistry in the water circuit of the SGHWR and there has been continuing development of these instruments over the last few years. The developments that have been reported by workers at the ‘CTKAEA’s establishment at Winfrith have included the on-line measurement of dissolved gases in the reactor coolant by automatic gas chromatography and the use of the Technicon analyser in an on-line analyser for determining boron in the heavy-water circuit.Laboratory automatic analysers have been used to supplement these on-line analysers. On the fast reactor the analyst’s attention has been concentrated on the problems associated with the control of the 295296 ANALYSIS IN THE ENERGY INDUSTRIES Proc.AnaZyt. Div. Chem. Soc. sodium coolant. Chemical methods of analysis continue to play an important role but sampl- ing of the very “hot,” both radioactively and thermally, liquid sodium is time consuming and involves complicated equipment on the reactor. The subsequent analyses often have to be carried out remotely and in facilities with inert atmospherics.Such measurements call for exceptional skill on the part of the analyst. On-line techniques, largely based on electro- chemistry, are beginning to play a major part in the control of these circuits, especially for the measurement of non-metallic impurities, oxygen, hydrogen and carbon, which are present to the extent of a few parts per million. Equipment that is compatible with the liquid sodium is being developed by the UKAEA at Harwell and DERE and by the CEGB at the Berkley Nuclear Laboratories.Oxygen meters based on e.m.f. measurements with a solid-oxide electrolyte and a solid-oxide reference electrode are being developed and tested. Carbon meters based on the equilibration of carbon from the sodium with iron and then the measurement of its potential with respect to an iron - iron carbide reference electrode have also been developed.Qther carbon measuring devices are also being tested in the Prototype Fast Reactor at DERE. Accounting accurately and precisely for nuclear material in laboratories, plants and reactors has always been a requirement in the UK. Various improvements have been achieved over the last few years and when, in more recent times, the UK became subject to nuclear safeguards under Euratom, the analytical procedures for accountancy met all the requirements of the independent inspectors.Measurements of nuclear material in waste streams from nuclear processes have been improved as the technology of the nuclear industry has advanced. Greater sensitivity and greater accuracy have been achieved even as the waste streams become more complex.The health and safety of employees and the general public are of prime concern to employers and the nuclear industry is no exception in this respect. Improved methods of bioassay have been developed to deal with radioactive nuclides. These improvements have yielded more sensitive and robust methods for the assay of plutonium and other transuranic elements in biological samples.In the underlying research of the nuclear industry there is a continuing requirement for new analytical procedures and many papers have been written that deal with them. The most noteworthy of these procedures involve the wider use of proton and particle activation techniques. Workers at AERE, Harwell, have been developing both gamma and charged- particle activation techniques, especially for the measurement of non-metallic elements in steel, etc.A nuclear microprobe has been designed, which permits the measurement of the distribution of elements such as carbon, oxygen and nitrogen in steels. A general trend in the nuclear industry over the past few years has been the consolidation of earlier development work and the use of analytical procedures in an increasingly commercial and industrial environment.The need to have effective control in large fuel fabrication and irradiated fuel re-processing plants will lead to increasing development of on-line equipment for control and measurement. Analysis in the Electricity Supply Industry G. I. Goodfellow Centval Electvicity Reseavch Labovatovies, Kelvin Avenue, Leathevhead, Suvvey, KT22 7 s E The electricity requirements within the UK are met by several nationalised electricity under- takings.In terms of generated power, the CEGB is by far the largest of these undertakings, and although this paper is specifically concerned with the work of the analyst in this organi- sation it undoubtedly reflects much of the work in other parts of the UK supply industry. It may not be immediately apparent why a predominantly heavy engineering industry producing electrical energy should require the services of analysts. However, there are in fact many different types of work in which analysts are engaged, and it is the aim of this paper to illustrate some of the aspects of this work on the operations side in power stations and to highlight some of the recent developments and applications of analytical techniques.The term “analyst” is used in its broadest sense to include not only professional chemists, but also personnel from other scientific disciplines who are engaged in the qualitative andOctobev, 1976 ANALYSIS IN THE ENERGY INDUSTRIES 297 quantitative characterisation of the composition of materials.There are three principal sectors of the CEGB in which analysts are employed: (1) the Power Station Chemistry Departments, of whichthere are about 140; (2) the laboratories of the Scientific Services Departments (SSD) of the five geographic Regions; and (3) the three laboratories of the Research Department, vix., the Berkeley Nuclear Laboratory (BNL) , Central Electricity Research Laboratory (CERL) and Marchwood Engineering Laboratory (MEL).The analytical work in the Station laboratories is essentially of a regular day-to- day nature, the prime purpose of which is to maintain the efficient generation of electricity. In the Regional SSD and the Research Department laboratories, not only are personnel involved in service analyses to support investigational teams but there is also considerable effort allocated to research into new analytical procedures and techniques. Considerable use is made of instrumentation in power stations both on-stream for con- tinuous monitoring and in the laboratory for discrete sample analysis. The more specialised instruments, such as X-ray fluorescence, Auger and direct-reading emission spectrometers, are located mainly in the SSD or Research Department laboratories.Power Station Analyses The scope of regular routine analyses varies from station to station and depends, ivttev alia, on the individuality of station design, the location of the station and availability of local resources (such as water supplies) and the operational management of the station. However, taking all types of station into consideration, the routine monitoring of the steam and water circuit, either by manual laboratory analysis or by on-stream instrumentation, probably constitutes one of the larger demands on the analytical effort.In modern boilers with pressures up to 2 400 lb in-2, giving superheated steam temperatures of about 560 “C and boiler water temperatures of about 350 “C, there exist highly reactive fluid media in which corrosion of the various containment materials and system components can readily take place, unless strict control of the purity of these media is maintained.Water from the treatment plant being fed into the boiler feed system is very pure, having a conductivity generally within the range 12-20 pS m-1 at 20 “C; this value can be com- pared with the “classical” value of 5 pS m-1 reported by Kohlrausch and Heydweillerl for “absolutely pure” water.Although water of this purity enters the plant, “aggressive” and “unwanted” species invariably “leak” into the steam - water system because of structural deficiencies in various parts of the plant, and cause corrosion of the containment materials.For example, chloride can arise from ingress of condenser cooling water, and oxygen from the atmosphere can enter into the circuit, particularly within the vacuum section of the condenser system. To nullify the deleterious effects of such contamination, very low concentrations of certain substances are introduced : ammonia and sodium hydroxide to produce an alkaline environment (pH 9-9.5) in the boiler, and hydrazine to reduce residual oxygen after the de-aerator.In addition, impurities such as silica in the steam can be deposited on turbine blades and cause a decrease in efficiency. The operational concentrations in a modern 2 350 lb in-2 (160 bar) boiler at which some impurities and additives are maintained and for which regular analyses are necessary are shown in Table I. The principles for the analyses of these species are mainly based on those TABLE I CONCENTRATIONS OF IMPURITIES AND ADDITIVES Impurities and additives Water or steam Feed-water Boiler water Steam Feed-water , I Type Species Concentration/mg 1-1 Impurities 0 2 < 0.005 < 0.020 c1 <0.013 Fe -t Cu + Ni Additives SiO, < 0.02 N,H, 0.01-0.1 NH, 0.1-1.0 Na <0.005298 ANALYSIS IN THE ENERGY INDUSTRIES PYOC.A.tzaZyt. Dizr. Chenz. SOC. of spectrophotometry and electrochemistry (particularly potentiometry) . Atomic-absorption spectrometry is also used in the larger power station laboratories for determining metallic impurities. These various techniques are favoured because they are capable of good selec- tivity, a high degree of sensitivity and in general are simple in their application.The measurement of conductivity has been universally employed for many years because, although non-specific, it provides a very reliable means of assessing the general ionic quality of the water. Whether the analysis for the various species is carried out in the station laboratory or with instrumentation within the plant itself is to a considerable extent at the discretion of individual station management.However, much of the pH, conductivity and oxygen measurement for control purposes is carried out instrumentally, because of the difficulties of collecting and transporting discrete samples from the plant to the laboratory without incurring contamination from components of the atmosphere.Apart from the analysis of the steam - water circuit and the ancillary water systems such as cooling water and raw water supplies, the Station Chemistry Department carries out regular analysis associated with other functional parts of the station. At nuclear stations, the carbon dioxide coolant is monitored for impurities such as water vapour, carbon monoxide, methane and hydrogen using gas-chromatographic, infrared and hygrometric techniques. Similar techniques are used in the monitoring, for water vapour and air, of the hydrogen coolant gas in high-power alternator systems.In fossil-fired stations, instrumental measure- ments of carbon monoxide and oxygen are made in order to assist in the control of com- bustion conditions within the boiler. The analysis in fossil-fired stations of coal and fuel oil for such parameters as calorific value, ash content and moisture is required for the calculation of efficiency values, although nowadays much of this analysis is actually carried out in central SSD laboratories.However, other types of oil used for lubrication and insulation are regularly examined in station laboratories, applying standardised procedures such as those proposed by the Institute of Petroleum. The above is a necessarily abbreviated account of some of the diverse analytical work in power station laboratories.In the next section, a few examples are given of recent analy- tical research activities; they are mainly examples of combined work between SSD and Research Department laboratories.Analytical Research and Development Analysis of High-purity Water An industrial instrument, which is now being commercially manufactured under licence to the CEGB, has been developed for the continuous potentiometric determination of chloride in the range 1-150 pg 1-1,2 its principal application being to monitor feed-water systems. A chloridised silver rod is used as the sensing electrode and the sample stream is buffered to pH 4.7 by addition of ammonium acetate to eliminate the formation of silver hydroxide, which would otherwise occur with sample streams of high pH.Below approximately 5 mg 1-1 of chloride, the Nernstian response of e.m.f. ueYsus log [Cl] is no longer linear because of the contribution to the total chloride ions at the electro- active surface by dissolution of the silver chloride itself.The effect of this is that in the range 1-150 pg 1-1 of chloride the e.m.f. becomes directly proportional to chloride concentra- tion in the sample stream with a sensitivity at 25 "C of only about 2.3 mV per 10 pg of chloride per litre. Notwithstanding this basic problem, the technique has been successfully utilised by careful attention to a number of factors that affect noise and long-term drift.The solu- tion temperature in the potentiometric cell is controlled to within *0.1 "C and is also de- creased to 10 "C to decrease the solubility of the silver chloride. The silver chloride electrode in the flow cell is shielded from extraneous light, and earth loops are eliminated. By stan- dardising every 2 h, any errors from drift are minimised. The blank water for setting the zero is provided from a supply of water continuously re-circulated through a deionisation system, the latter being an integral part of the instrument.While such potentiometric techniques permit the direct measurement of certain species at the microgram per litre level there are some determinations that will be required for "once- through" boilers of AGR stations for which no direct measurements can as yet be envisaged.For example, it is expected that measurements of sulphate in the range <1-50 pg1-I onOctober, 1976 ANALYSIS I N THE ENERGY INDUSTRIES 299 condensed steam after ion-exchange polishing will be necessary. Although a sensitive colorimetric method for direct analysis has been recently developed at CERL, its limit of detection is only 50 pg 1-l.A simple means of increasing the sensitivity of this measurement has been devised, in which the sulphate ions from a large volume of sample (1-10 1) are ab- sorbed by filtration (under suction) on to a pair of thin discs of anion-exchange material plac'ed one above the other. The sulphate ions are then eluted with a small volume of dilute perchloric acid, and determined directly by the colorimetric method referred to above.The discs, left in the perchlorate form, can be used repeatedly for the analysis of other samples. A standard deviation of about 0.4 pg of sulphate can be obtained over the range 2-10 pg with a limit of detection of about 1 pg. Using 10-1 portions of sample, the sulphate content of laboratory deionised water has been found to be about 0.2 pg 1-1.Hydrogen Coolant Analysis Although large, 500-MW alternating generators are cooled by a re-circulatory gas stream, currents induced within the system can cause temperatures to rise locally, which, if excessive, will accelerate the thermal degradation of the insulating materials that are an integral part of the generator construction.Eventually, the insulation can fail completely, causing internal arcing, which, under extreme circumstances, can result in serious damage and com- plete break-down of the alternator. Most insulators contain some type of organic resin, which, when heated, will give rise to a variety of volatile degradation products. When hot spots occur in the alternator system, these products will accumulate in the hydrogen gas used as the primary coolant.This effect has led to the proposition that monitoring the gas for specific degradation products might provide an early warning of potential electrical break- down conditions. A large programme of work is currently in progress to test the validity of this proposition. The analytical work involved can be divided into three stages: (1) the correlation of volatile break-down products with specific insulating materials heated to various temperatures ; (2) a survey of coolant gas from different generator systems from a number of different CEGR stations to establish background levels of volatile organic species; and (3) the establish- ment of any relationship between abnormal concentrations of selected volatile species and electrical fault conditions. The application of coupled gas chromatography - mass spectrometry to the work in stage (1), using specimens of insulating materials heated under controlled laboratory conditions in hydrogen, has given firm evidence of the correlation of certain degradation products with specific insulating materials.However, in stage (2), from the purely analytical viewpoint, one of the greatest difficulties is that the concentrations of degradation products in the hydro- gen are not high enough for direct gas-chromatographic examination. This problem has been largely solved by using pre-column devices for concentrating the impurities from a large volume (typically 3 1) of hydrogen coolant, and subsequently eluting and analysing by gas chromatography.By passing hydrogen coolant directly from the alternator system at 100 ml min-l through pre-columns of either Porapak T cooled to -78 "C or Tenax GC at ambient temperature, ali- phatic and aromatic species whcse boiling-points span a wide temperature range are absorbed. After absorption, the pre-columns are transferred to the laboratory and separately connected to a gas chromatograph with analytical columns of either Porapak Q + Porapak T (for the Porapak T pre-column) or of Tenax GC (for the Tenax GC pre-column).The absorbed species are quickly released from the pre-column by heating rapidly to 150-200 "C and flushing into the gas chromatograph with helium. A combination of isothermal and tem- perature-programmed sequences is used for the analysis of either of the two pre-columns.Although the over-all programme has yet to be completed, much more is known about the chemical purity of hydrogen coolant systems than hitherto. This information should materi- ally assist in predicting impenidng faults in alternators and thus enable steps to be taken to avoid major electrical failures and the resulting costly repairs. Conclusion In this paper it has been possible to discuss in detail only a few of the analytical activities in However, there are many other areas, including liquid the electricity supply industry.300 ANALYSIS IN THE ENERGY INDUSTRIES PYOC.Analyt. Div. C h e ? ~ . SOC. metal coolants, environmental studies, biochemistry and radiochemistry, in which a variety of analytical techniques are widely used, but because of considerations of space it has not been possible to mention them.I acknowledge the assistance of many colleagues in the CEGB who have provided infor- mation for inclusion in this paper, which is published by permission of the Central Electricity Generating Board. References 1.2. Kohlrausch, F., and Heydweiller, A., Z.Phys.Chern., 1894, 14, 317. British Patent Application No. 31046/74, 12 July, 1974. Progress in Analysis in the Solid Fuel Industry H. C. Wilkinson British Carbonization Reseavch Association, Chestevfield, Devbyshive, S42 6 J S Coal, and the solid products derived from it by heat treatment, represent a considerable proportion of the various sources of energy available to mankind and the control of the quality of these materials is of paramount significance from both technical and economic considerations. The analysis carried out on solid fuels is thereby concerned with the deter- mination of the amounts of those materials present which affect its use under industrial con- ditions, for example the amount of sulphur present in coke has important repercussions on blast-furnace operation and the amount of ash present in a fuel detracts from its potential heating value.The complex nature of these fuels, and the fact that they are produced and consumed in large amounts, makes it essential that the relatively small amounts required for analysis are fully representative of the gross sample; consequently, the sampling of coal and coke is a science in its own right and careful schemes of sampling must be followed to ensure that the analytical results obtained are meaningful. The heterogeneous nature of solid fuels and the differences in their properties when compared with those of liquid or gaseous fuels have an important impact on the methods adopted for their analysis.The analysis of solid fuels is generally divided into two broad subdivisions, known as proximate and ultimate analysis.In the former group, considerable use is made of empirical tests, for example in the determination of moisture, ash and volatile matter. These tests are naturally carried out under strict regimes of sample mass, particle size, temperature and duration of the test. They are simple, easily adaptable to batch analysis and they have stood the test of time.Therefore, there has been little development of these well established methods until the last decade, when there has been a move towards the use of continuous or automated tests, suitable for monitoring the quality of material used in a continuous process such as coal washing or coal carbonisation.Ultimate analysis involves the determination of the amounts of the major elements present, such as carbon, hydrogen, nitrogen, oxygen and sulphur. Additionally, determinations of chlorine and phosphorus are frequently made and a knowledge of the arsenic content is sometimes required. Most of these determinations are still based on the use of classical systems of gravimetric, volumetric and colorimetric analysis, but new techniques are beginning to be employed in certain instances.A continuous method for the measurement of the moisture content of coal that is being successfully used on an industrial scale1 is based on the principle that there is a significantly large difference between the dielectric constants of water and coal which is demonstrated by the extent to which microwaves, of wavelength about 3 cm, are attenuated by coal and water, respectively.From suitable calibration graphs, a direct reading of the moisture content of coal can be obtained. Continuous methods for the determination of moisture in coke are also in use,2 but because coke is a conducting material techniques based upon nuclear magnetic resonance or neutron scattering are employed.For both coal and coke the methods are The effect of such impurities upon the environment is also significant.Octobev, 1976 ANALYSIS IN THE ENERGY INDUSTRIES 301 subject to interference from various sources, notably particle size, and careful control must be maintained over such parameters so as to ensure satisfactory precision of the methods.Developments in the determination of ash have largely been concerned in reducing the time taken by the traditional methods, but alternative approaches are now available3 in which use is made of the difference in the amount of short-wave radiation (X-rays or y-rays) that is scattered or absorbed by the carbon and mineral matter, respectively, in the coal. This difference can be used to measure the ash content of the coal.No corresponding method has as yet been developed for the continuous measurement of ash in coke, but a laboratory method is available that enables a determination to be made in about 20 min.4 Rapid laboratory methods based on traditional combustion, absorption and titrimetric techniques are used for the determination of sulphur, or sulphur and chlorine, in solid fuels.They are simple, eminently suitable for routine use and can be completed within 15 min. Under these conditions there is little impetus to develop sophisticated methods of analysis, but some work has been carried out using X-ray fluorescence5 for the determination of sulphur. For a suite of 32 coal samples, ranging in sulphur content from 0.3 to 3.7%, the mean difference between the results obtained by X-ray fluorescence spectrometry and by a classical method was 0.02%.The major elements present in coal, namely carbon, hydrogen and nitrogen, are determined by classical combustion methods (carbon and hydrogen) or by a Kjeldahl method (nitrogen), the last method being used on the semi-micro scale. The traditional Liebig method has been replaced by the much more rapid Sheffield high-temperature method,6 an actual determination by this method (apart from the cooling period required after the test) taking only 10 min.The refractory nature of the ring-nitrogen present in coke poses some problems when using the Kjeldahl method and in recent years commercial carbon - hydrogen - nitrogen analysers have been used for the determination of these three elements.Although the precision of these determinations may not match that obtainable by the classical methods, which are a good test of the analyst’s skill, they are adequate for routine use. Oxygen determinations in solid fuels are rarely undertaken, as it is difficult to apportion the total amount of oxygen released between that in organic combination with the coal and that present in various inorganic forms in the mineral matter, both being liberated on combustion.Oxygen can be determined by a modified Unterzaucher method using a titrimetric or conduc- timet ric finish. Neutron-activation methods have been applied to this determination8 but again they do not distinguish between the different forms of oxygen present.An acceleration in the speed at which phosphorus determinations can be made was recently de~cribed.~ It employs the Schoniger flask as the combustion unit followed by reduction of the molybdophosphate with ascorbic acid and potassium antimony1 tartrate. A determination can be completed in 45 min and the results show excellent agreement with those determined by a standard procedure.Optical methods are now playing a much greater part in the assessment of coal rank and the measurement of the different rock types present in coal. These data provide a valuable insight into certain aspects of coal behaviour and are the subject of development work to enable them to be used as a means of continuous quality control. A further approach using an instrumental technique has utilised the difference in the electri- cal conductivities of coal and coke to determine the amount of fine coke less than 0.5 mm in size, which is sometimes added to a coke oven charge to improve coke quality.1° Finally, perhaps the most widespread use of modern analytical techniques in the field of solid fuel analysis arises from the recent awareness of the possible effects upon the environment of trace elements released during the utilisation of solid fuels.About 60 elements have been recognised in solid fuels and methods for the determination of the more volatile of those ele- ments, e.g., antimony, arsenic, boron, fluorine, germanium, iodine, mercury and selenium, are currently the subject of considerable research. Those methods tried include neutron activa- tion, optical emission, atomic-absorption, X-ray fluorescence and ion-selective electrode techniques.11 Most of these methods suffer from some deficiencies, but opinion appears to be hardening in favour of using atomic-absorption spectroscopy as a general method, with optical- emission spectroscopy as a second choice.The amounts of the elements present are generally very small and careful sampling and sample preparation is essential.While progress in the analysis of solid fuels has been steady, if not spectacular, growing use302 ANALYSIS IN THE ENERGY INDUSTRIES PYOC. Aizalyt. Div. Chewz. SOC. is being made of instrumental methods for monitoring the qualities of feedstock and products and sophisticated analytical techniques are coming into prominence for the analysis of trace elements and substances of importance in relation to the quality of the environment.1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. References Hall, D. A., Sproson, J. C., and Gray, W. A., J . Inst. Fuel, 1972, 45, 163. Dartnell, J., J . Iron Steel Inst., 1972, 210, 145. Crossland, R., et al., 9th Commonwealth Mining and Metallurgical Congress, 1969, Paper 24.Relcher, R., and Spooner, C. E., Fuel, LoNd., 1944, 23, 46. British Coke Research Association, Coke Res. Rep., 1972, No. 71. Mott, R. A., and Wilkinson, H. C., Fuel, Lond., 1955, 34, 169. Kirk, B. P., and Wilkinson, H. C., Talanta, 1970, 17, 475. Bate, L. C., Nucleonics, 1963, 21, 72. Kirk, B. P., and Wilkinson, H. C., Talanta, 1972, 19, 80. Moulson, I., Sullivan, G., and Wilkinson, H.C., Fuel, Lond., 1976, 55, 148. Ruch, R. R., Gluskoter, H. J., and Shimp, N., ISGS Etzuiv. Geol. Note, 1974, No. 7 2 . Analysis in the Petroleum Industry A. Quayle Shell Heseavch Ltd., ThovvLtovz Reseavch Cevztve, P.O. Box 1, Chestev, CHI 3SH Although this paper was part of the Symposium on “Analysis in the Energy Industries,” it was assumed that conservation of energy was just as important as its conversion by burning fossil fuels, and hence analytical problems of lubrication were included.The progress of petroleum was followed from production from the ground, through transportation and refining, to its final end-use by the consumer. Analysis associated with the initial production phase was illustrated by the determination of the composition of a reservoir fluid.This involved the use of gas chromatogradhy to deter- mine the molar composition of various liquid fractions and the gases in equilibrium with them, the components ranging from methane to pentacosane. Marine transportation can offer a variety of operafional problems, including those of boiler efficiency. X-ray diffraction analysis of deposits on superheater tubes (withdrawn during dry-docking) can give information about the temperature regime to which they have been subjected.Thus, the sodium vanadyl vanadate (5Na20.V20,.11V,0,) is formed only above 660 “C, and if its presence in the deposits is shown by X-ray diffraction, flame impingement on the tubes may be suspected and a check made of the oil burners. It may be necessary to identify the source of an ocean spillage, and a comparison of a vessel’s cargo or bunkers with an oil pollutant might be needed.Our experience is that, in order to avoid errors, it is desirable to obtain several different types of analytical results. For example, gas chromatograms of the hydrocarbons of pollutant and reference, determined with a flame-ionisation detector, may be similar but (as in the example presented) the sulphur compounds, determined with a flame-photometric detector, may be different.Additional evidence may be gleaned from the concentrations of the isoprenoids pristane and phytane (by high-resolution gas - liquid chromatography) or from the nickel to vanadium ratio (by emission spectrography) . Analysis in the refinery has four main purposes: to ensure that the plants are running efficiently and economically; to ensure that the products meet the required specifications; to protect the environment from undesirable discharges; and to carry out trouble-shooting if or when things go wrong.On-line automatic analysers (quality measuring instruments) are used extensively. An example presented was that of a continuous octane rating analyser used in the control of gasoline blending.Essentially an automated CFR engine, this gives the octane rating of a flowing stream to *0.15 ON. Gas chromatography is also widely used for on-line analysis of plant streams. Specification properties of petroleum products determined in the laboratory include melting-points of waxes, pour-points of heavier oils and “pene- trations” of bitumen.To reduce labour demands, automatic flash-point apparatus and automatic viscometers are used. Chemical analyses are carried out on boiler water, cooling waters and effluent streams, as well as on products (e.g., chloride in water, cobalt in gasoline,Octobev, 1976 ANALYSIS I N THE ENERGY INDUSTRIES 303 sodium on catalysts, sulphur in “Merox” solution).The list of analyses is not confined to simple tests, however, as emission and absorption spectroscopy, polarography and com- puterised gas - liquid chromatography are used as appropriate. The blending of lubricants containing metallic dispersants is often controlled by atomic-absorption spectroscopy : examples of the apparatus used and the results for the calcium, zinc, magnesium and/or barium contents of lubricating oils were shown.From the consumer’s viewpoint, the product must meet the demanding requirements of more powerful engines and machinery. Changes in petrol engines have been aimed at reducing both fuel consumption and the emission of pollutants. Exhaust gases can be analysed with, amongst other devices, non-dispersive infrared gas analysers or chemiluminescent equipment (for nitrogen oxides).Information on the volatility of a gasoline and on the distribution of anti-knock properties throughout its boiling range is obtained from compositional studies using gas chromatography. Examples were given of a low-resolution chromatogram, ob- tainable in about 10 min, and of a high-resolution trace, containing 275 peaks but requiring li-2 h to complete.Aviation turbine fuels have to meet extremely high standards of cleanliness so as not to block filters in the aircraft or in the airfield distribution system. We have studied the removal of surfactants (which might hold contaminants in suspension) using radio-tracer techniques, employing a sulphur-35 labelled organic sulphonate, an iron-59 labelled iron naphthenate and a tritiated phenolic antioxidant added to the aviation kerosene at the parts per million level.Aviation turbine lubricants are based on synthetic esters (e.g., dioctyl sebacate and penta- erythrityl valerate), incorporating antioxidants and extreme-pressure additives. Anti- oxidant concentrations have been determined by thin-layer or gas chromatography or ultra- violet absorption, but most recently we have found high-performance liquid chromatography to be very effective: it is rapid (a chromatogram takes less than 12 min), sensitive and resolves the various components extremely well.Of interest to many airline operators is the ability to detect the onset of wear in an aircraft engine before it becomes serious enough to ground the aircraft.Emission spectrography is a useful means for determining wear metals in aviation lubricants at the parts per million level, and an analytical report typical of those sent to airlines on a regular basis was shown. Ten elements ranged in concentration from 5 to less than 0.5 p.p.m., but the airline’s attention was drawn to one sample containing 22 p.p.m. of iron and 4 p.p.m of nickel for further in- vestigation. The interaction between lubricants and surfaces is a major subject of research, with the need to reduce gear train or valve and tappet wear in the face of increased loadings.A technique proving valuable in these investigations is X-ray photoelectron spectroscopy (“electron spectroscopy for chemical analysis,” ESCA), which can analyse a very thin film (0.2-0.3 nm thick) on the surface of a metal specimen.Spectra obtained from a metal treated with an extreme-pressure additive, zinc dialkyldithiophosphate, under different conditions were shown. In everyday problems, X-ray techniques are powerful aids in an analytical department. For example, corrosion was observed in a gear pump circulating lubricant to a metal rolling mill.and the oil was suspected to be the cause. However, X-ray diffraction of the corrosion product showed the presence of P-iron(II1) hydroxide, a form of rust normally produced only under acid chloride conditions. Chlorine was confirmed (by X-ray fluorescence) on the surface of the gear bearings, but was not found in the retained sample of the unused lubricating oil. Eventually, it was established that the acid chloride had come from the material that had been used to clean the pipe system and that had not been adequately flushed before re- charging with new oil, thus exonerating the lubricant from blame.Lubricating oil base-stocks are complex mixtures of hydrocarbons with minor concentrations of sulphur and nitrogen compounds. The hydrocarbons can be analysed by ultraviolet spectroscopy to determine the aromatic components (alkylbenzenes, -naphthalenes, -phenan- threnes and higher ring compounds); the polynuclear aromatics are analysed by a variety of spectroscopic and chromatographic techniques, including ultraviolet fluorescence and both gas and liquid chromatography.For some years we have used a mass-spectrometric technique that can analyse the relative molecular mass distributions of several hydrocarbon types.Unfortunately, certain sulphur compounds have the same nominal mass as the hydrocarbons. Their removal by adsorbent beds was assessed by p- and y-counting.304 ANALYSIS IN THE ENERGY INDUSTRIES Proc. Analyt. Div. Chew. SOC. For example, both benzthiophen and butylbenzene have a relative molecular mass of 134.However, we are now applying a mass spectrometer of very high resolving power (with a specification of 150 000 resolving power) to distinguish compounds such as C,,H,, and C26H42S, which require a resolving power of 114 000 to separate them fully. Part of a mass spectrum was displayed, showing the resolved multiplet 386.304 1 (C2,H4,S2)/386.300 7 (C2,H4,S) /386.297 3 (C2?H3?).Other applications of spectroscopy include the use of infrared techniques to determine the concentration of hindered phenolic antioxidants during the blending of lubricating oils based on the intensity of the absorption band at 3600 cm-l. Multigrade lubricating oils are designed to have a very small change in viscosity with temperature (i.e., a high viscosity index), smaller than is possible with most naturally occurr- ing hydrocarbons; this is achieved by incorporating a polymeric thickener.It may be necess- ary on occasions to determine whether an oil contains a polyisobutene or a poly(alky1 meth- acrylate) additive. We have found that this problem is readily solved by first concentrating the additive by dialysing the oil through a rubber membrane and then analysing the residue by proton nuclear magnetic resonance.We have also found that one of many useful applica- tions of carbon-13 nuclear magnetic resonance spectroscopy (in its digital Fourier transform mode) is as a means of distinguishing between dipropylene glycol and diethylene glycol in a complex mixture used as an anti-icant in gasoline. Modern developments in the petroleum industry must be supported by similar developments in the analytical sphere. Each year there is a need to analyse more and more products for smaller and smaller concentrations of components : acceptable limits of detection are forever being reduced.There is thus the need to make every possible use of new scientific dis- coveries and techniques. To use manpower efficiently, automatic systems, dedicated com- puters and microprocessors must be used whenever they are applicable.We must apply the latest ideas in both inorganic analysis (such as flameless atomic-absorption spectroscopy for determining sub-parts per million concentrations of silver in aviation turbine oils) and in organic analysis (as in determining parts per billion of specific polynuclear aromatics). This survey has attempted to illustrate many of the analytical problems of the petroleum industry, with reference to the parts of the industry where they arise, and to demonstrate the techniques used for their solution.I am indebted to Messrs. Venables and Gee of Stanlow Refinery and to many colleagues inside and outside the Analytical Division of Thornton Research Centre for much of the detailed information presented.An Integrated Approach t o the Analysis of Air-pollutant Polynuclear Aromatic Hydrocarbons K. D. Bartle M. L. Lee and M. Novotny School of Chemistry, University of Leeds, Leeds, LS2 9JT Department of Chemical Engineering, Massachusetts Institute of Technology, Cambridge, Mass., U S A Depavtment of Chemistry, Indiana Univenity, Bloomington, I n d ., USA Polynuclear aromatic hydrocarbons (PAH) are the largest known group of chemical carcinogens in urban air, arising mainly from the burning of coal and oil for heating and power generation and from the combustion of transport fuels. It is thus of particular interest to the energy industries to identify the PAH in air po1lutants.l While many procedures based on chromatographic and spectroscopic methods have been devised for the study of PAH, no single method provides complete resolution of the isomers, which show wide differences in tumour-promoting activity.The integrated scheme2 described here incorporates the separation of PAH by solvent partition, followed by column chromato- graphy on a lipophilic gel, and then high-resolution liquid chromatography.IdentificationOctober, 1976 ANALYSIS I N THE ENERGY INDUSTRIES 305 of the individual compounds was made by ( a ) high-efficiency gas chromatography on glass capillary columns, combined with mass spectrometry ; (b) Fourier-transform proton magnetic resonance ; and (c) ultraviolet spectroscopy and fluorimetry. All separations were also moni- tored by gas chromatography on inert glass capillary columns using splitless injection.Three hundred glass-fibre filters through which air from cities in Indiana, USA, had been drawn at 73 m3 h-l for 24 h were Soxhlet extracted with dichloromethane. PAH were obtained from the extract (3.6 g) by a solvent-partition scheme in which phenols and bases were removed by washing with aqueous alkali and acid, respectively, and other neutral com- pounds were separated from the hydrocarbons by washing with aqueous methanol.Finally, PAH (1.5 g) were obtained by partitioning between cyclohexane and nitromethane. The PAH were first separated on the basis of ring number using Sephadex LH-20 lipophilic gel but propan-2-01 as mobile phase : aromatic hydrocarbons are eluted in order of increasing relative molecular mass, and the retention volumes of isomers and their alkyl derivatives are similar.As a preliminary, the optimum flow-rate was selected by determining the dependence of column efficiency on flow-rate. The dependence observed is similar to that observed by Sjovall et aZ.3 for a lipophilic gel in the exclusion mode. The degree of separation, shown by chromatography on an inert glass capillary column4 coated with SE-52 methylphenyl silicone elastomer stationary phase, showed that further fractionation was necessary.This fractionation was carried out by repetitive high-performance liquid chroma- tography with a polar chemically bonded phase (alkylnitrile on Porasil C, 37-75 pm) with hexane as mobile phase.Capillary gas-chromatographic monitoring of these fractions sug- gested that the range of compounds was now much less. Ultraviolet and, to a more limited extent, fluorescence spectra of the fractions were used to determine the aromatic types present. Especially for the fractions of low relative molecular mass, the evidence suggested that similar ring types and their alkyl derivatives were con- centrated in the same fraction, e.g., anthracenes - phenanthrenes, pyrenes - fluoranthenes and chrysenes - benz[a]anthracenes.Combined gas chromatography - mass spectrometry of the liquid-chromatographic fractions was carried out with an SE-52 capillary column coupled directly to the ion source of a dodecapole mass spectrometer without apparent loss of resolu- tion.Retention data allowed the assignment of a number of peaks, for example the three methylpyrenes in the pyrene - fluoranthene fraction; five other compounds with relative molecular mass 216 in this fraction were assigned as the methylfluoranthenes. In a chroma- togram from a fraction that ultraviolet spectroscopy showed was mainly chrysene and its derivatives, with some benz[a]anthracene, peaks for compounds with relative molecular mass 242 were attributed to methylchrysenes.A list of compounds identified by a combination of gas chromatography with mass spectro- metry and gas-chromatographic retention data is contained in Table I. However, in spite of the power of gas chromatography - mass spectrometry preceded by ultraviolet spectroscopy certain vital information is still lacking, namely the identity and position of substitution of methyl derivatives, which of course vary markedly in carcinogenic activity.In this respect5 and in providing information concerning aspects of molecular symmetry, proton magnetic resonance (PMR) is unique; however, until the advent of pulse Fourier- transform spectroscopy, which allows many scans to be recorded and averaged in a short time, the technique has been limited by lack of sensitivity.Indeed, continuous-wave, ie., single- scan, PMR spectra of the PAH fractions revealed little except in very favourable instances where high molecular symmetry resulted in intense signals. For example, the single-scan spectrum of a fraction of high relative molecular mass (about 300) consisted only of a diffuse band in the aromatic region, but with a sharp singlet at 8.95 p.p.m., the entire spectrum of coronene.For other fractions, pulse Fourier-transform PMR was necessary. Thus the 90-MHz FT spectrum of the chrysene fraction not only confirms the strong con- tribution from chrysene, and to a lesser extent benz[a]anthracene, but also shows peaks in the methyl-proton region.From chemical-shift data, four of the six possible methylchrysenes were assigned: the 1-, 2-, 3- and 6-methyl derivatives; 1-, 2- and 6-methylchrysenes are moderately carcinogenic, while 3-methylchrysene is strongly carcinogenic.6 The potent 5-methylchrysene is apparently absent, as is the similarly sterically hindered 4-methyl compound. The methyl region of the FT PMR spectrum of the pyrene - fluoranthene fraction Appropriate fractions from the Sephadex LH-20 column were bulked.306 ANALYSIS IN THE ENERGY INDUSTRIES PYOC.Aaalyt. Div. Chenz. SOC. TABLE I COMPOUNDS IDENTIFIED BY CAPILLARY-COLUMN GAS CHROMATOGRAPHY - MASS SPECTROMETRY I N URBAN AIR PARTICULATE MATTER Peak 1 2 3 6, 7, 8 9 10 i l 12 13 15 I 6 17-22, 25, 26 23 24 25, 30-33 29 34, 35, 43 36-40 41 42 44 45 47-53 54-56 57, 59, 65 60, 63, 64 Relative llio lec ular 184 178 178 198 192 192 190 192 192 212 204 206 202 202 218 202 220 1ll;LSS 216 216 216 216 216 232 230 244 234 co I npo u 1 I( 1 Dibcnzo thiophen Phenanthrene Arithraccne 1Clethyldibenzothiol,hc :IS 3-lClcth y Iphenan thrci IC' 2-Methyiphenanthr tile 4H-Cycl0 1Ieilta idef I p h n- 9-Meth-ylphenaiithr~lil: l-Mcthylphenanthrcne Dimethyl- or ethyldibcnzo- thiophcn Mcthyl-4H-cyclopenta- rdeflphenaiithrene Dimethyl- or ethylphenan- threncs or -anthraccnes Fluoranthenc Benzacenaphth ylenc Dimethyl- or ethylcyclo- penta[def] phenanthrenes Pyrene Trimethyl- or methylethyl- aiithicne phenanthrencs or anthracenes LVethylfluoranthencs Benzo[a]fluorene Benzo[b]fluorene +- 2-me- thylp yrcne 4-Methylpyrcnc l-Methylpyrene Trimethyl- or methylethyl- -4H-cyclopentaCdef] - phcnanthrenes Dimethyl- or ethyl- fluoranthenes or -pyrenes Trimethyl- or methylethyl- fluoranthenes or -pyrenes Naphthobenzothiophens Peak 61 62 66 67 69, 71 70 74 76-80 81-53 84-90 9 1-94 95 96 97 98 99 100 101-105 106 108, 110, 113, 114, 111,112 115 116 117, 118, 121, 122 120 Relative molecular mass 226 228 228 228 242 240 248 242 254 256 268 252 252 252 252 252 252 266 306 276 278 292 304 302 300 Compound Benzorghi] fluoranthene Benzo[c]phenaiithrene Renz [alanthracene Chrysene Methylbenzo [c] phenan- threnes Methvlbenzo[ghi]fluoran- thene Methylnaphthobeiizothio- phen Methylchrysencs or methyl- benz[a] anthracenes Binaphthyls Uimethyl- or ethylchry- senes or -benz[a]anthra- cenes Methylbinaphthyls Benzo[j]fluoranthene Benzo[k] fluoranthene Renzo [h] Auoranthen e Renzo [el p yrene Benzo [a] pyrenc Pcrylene Methylbenzopyrenes or benzofluoranthenes Quaterphen yl Dibenzanthracenes Methyldibenzanthracene Diphenylacenaphthylene Dibenzopyrcnes Coronene allowed positive identification af all five methylfluoranthenes for the first time in air- pollutant PAH.Part of the over-all analytical scheme was now compressed into a simple fingerprinting pro- ~ e d u r e .~ Single filters were extracted with cyclohexane and the extract was partitioned with nitromethane to yield a PAH fraction for capillary gas chromatography. Filters from different locations (industrial, downtown and residential) in the same city showed differences that were greater than those between filters from the same sites, and reflected the likely PAH sources, namely the burning of coal, gasoline and oil or gas, respectively.As well as providing a rapid assessment of the level of certain individual pollutants, this method may be capable of indicating the origin of a given type of air pollution. The over-all analytical scheme has also been applied to the PAH in tobacco and marijuana smoke condensates.Marijuana smoke is markedly richer in PAH carcinogens of high relative molecular mass.8~~ References i. 2. 3. 4. 5 . Butler, J. D., Chemy Bvit., 1975, 11, 358. Novotny, M., Lee, M. L., and Bartle, K. D., J . Chvomat. Sci., 1974, 12, 606. Sjovall, J., Nystrom, E., and Haahti, E., Adv. Chvomat., 1966, 6, 119.Novotny, M., and Rartle, K. D., Chvomatograplzia, 1974, 7, 122. Bartle, I<. D., and Jones, D. W., Adv. Ovg. Chem., 1972, 8, 317.October, 1976 ANALYSIS I N THE ENERGY INDUSTRIES 6. 7. 8. 9. Hoffmann, D., Bondinell, W. E., and Wynder, E. L., Science, N.Y., 1974, 183, 215. Bartle, K. D., Lee, M. L., and Novotny, M., Int. J . E n v i v . AYzalyt. Chew., 1974, 3, 349. Lee, M.L., Novotny, M., and Bartle, K. D., Analyt. Chew., 1976, 48, 405. Lee, M. L., Novotny, M., and Bartle, K. D., Expevientia, 1976, 32, 280. 307 Application of the “SOLFA” On-line Analyser t o the Measurement of Total Sulphur in Petroleum Distillates and Residual Fuels C. F. Gamage Applied Reseavch Labovatovies Ltd., Wingate Road, Luton, Bedfovdshive, L U4 8P U Why Measure Sulphur? Most products from the refining of crude petroleum are eventually burnt, for example in engines as diesel fuel or in boilers as fuel oils.The presence of sulphur in these products is undesirable as the chemical compounds produced can aggravate engine wear and increase corrosion of combustion equipment. More important is the general problem of pollution of the atmosphere with the combustion products of sulphur when the petroleum products are burnt.Maximum sulphur levels for each product are generally specified, and these levels are continually being reduced in order to meet customer requirements and legislation on maximum levels of sulphur emission. Processes for removing sulphur from petroleum products do exist, but the de-sulphuration processes are expensive and, if they can be improved, production costs can be reduced.The availability of low-sulphur crude petroleums is limited; they cost more and most efficient use must be made of them in combination with other crudes. The blending of different distillation products is often carried out in order to obtain products of the correct specification, including sulphur content. Obviously the manufacture of products with significantly less sulphur than the specified maximum is uneconomic. This “sulphur give- away” can be very expensive and so measurement and control of sulphur is an important aspect of refinery operations.Why Measure On-line? The time factors associated with laboratory testing can be inconvenient and even critical. With on-line blending and direct loading of products without storage, real-time measurement of product quality becomes increasingly important. Many key properties, such as viscosity and density, are already measured and controlled on-line.Sulphur content is also a key property and must also be measured and controlled on-line. X-ray Fluorescence Fluorescent X-rays are emitted by the constituent atoms of a sample when it is bombarded with high-energy X-rays.The primary high-energy X-rays can be generated in an X-ray tube or with a radio- active isotope. The fluorescent X-rays from each element have energies that are unique to that element. Thus, by identifying each X-ray energy, it is possible to identify the elements in the sample. By measuring the intensity of each energy it is possible to establish the con- centration of each element.The non-dispersive technique facilitates close coupling of the X-ray source, sample and detector. This enables low-power sources to be used, such as a radioactive source as used in the ARL N940 non-dispersive X-ray analyser. Alternatively, a low-power X-ray tube operat- ing at typically 30 kV and 200 pA (6 W) can be used. At these low powers, a simple voltage generator can be used.Air cooling of the X-ray tube can be used instead of water cooling. Both of these X-ray sources (radioactive isotope and low-power X-ray tube) have been shown to give excellent analytical performance for the analysis of sulphur in petroleum products in laboratory instruments. For an on-line instrument, the X-ray tube is preferred as it gives the possibility of greater safety.The SOLFA analyser uses the techniques of non-dispersive X-ray fluorescence.308 ANALYSIS IN THE ENERGY INDUSTRIES YYOC. Analyt. Div. Chenz. SOC. The general principal of operation of the SOLFA analyser is as follows. High-energy X-ray rays bombard the oil sample, which is flowing through the flow cell. Fluorescent X-rays from the sample are detected with a sealed gas-filled proportional counter and the resultant pulses from the detector are then amplified.The pulses arising from sulphur radiation are electronic- ally selected and integrated for a chosen integration time and the resultant integrated signal is displayed on a digital voltmeter. Before delivery, each SOLFA analyser is calibrated and tested using samples of known sul- phur content.When installed, the calibration of the analyser must be checked in the operating environment, using oil samples of accurately known sulphur content and typical of those products which it will be routinely analysing. The liquid samples of known sulphur content are recirculated in turn in order to obtain digital voltmeter readings from which a calibration graph of percentage of sulphur by mass against voltmeter reading can be established.The zero and gain calibration controls can then be adjusted to give a direct display of sulphur content. Instrument Description Safety Features All cabinets of the analyser are of flameproof-type boxes manufactured generally to British Standard 229 : 1957 (“Flameproof Enclosures of Electrical Apparatus”).The measurement head and electronics’ enclosures are independently purged with clean, dry air and pressure switches are provided to isolate the power to these units if the internal air pressure falls below a set value. Pressure switches in the air-purging lines prevent electrical mains being switched on until purging air has been established at the required pressure. Any drop in this pressure, for example if a cabinet door is opened, will cause the pressure switch to activate a relay that isolates the mains electrical supply to the SOLFA analyser.To meet the specific safety requirements of the Physikalisch-Technische Bundesanstalt in Germany and authorities in the USA, air-purge monitor systems are fitted to units intended for use in these countries. The two air-purge monitor systems are similar in design and operation but differ in detail of construction.Their purpose is to ensure that the instrument cabinets are purged with a known volume of air in order to remove any combustible gases before electrical power is applied. Each cabinet door is fitted with a Castell lock in a system so arranged that all doors must be locked before the mains electrical supply can be switched on.In the event of a leakage of oil from the flow-cell window, a detection system automatically switches off the mains electrical supply to the analyser and the sample flow. The X-ray tube was specifically incorporated to overcome objections to the use of radioactive isotopes in pot entially hazardous areas. All of the safety features noted above result in complete electrical isolation of the SOLFA analyser.Under this condition, the X-ray tube is completely safe to be handled. In the event of a catastrophic failure, no hazardous radiation source is left energised. With a radio- active isotope this situation cannot exist as an isotope can never be switched off. The use of an X-ray tube is a major safety feature of the SOLFA analyser.Performance Reliability was initially assessed by running the SOLFA analyser continuously day and night for approximately 2 000 h. Since that time, many thousands of hours of running have been accumulated both in the laboratory and on-line. Key items of the SOLFA analyser design, such as the flow cell, X-ray system and electronics, behaved excellently.Accuracy and stability were assessed by a statistically designed programme covering 5 consecutive days and nights during which the analyser had to run continuously on hot cir- culating oil. No adjustments whatsoever were made to any of the instrument parameters. Six gas oils and five residual fuel oils were used, all accurately tested for sulphur content, vanadium, nickel, carbon to hydrogen ratio, specific gravity plus viscosity and pour point for the residuals.Each of the 11 test samples was run through the analyser, in random order, on each of the five days. Ten consecutive readings were taken on each sample on each run. Over 800 measurements were obtained from the 5-d test programme and were interpreted as follows.Octobev, 1976 ANALYSIS IN THE ENERGY INDUSTRIES 309 Calibration The calibration line relating digital voltmeter reading to sulphur content was completely linear.The maximum deviation from the calibration line for the gas oils examined was 0.015y0 m/m of sulphur and for the fuel oils O.OOS~O m/m of sulphur. The fuel oils contained 11-60 p.p.m. of vanadium and 12-26 p.p.m. of nickel. There was no correlation between deviation from the line and metals content for any sample.Thus, for the vanadium and nickel levels present, no interference was recorded. Over-all Accuracy For the whole 5-d run, the standard deviation ((3) for the scatter of every single sample measurement about the calibration line was 0.024% m/m of sulphur. Calibration correction reduced this o value to 0.016yo m/m of sulphur for the gas oils and 0.01270 m/m of sulphur for fuel oils.On this basis, the over-all accuracy for a single determination at the 95% confidence level (i.e., &20) was &-0.03Y0 m/m of sulphur with daily calibration and &0.05y0 m/m of sulphur with weekly calibration. This over-all accuracy is a composite of several factors that can be isolated and examined separately.Long-term Precision was 0.009yo m/m of sulphur for gas oils and 0.015y0 m/m of sulphur for fuel oils. The standard deviation for the differences between the mean daily values on each sample Conclusion The performance of the SOLFA analyser compares very favourably with the best laboratory methods for analysing for sulphur. The over-all accuracy at the 95% confidence level is &o.03y0 m/m of sulphur with daily calibration and &0.05~0 m/m of sulphur with weekly calibration.This accuracy is virtually independent of product type and sulphur level. The Model N920 SOLFA analyser is a joint development between Applied Research Lab- oratories Ltd. and the British Petroleum Company Ltd. The author gratefully acknowledges the permission to publish this paper and the assistance and advice from colleagues at ARL and BP.ldentif ication of Crude Oils by Luminescence Techniques P. John and I. Soutar Depavtrnent of Chemistvy, Heviot- Watt Univevsity, Riccavton, Cuvvie, Edinbuvgh, EH14 4A S The detection and determination of crude-oil contamination in a variety of environments is of increasing importance. Of the numerous techniques that are available to the analyst, fluorescence spectrophotometry has a number of distinct advantages but, when used in the conventional mode, it fails to distinguish adequately between crude oils from different sources.This paper outlines a novel method of characterising crude-oil samples. Variations in the composition of the complex mixture of hydrocarbons and heterocyclic compounds that comprise crude oil are insufficient to cause marked changes in fluorescence emission spectra.Published fluorescence spectra of oils, both neat and in solution, and results obtained in this laboratory confirm this view. Attempts at “fingerprinting” oils have been based mainly on the changes in the intensity of fluorescence emission, following a judicious choice of a short excitation wavelength below 300 nm. Only minor variations in the band contours are apparent in conventional fluorimetry and this technique is of limited use as an exact diagnostic tool. I n conventional fluorimetry, the fluorescence intensity is recorded as a function of the emis- sion wavelength while the excitation wavelength is held at a constant value. Excitation fluorimetry involves the reverse situation, namely, variation of the excitation wavelength at a constant emission wavelength. A third possibility, known as synchronous excitation3 10 SAMPLING-PROBLEMS AND SOLUTIONS PYOC. Analyt. Div. Clzem. SOC. fluorimetry, can be envisaged, whereby neither wavelength is kept constant but with the constraint that the difference between the excitation and emission wavelengths should remain constant throughout the spectrum. Synchronous excitation of a sample of crude oil utilises the complex nature of crude oil by maximising the fluorescence intensity of each component. Thus, the resulting synchronous spectrum shows considerably more structure than the conventional spectrum. These factors relevant to the identification of crude oils, namely, wavelength increment, solvent, concentration, temperature and frequency band pass, have been evaluated. Wavelength Increment The spectral distribution is a function of the difference, Ah, between the excitation and emission wavelengths. The optimum value, for discrimination purposes, of Ah lies in the range 20-25 nni, corresponding approxiniately to the difference between the absorption and emission maxima in simple aromatic compounds. Solvent Non-quenching solvents, of high fluorimetric purity, were employed during this study. The spectra were usually recorded in cyclohexane solution. The application of the present technique to neat oil samples was demonstrated by employing frontal illumination of a thin film of crude oil contained between optically flat quartz plates. Comparison between standard and synchronous excitation spectra showed greater discrimin- ation between the oils for the latter technique. Concentration Marked shifts to shorter wavelengths as the concentration was decreased occurred for both Energy transfer and inner-filter effects were minimised the normal and synchronous spectra. at high dilution but characterisation of crude oils was achieved at a fixed concentration. Temperature and Frequency Band Pass As ex- pected, increasing the band width decreased the spectral resolution with consequent loss of fine structure. In addition, the relative intensities of the main peaks in the synchronous excitation spectra were less dependent on the wavelength increment. In conclusion, therefore, the technique of synchronous excitation fluorimetry can be used to characterise crude-oil samples. Although in certain instances a unique identification is not possible, this rapid method used in conjunction with other analytical methods reduces the effort required in identifying a source of oil pollution. Over the temperature range 20-49 "C the synchronous spectra were unaltered.

ISSN:0306-1396    

DOI:10.1039/AD9761300295

出版商:RSC    

年代:1976

数据来源: RSC

摘要:

3 10 SAMPLING-PROBLEMS AND SOLUTIONS PYOC. Analyt. Div. Clzem. SOC. Sampling-Problems and Solutions The following is a summary of one of the papers presented a t a Meeting of the Automatic Methods Group held on October 8th, 1975, and reported in the November issue of P y o c e e d i y s (p. 255). Automatic Sampling and Weighing Systems for Use in the Pharmaceutical Industry Erica Evans C I ElectroMics Limited, Bvunel Road, Churchfields, Salisbuvy, Wiltshive It is required by law that samples of tablets and capsules be checked in order to ensure uniformity of mass.The rules laid down in the regulations in the British Pharmacopoeia are given in Table I. Most companies that CI Electronics supplies take sample tablets or capsules during theOctobev, 1976 SAMPLING-PROBLEMS AND SOLUTIONS 311 manufacturing process and subsequently for quality control. The normal practice during manufacture is for the tablet-press or capsule-filling machine operator to take ten samples and weigh them on an analytical balance, take the average mass and plot this on a graph of mass zwsuus time. I t is during this slow procedure that adjustment to the tablet machine can be made.Owing to the different performance of machines that most companies operate, the number of samples varies enormously. They range from single-stroke or very slow tablet machines to the latest design of tablet machines, which can produce 10 000 tablets per minute. In capsule production the types of machine used are numerous, ranging from hand-operated units to the latest machine, which is designed on the rotary principle and is capable of pro- ducing 15 000 capsules per hour.The pharmaceutical companies set their own limits well within the BP specification. The automatic balance equipment described below is designed to meet these requirements of the pharmaceutical industry. CI Electronics first became involved in the pharmaceutical industry about 8 years ago and the first European Automatic Tablet and Capsule Balance was designed for Roche Products' Analytical Department.This balance was suitable for taking a sample of tablets and producing a group of actual tablet masses in the form of square waves on a chart recorder. The balance was subsequently developed to be used with a pre-programmed calculator and a printed record of individual tablet or capsule masses obtained.During the life of this unit its use has changed. Initially the balance was used exclusively by quality-control depart- ments but today this type of equipment is used in or near the production areas in order to provide faster feedback to the machine operators. During the last 5 years similar equipment has been produced by both Sartorius and Mettler.All this type of equipment is now offered with either programmable calculators giving statistical results or with a teletype, which pro- duces hard copy and punched-paper tape for subsequent computer analysis. The Carousel Tablet Balance has the advantage that it can be loaded with up to 16 different products and can then be left to run unattended. The method of using Carousel is simple.A coded tag is produced to customer specification for every product to be weighed. This tag is pre-punched with the upper and lower mass limits of the product. When needed it is placed in position on the Carousel. Several containers can be used for the same product. Information stored on the first code is retained for successive containers until updated by reading another tag noting a change of product. The number of tablets or capsules to be sampled can be pre-set, e.g., 20, and they are then counted automatically and any samples left on the feeder will be flushed through the system.When the Run button is pushed the Carou- sel automatically indexes and deposits the samples on the vibratory feeder. Any double weighings can be ignored.A mean mass is printed out on the Teletype at the end of every 10 weighings and also at the end of the sample run. The calibration mass is automatically checked and printed out. Any drift can then be taken into account by the computer program used to analyse the data. The data is presented in such a way as to enable it to be analysed by either the customer's in-house computer or remotely by a computer time sharing service.Connection to the computer is made via a standard telephone and then switched to the tele- type by either a PO Modem or acoustic coupler. The teletype supplied with the Carousel system is suitable for use as the terminal to the computer. During the last 2 years, certain factors have caused the manufacturers to demand a much TABLE I BP LIMITS FOR TABLETS AND CAPSULES Bl' limit, yb Tablets <:so 111:: 80-250 nig >250 ing i 10 I- 15 .i 5 - c 10 f 7 .5 -z 12.5 Cajisu Ics Content < 120 iiig 5 10 3: 50 Content > 120 nig 5 7 . 5 4- _ _ 15 * Two tablets in 20 are permitted outside this limit. No tablets are perniittcd outside this limit.312 EQUIPMENT NEWS PYOC. Analyt. Div. ClaePn. SOC. tighter production control system.These factors are: much higher prices for raw material; faster output from tablet presses and capsule-filling machines; and in the instance of capsules much stricter limitations on re-working rejected material (the cost of the empty capsule shell is also a factor). It is possible to sort rejected capsules. The only automatic sorting balance in use in the UK a t present is the SADE sorting balance.It is used to recover capsules that have been rejected as being outside mass tolerances. At a weighing speed of 20 per minute in each head the accuracy is *l mg. The weighing cycle can be speeded up with a consequent loss of accuracy. The standard hopper holds approximately 28 000 capsules so the machine can safely be left to run overnight.The upper and lower mass limits are set on the front of the balance and the capsules are sorted into accept or reject. A count is kept of the numbers falling into three categories, i.e., high, low and accept. The normal recovery figure obtained is in the range between 80 arid 90%. Companies have recovered the cost of this equipment in from 9 months to 1 year. CI Electronics operates a capsule-sorting service for the industry and approximately 60 x lo6 capsules per month are sorted.This machine can be used to sort tablets if a minor adjustment is made to the bowl feeder. This is a semi-automatic on-line mass-control system, designed and installed at Evans Medical, Liver- pool. It provides production control a t the time of manufacture and the mass information obtained is used as quality control records. This system enables information, such as tablet press performances, to be obtained. In addition, mass reconciliation between bulk powder being processed and tablets being manufactured can be stored on the computer for stock records. Detailed information on the data capture and system operation is available from the author. The most interesting development combines production and quality control.

ISSN:0306-1396    

DOI:10.1039/AD9761300310

出版商:RSC    

年代:1976

数据来源: RSC

摘要:

312 EQUIPMENT NEWS PYOC. Analyt. Div. ClaePn. SOC. Equipment News Chart Recorders The range of the 28000 series of chart recorders has been extended by the addition of four new systems versions and an integrator model. A choice of seven 250-rnm chart width potentio- metric recorders plus several options is now offered. There are single- and two-pen versions with their sensitivity pre-set by the supplier to meet customers’ requirements.The chart speed can also be pre-set or the instrument supplied with the normal ten-position chart- speed selector with speeds in the range 0.5 mm min-1-10 mm s-l. The usual 28000 series options are also available with these new systems, e,g., event markers, remote pen lift, chart take-up spool and re-transmitting potentiometers that give an output proportional to the pen position.The new integrator model can be applied to tech- niques, such as gas chromatography, with which the area beneath the curve is required. It is a two-pen system, the first pen operating over the full input range, variable from 250 pV to 100 V for f.s.d., the sccond pen writing the integral trace at the right-hand side of the chart.Bryans Southern Instruments Ltcl.. 1 Willow Lane, Mitcham, Surrey, CR4 4UL. The Tekman range of recorders is now marketed in the UK by Cherwell Laboratories. A number of developments has been incorporated in the latest TE200/220 range and these developments include a variable control heated stylus, which avoids pen blockage and gives finer traces, a selection of input ranges from 50pV to 100 V with a variable control t o enable full scale deflection to be set at any point, a very fast pen response with a choice of 23 chart speeds from 10 mm 11-l to 600 mm min-l and a zero check, which can be used a t any time without affecting the input signal.A number of standard items such as remote on/off switch- ing, facilities for external pulse or sine wave drive, etc., are fitted to these units. Cherwell Laboratories Ltd., P.O.Box 3, 1 Murdock Road, Bicester, Oxon., OX6 7XH. Electron Microscopy Stereoscan 150 is the name of a new all-purpose scanning electron microscopc. From the basic instrument an extensive modular system pro- vides for expansion to a full research-scale microscope. It features a guaranteed resolution of 7 nm, continuously variable accelerating voltage up to 40 kV and a magnification range of 5 x to lo5 x (with 3 : 1 zoom).Features such as automatic or push-button manual focusingOctober, 1976 EQUIPMENT NEWS 313 and fully automatic vacuum sequencing facilitate its operation. I t is claimed that down-time is virtually eliminated by instant push-button aperture cleaning and quick- change column linear replacement.The photo- graphic recording system is fast with a magni- fication marker and alpha-numeric data automatically included on the micrograph. Microanalysis facilities include vertical and horizontal fully focusing spectrometers, energy- dispersive systems and the Cambridge inte- grated X-ray analysis system, which combines wavelength-dispersive ancl energy-dispersive analysis.Full signal-processing capabilities are offered and a high-resolution recording cathode- ray tube is also available. Cambridge Instruments, Moat House, Mel- bourn, Royston, Herts., SG8 6EJ. Automatic Analyses The AC 30 is a flexible kinetic and end-point analysis system which combines the AC1 Automatic Chemistry Unit, the SP30 digital spectrophotometer and the DI< 16 printer.It provides total automation of all stages in the wide variety 01 chemical determinations which the Automatic Chemistry Unit is designed to perform. Up to 89 kinetic or 240 colorimetric tests per hour can be processed with low reagent usage. IXlution, reagent addition, mixing, incubation, sample identification and measure- ment are carried out automatically. The AC30 is claimed to be the perfect system for spectro- photometric analysis in the 300-750-nm spectral range: it provides a print-out directly in any desired units.Other features include the use of solid-state electronics, pneumatic operations ancl corrosion-resistant materials. Pye Unicam Ltd., York Street, Cambridge. Low-temperature Ashers In the LTA-505 and LTA-302 low-temperature ashers no energy is applied directly to the specimen.It is claimed that analyses for trace elements and studies of crystalline structure are therefore simplified and can be pursued to greater depths. In these models the only oxidising agent is oxygen and gentle low-temperature ashing occurs when the oxygen is excited by a radio-frequency electromagnetic field. The controlled removal of organic materials is thus achieved while volatile trace elements and the original morphology of the inorganic constituents of the ash are maintained. The LTA-505 has five ashing chambers and is suitable for a large number of samples while the LTA-302, with two chambers, is suitable for laboratory use a t lower sample throughput.Both are equipped with automatic plasma control and sample agitation.ICN Instruments Division, ICN Pharm- aceuticals (TJK) Ltd., Riverdene Industrial Estate, Hersham, Surrey, KT12 4RG. Liquid Scintillation Counters Recent additions to the Intertechnique range of automatic liquid scintillation and gamma counting equipment include the SL 4000 and CG 4000 systems, respectively. Both of these models have been designed to facilitate the handling of larger numbers of samples.Intertechnique Ltd., Cottrell House, 53-63 Wembley Hill Road, Wembley, Middx., HA9 8BE. Water Sampler The Model 1680 high-speed sequential and composite sampler has a quartz-crystal timer allowing collection a t intervals between 1 and 999 min. Alternatively the sampler can be controlled by a flow meter. A high-speed peris- taltic pump is said to ensure sufficient line velocity to prevent settling of suspended solids but to be not fast enough to pick up static bottom sediments which may affect sample quality. For information on this and other models, including refrigerated and explosion- proof versions, contact MSE Scientific Instru- ments, Manor Royal, Crawley, Sussex.Liquid Chromatography A new instrument has been developed for preparative-scale separations based on liquid chromatography.The PrepLC/System 500 is for routine use and is said to combine speed and economy with purity and amount. Funda- mental to the design and operation are large- diameter radially compressed preparative columns, Purity and amount of product can be increased by using several columns in series or the recycle capability.For a specific separation problem the output of the system can be kilogram amounts per day. Waters Associates (Inst.) Ltd., 324 Chester Road, Hartford, Northwich, Cheshire, CW8 2AH. The SCMlOO is a low-cost compact liquid chromatograph of modular construction. It incorporates such features as push button controlled precision injection, compressed air operation and a variety of syringe capacities.It can be used with existing pumps and detectors or be supplied complete with a matching pump-3 14 EQLJIPMENT NEWS PYOC. Analyt. Diu. Cheutz. SOC. ing unit and detection system. I t can easily be converted for automatic operation. The SCM100A is a high-pressure liquid c1iromatog;aph with an automated injection facility for unattended operation.Up to 60 sample containers can be accommodated in the sample changer for continuous sampling or alternate sampling and flushing. These and other high-pressure liquid- chromatographic units and accessories are available from Siemens Ltd., Great West House, Great \h'est I b a d , Brentforcl, Middx., TW8 9I)G. Automatic Sample Changer A new sample changer for use in hybrid auto- matic-analysis systems is announced.The probe moves up and down with a powered downstroke capable of penetrating a protective sample cover. A number of sample trays are available, taking cuvettes from 2- to 12-nil capacity, and in-line sample trains are also catered for. A very accurate timer is incor- porated and there are optional extras. The Newton Instrument Co. Ltd., Laboratory Automation, Carr Lane, Hoylake, Wirral, Merseyside, L47 4AU.Coulometry The new Metrohm coulostat can be used as a galvanostat for the electrolytic generation of reagents and as a potentiostat for the selective coulometric determination of polarographically active substances. As a galvanostat the instrument has 13 constant current ranges and the amount of reagent gcnerated is displayed directly on a five-figure digital indicator calibrated in micro-equivalents.When used as a potentiostat the potential of the working clectrocle against the reference electrode can be presented digitally on a four-figure selector over the range - 3 999 to + 3 999 mV. In this mode a current - time integrator is available. Other uses for this instrument include electrogravi- metry, the plotting of current - voltage curves and thc removal of unwanted metallic ions by pre-electrolysis.It is also compatible with the Metrohm range of automatic titration equip- ment, forming a coulonietric titration set. Roth Scientific Co. Ltd., Zurcourt House, 27 Osborne Road, Farnborough, Hants ., GU 14 BAA. High-viscosity Diluter An instrument is now available, based on the ADP-30 series of dispenser - diluters, which can sample and dilute liquids with viscosities of up for preventive maintenance in which oil samples are precision diluted with xylene prior to analysis for metals by atomic absorption. ICN Instruments Division, ICN Pharmaceu- ticals (UK) Ltd., Iciverdene Industrial Estate, Hersham, Surrey, KT12 4RG.Digital Densitometer Model DMA 40 allows the density of liquids and gases to be measured in 1-2 min.A precision of & 1 x g ~ m - - ~ is claimed with the possi- bility of automatic measurement when using the sample-changer accessory. Sample size is 0.7 rnl and, with a pressure adaptor, continuous measurements can be made. After introduction into a U-tube the sample is electromagnetically excited to vibrate a t its natural frequency, from which the density can be determined in- dependently of viscosity and surface tension.The value is displayed every 2 s on a digital printer and can be shown on an external printer. Stanton Redcroft, Copper Mill Lane, London, SW17 OUAT. Gas-sensing Probes Improved versions of the ammonia and sulphur dioxide gas-sensing probes have been announced.They are supplied in kits, which include refilling solution, spares and a flow-through adaptor. Electronic Instruments Ltd., Hanworth Lane, Chertsey, Surrey. New Materials New products for gel chromatography are announced. The CNBr-Activated Sepharose 6MR is for affinity Chromatography of whole cells and shoulcl facilitate the study of mem- brane-associated phenomena, while the DEAE- and CM-Sepharose CL-6B are designed for ion- exchange chromatography of polymers of high relative molecular mass and are particularly useful for large-scale applications.Pharmacia (Great Britain) Ltd., Paramount House, 75 Uxbridge Road, London, W5 5SS. Glass-lined stainless-steel tubing of 0.25 in 0.d. and bore size 3 or 4 mm is now available. Neutral borosilicate glass is fused to the bore of metal tubing and the resulting product can be used at temperatures up to 500 "C.It can be heated electrically by applying a low voltage across the metal casing. This new material could be used as a column in high-pressure liquid chromatography and in other situations where inert piping is required. to 10 000 cP. The HV-100 unit has been used International Marketing Department,Octobev, 1976 CHEMICAL SOCIETY LIBRARY Scientific Glass Engineering (UK) Ltd., 657 ,h;orth Circular Road, London, NW2 7AY.Pre-coated plates in various sizes for high- performance thin-layer chromatography (HP- TLC) are announced. A silica gel with a medium pore size (60 nm) is used, giving a specific surface of 500 m2 g-l and a pore volume of 0.75 ml g-l. Advantages claimed from the use of HPTLC plates include higher resolution, smaller loads, shorter analysis times and a higher degree of reproducibility. Anderman & Company Ltd., Laboratory Supplies Office & Warehouse, Central Avenue, East Molesey, Surrey, KT8 002. Porous microspheres (hyperspheres) based on the new spherical microparticulate silica, Hypersil, are now available. It is claimed that with these materials high efficiency, capacity, resolution and speed of analysis are obtained with peak symmetry approaching the ideal Gaussian curve. Various organic groupings are incorporated in this series of hyperspheres to give materials suitable for various applications. Shandon Southern Products Ltd., 95/96 Chadwick lioad, Astmoor Industrial Estate, Runcorn, Cheshire, WA7 1 P I i . 315

ISSN:0306-1396    

DOI:10.1039/AD9761300312

出版商:RSC    

年代:1976

数据来源: RSC

摘要:

Octobev, 1976 315 CHEMICAL SOCIETY LIBRARY Spectroscopic Problems in Chemistry. B. J . Brisdon and Ll. W. Brown. Reinhold. 1973. Bibliography of Electrophoresis, 1968-1972, and Survey of Applications. Z. Deyl. Jouvuzal of Chvomatogvaphy, Supple- mentary Volume No. 4, 1975. Elsevier. 1975. Instrumental Methods of Chemical Anal- ysis. G. W. Ewing. McGraw-Hill. 1975. Practical Scanning Electron Microscopy : Electron and Ion Microprobe Analysis.Edited by J . I. Goldstein and H. Yakowitz. Plenum. 1975. Van Nostrand Chemical Society Library The following publications of analytical interest have been added to the Library since the last list appeared in Pvoceedings (1975, 12, 324). Analytical Methods in Oceanography. Symposium of the Division of Analytical Chemistry’ of the American Chemical Society, Atlantic City, 1974.Edited by Thomas R. P. Gibb, J r . Advances in Chemistry Series, No. 147. ACS. 1975. Forensic Science. Symposium of the Divi- sion of Analytical Chemistry of the Ameri- can Chemical Society, Atlantic City, 1974. Edited by Geoffrey Davies. ACS Symposium Series, No. 13. ACS. 1975. Isoelectric Focusing. Edited by J . P. Arbuthnott and J.A. Beeley. Butterworths. 1975. Spectroscopic Methods of Identification of Microquantities of Organic Materials. G. M. Ayling. Dekker. 1974. Stationary Phases in Gas Chromatography. G. E. Baiulescu and V. A. Hie. Pergamon Press. 1975. Mossbauer Spectroscopy. Edited by U. Gonser. Springer-Verlag. 1975. Chemical Methods of Rock Analysis. ond Edition. P. G. Jeffery. Pergamon Press.1975. Sec- Atomic Absorption and Fluorescence Spectroscopy. G. F. I<irlrbright and M. Sargent. Academic Press. 1974. Infrared Spectra of Surface Compounds. A. V. Kiselev ancl V. I. Lygin. Israel Program for Scientific Translations. 1975. Chemical Analysis : An Advanced Text and Reference. Second Edition. H. A. Laitinen ancl W. A. Harris. McGraw- Hill. 1976. The Determination of Organic Compounds with N-Bromosuccinimide and Allied Re- agents.N. K. Mathur and C. K. Narang. Academic Press. 1975. Functional Group Determination of Olefinic and Acetylenic Unsaturation. K. Muller. Academic Yress. 1975. Activation Analysis with Neutron Genera- tors. S. S. Nargolwalla and E. P. Przybylowicz. Wiley-Interscience. 1973. Code of Practice for Chemical Laboratories. Royal Institute of Chemistry. 1976. Thermal Analysis : Comparative Studies on Materials. Edited by H. Kambe and P. D. Garn. Pro- ceedings of the U.S. - Japan Joint Seminar held in Akron, Ohio, 1974. Wiley. 1974.

ISSN:0306-1396    

DOI:10.1039/AD9761300315

出版商:RSC    

年代:1976

数据来源: RSC

摘要:

316 PORTABLE OXYGEN MONITORS PYOC. Analyt. Div. Chew. SOC. Survey of Portable The determination of oxygen in the atmosphere is of crucial importance for safe working in a wide variety of industrial operations. Where continuous monitoring is needed on-line instru- mentation is often installed a t fixed locations. but there are many situations for which portable monitors are desirable. h considerable number of such monitors is available and to assist the potential user a sur- vey of them has been undertaken, the results of TABLE I-PORTABLE Sensor - h-- (i) M e t e r f-- Scale (= range) Type Life x %02/ Dimensions/mm (ii) Accuracy (in ( A = audible (life in months in and Alarm h x l o 3 Manufacturer and Models and Mass parentheses) V = visual) parentheses) Bacharach Instrument Co.' (6 months) Sentox 2, portable 267 x 172 x 165 0-100% LEL AV Electrolytic 3.4 kg 0-25% O2 Adjustable cell (-) K25, portable 76 x 146 x 111 0-25% 0, None Electrolytic (6 months) 1.1 kg (=0.1% 0,) cell Biomarine Industries Inc. OA222R.portable with 51 x 64 x 127 0-40% O2 remote sensor 0.41 kg ( = 1 .O% f.s.) 0M322. portable with 127 x 64 x 51 0-40% O2 remote sensor 0.51 kg ( * 1 .O% f 5 ) 900 [combined combustib!e 102 x 210 x 760 0-100% LEL gas (c.g.) and oxygen 1.3 kg 0-40% 0, monitor], portable 0-5% CH4 ( * l % 0,: =5% c.g.) None Galvanic ( > 12 months) cell A Galvanic ( >- 12 months) Set for cell 19.5% 0, AV Galvanic cell (0,) ( > 12 months) Set for Catalytic (c.g.) 19.5% 0, Octo bey, 1976 Oxygen Monitors PORTABLE OXYGES MOSITORS 317 which are given in Table I.This survey is based on a table designed and supplied by the manufacturers is up-to-date to constructed by Rlr. C. H. Dickinson of the mid 1976. For further information the Control Engineering Group of the North West individual manufacturers should be approached. The information Region of ICI Ltd. OXYGEN MONITORS Price Response t o r--h-_. -7 90% of step Temperature Basic Replacement Additional information changeis Power supply compensation C e r t i f i c a t i o n unit c e l l - Rechargeable -12 to 49 'C Constructed to be €340 Reactivation Available as a dual monitor for battery intrinsically kit f l l combustible gas and oxygen safe (€378).- None -12 to 49 'C Factory Mutual f l 5 3 Reactivation Sample aspirator bulb fitted.required Cert. No. 17859 kit f l l Also available K525: 0-5 and 0-25% scales and K2500: 0-25 and 0-1 00% scales. <10 None 0 to 40 "C MESA approved $300 262440 (US Bureau of Mines) required <10 Alarm requires -15 to 40 'C MESA approved $400 2G2467 (US batteries Bureau of Mines) 10 (02) Built-in -1 5 to 40 'C MESA approved $600 5 (c.g.) rechargeable 8C-34 (US battery Bureau of Mines) - Also available 0A255: 0-10. 0-25 and 0-1 00% scales, remote sensor.OA202: 0-100% Built-in 0A222: 0-40% lsensors, Will 0A225: 0-25% (also accept OA233: 0-2 Atm. 1 remote sensors - Also available OM3253 0-25% scale. - Instrument also alarms for high CH4 and low battery voltage. Remote sampling kit included. Remote sensors available. Model 900R includes remote sensors.BOC Medishield Ltd. Harlake, portable 89 x 127 X 108 0-100% 02 AV Microfuel cell C1, 240 0.68 kg (&2.0% f s . ) For high or C1 (long life); C2,lOO low levels. C2 (for use Adjustable in anaesthesia) 26 1.5-V batteries Range - f182 C1. f 3 7 For medical use. (4 off) not excluding C2, f 2 8 Sensor fitted to retractable cable for alarm given cell Detection Instruments Ltd. - Edmont 60-625, portable 76 x 127 x 127 0-25% 0, A with /emote sensor 0.45 kg ( =0.2% 0 2 ) Set for 19.5% 0 2 10 9-V batteries 15 to 50 "C - €207 - Instrument also alarms for low (2 off) battery voltage and if sensor needs recharging.Also available 66-20: as 60-625 but without alarm. For footnotes see p. 31 8.318 Octobev, 19 76 PORTABLE OXYGEK 310KITORS 319 PORTABLE OXYGEN NOXITORS Pvor.A iinl$. Dli'. Chew. SOL. TABLE I-PORTABL Sensor (I) Meter r 7 Scale (= range) Type Life x %02/ and Alarm h x l o 3 Oimensionslmm ( 1 1 ) Accuracy (in ( A = audible (life in months in Manufacturer and Models and Mass parentheses) V = visual) parentheses) OXYGEN MON ITORS-continued Price Response t o r--h- 7 90% o f step Tem peratu re Basic Replacement changels Power supply compensation Certification u n i t c e l l Additional information €27 Push-button testing facility.Mallory cells: - Constructed to €90 BASEEFA and MP 675 approval - Instrument alarms for cell or PX1 (4 off) measurement-battery failure (2 off) requirements Optional low alarm only. Draeger Normalair Ltd. Oxylarm E l 0, pocket 152 x 64 x 25 18-24% O2 A 0.50 kg (-) Set for low (19) and high (?3)% 02.Adjustment possible Polarographic cell (SMRE) Polarographic cell (SMRE) 130 8 E l 1, portable with 250 x 120 x 189 0-40% O1 A remote sensor 2.6 kg ( -5% f s 1 For high and low levels Adiustable BASEEFA €165 €26 Optional aspirator. Also available Mallory TR132N mercury cells 3 to 37 "C certified E l 2 (no alarm): 0-10,O-40 and (2 off) 0-100% scales. Gastec C0rp.t GOA-40D.po table with 140 x 180 x 90 0-40% O2 AV Galvanic remote sensor 2 kg ( z 5% f.s.) Set for cell 18% Oz.Adjustable GO-25C. po:table with 80 x 135 x 70 0-25% O z None Galvanic remote sensor 0 95 kg (-) cell GO-525D. portable with 140 x 70 x 65 0-5/0-25% O z None Galvanic remote sensor 1 05 kg ( I0.2 f.s./ i 0 . 5 f.s.) cell 180 < 10 5.6-V mercury 0 to 40 "C Intrinsically safe.€191 €17 Also available GOA-25D: 0-25% cells (2 off). Approved by scale and GOA-525D: 0-5 and Equivalent to Japan Dept. of 0-25% scales. Mallory TR164 I-abour 180 180 <10 None required 0 to 40 "C As for GOA-40D €145 €1 7 As for €1 98 €17 Also available GO-1 D: 0-40% scale AA dry cell 0 to 40 'C i 1 0 and GO-25D: 0-25% scale. batteries ( 2 off) GOA-40D Taylor Servomex Ltd.0A272. portable 330 x 330 x 406 0-5,O-25. None Magnetodynamic - 9.07 ko 0-1 00% 0, cell - €367 R20 dry cell 100 ml (2 off) (1 off) 0 to 50 'C 7 at min 6-F-100 dry cell 7 at R20 dry cell 0 to 50 "C BASEEFA, Lloyds, €328 100 ml (3 off) DNV and FM min-' 6-F-100 dry cell certified (1 off) Not Recommended for suppressed zero required or a 5% range. Also available 0A273: a.c. supply voltage version.Not Approved for marine use required 0A262, po"teble 203 x 152 x 254 0-10. 0-25, None Magnetodynamic - ( z l % f s : 3% f s for 0-10 scale) 5 67 kg 0-1 00% 02 cell OA250, portable 330 x 330 x 406 0-10,O-25, None Paramagnetic 9.07 ka 0-1 00% 0, 7 at R20 dry cell 0 to 50 C BASEEFA €250 100 ml (2 off) certified min ' 6-F-I00 dry cell (1 off) Not Requires sample flow.Hand available OA251 : a.c. supply voltage version. required aspirator supplied. Also ( = A % f.s. f i r max. temperature variation of 5 'C) Tekmar Medlcal Ltd T25, portable ~ ~~~~~ ~~~ ~~ ~ 30 None 1 to 52 ;C Intrinsically €110 €48 For medical use. required safe design Sensor fitted to extendable lead. 22-mm adaptor for gas line supplied. 145 x 91 x 61 0-1 00% o2 None Tekmar 240 0.50 kg ( =2%) T7 fuel cell Teledyne Analytical Instruments$ 3306, pocket 114 x 54 x 29 - e: 1 3 None required €40 Accuracy over operating temperature range is the greater of ~ 5 % of reading or 52% f.s.Also available 330D: 0-100% scale. 0 to 52 "C US Bureau of €95 Mines approved €40 Oxygen deficiency alarm, no meter 0 to 52 "C - €170 scale. Directions for use printed on case. €40 Sensor fitted to extendable lead.Accuracy over operating temperat ure range is the greater of &5% of reading or 50.25% 02. Will operate in humidity from 0-100%. Sensor fitted to extendable lead. Accuracy over operating temperature range is the greater of =5% of reading or &0.25% 02. Will operate in humidity from 0-100%. Battery test switch. 0 to 52 "C Intrinsically €1 30 safe design €40 0 to 52 'C - €270 0-25% O2 ( z 2% f.s. None Microfuel cell 185 Class 83 at constant temperature) - - 9-V battery. Equivalent to Mallory TR-146X <13 None required 333, pocket 114 x 54 x 29 0 34 kg A (ear plug) Microfuel cell ( -, 12 months) Set for 19% Class 83 O2 by factory None Microfuel cell 185 Class B3 331 B, portable 152 x 210 x 95 0.85 kg 0-25% O2 ( = O 25% O2 at constant temperature) 1:13 Type ,C (4 off) batteries 3326, portable 152 x 260 x 95 1.7 kg 0-25% O z at constant (10.25% 0 2 AV Microfuel cell 185 For high Class 63 and low levels. Adjustable temperature) * Agents: Shandon Southern Instruments Ltd. t Agents: D. A. Pitman Ltd. $ Agents: Analysis Automation Ltd.

ISSN:0306-1396    

DOI:10.1039/AD9761300316

出版商:RSC    

年代:1976

数据来源: RSC

摘要:

320 OBITUARIES PYOC. Analyt. Div. CJzeitt. SOC. For further information write to: Fifth International Symposium on Gas Kinetics, UMIST, P.O. Box 88, Manchester, M60 1QD. Conferences and Courses Fifth International Symposium on Gas Kinetics J u l y 11-14, 1977, Manclaestev This Symposium is sponsored by The Cliemical Society Gas Kinetics Discussion Group and is to be held a t the University of Manchester Institute of Science and Technology.Third Pye Unicam Analytical Conference Novenabev 30-Decembev 2, 1976, Bivntivzgham The first day of this Conference will consist of a colloquium on atomic-absorption spectroscopy in inorganic analysis, the second day on atomic absorption and chromatography in clinical and biochemical analysis and the third day on gas chromatography. The Conference is to be held a t the Metropole Hotel, National Exhi bition Centre, near Birmingham, and delegates may book for whole days, or, if they wish, for one and a half days to include all the atomic-absorption papers or all the chromatography papers.The lectures have been invited from acknow- ledged experts in their own fields of analysis and tlic three I’lenary Lectures are as follows: “Mechanisms of Interference Effects in Electro- thermal Atomisation,” by Dr.J . M. Ottaway (University of Strathclyde, Glasgow) ; “Present Status of Atomic Absorption in Clinical Analysis,” by Dr. H. T. Delves (Institute for Child Health, London) ; and “Errors in Qualita- tive Gas Chromatography Analysis Due to Tiquid Phase Oxidation,” by Ilr. M. B. Evans (Chemical Sciences Department, Hatfield Poly- technic).Further information can be obtained from Mr. D. A. Gallagher, Pye Unicam Ltd., York Street, Cambriclge, CB1 2PX. The Monitoring of Hazardous Gases in the Working Environment Decembev 12-14, 1977, Lo.tzdolz This three-day international Conference is t o be held a t the City university, London, and is being organised by the Chemical Society in conjunction with the Health & Safety Executive, the Electrical liesearch Association and the City University.There will be two Plenary Lectures outlining the use of gas-monitoring systems for promoting health and safety in the working environment. Thereafter, the programme will be directed towards the monitoring of flammable and toxic gases that are normally present in industrial and laboratory situations and are accidentally emitted into the atmosphere, including such gases which may be formed in situ during fires.The themes of the conference are: ( a ) monitoring and detection of flammable gases and vapours; and (b) monitoring and detection of toxic gases and vapours. Papers will beOctober, 1976 PUBLICATIONS RECEIVED 32 1 welcomed on any aspects of these themes and in particular on: (i) present applications of gas- detection systems to specific industries; (ii) the needs of industry in the near future; (iiz) new methods of detection; (iu) the development of the technology of gas-monitoring ; and (v) generally applicable techniques.Those wishing to present papers should submit a title and 200-word synopsis not later than January 31, 1977, to Dr.John F. C'b Ti son, The Chemical Society, Burlington House, London, W1V OBN, from whom further information can be obtaincd. Atomic Absorption and Emission Spectrophotometry Decenabev 13-17, 1976, Loughbovough This course is to be held in the Department of Chemistry of the Loughborough TJniversity of Technology and the following topics will be covered : shapes of spectral lines ; nebulisation ; flames and reactions in flames; atomisation of samples in flame and resistively heated sources, e.g., carbon furnaces and rods for analysis of small samples, use of plasma torch; intensity of emitted radiation for thermal and fluorescent excitation ; sources for absorption spectra, the absorption process, chemical and physical inter- ferences, sensitivities ; instrumentation and applications of atomic emission, absorption and fluorescence.Further details can be obtained from Mrs. P. A. Bartram, Department of Chemistry, Loughborough University of Technology, Loughborough, Leicestershire, LE 11 3TU.

ISSN:0306-1396    

DOI:10.1039/AD976130320b

出版商:RSC    

年代:1976

数据来源: RSC

摘要:

October, 1976 PUBLICATIONS RECEIVED 32 1 Progress in Analytical Chemistry. Volume 8. Edited by Ivor L. Simmons and Galen W. Ewing. Pvoceedings of the Eastevn Analytical Symposium held in New York, October, 1975. Pp. viii + 336. New York and London: Plenum Press. 1976. Price $35.40. Publications Received Detectors in Gas Chromatography. Jii-i SevEik. Jouvfial of Chvomatogvaphy Libvavy, Volume 4.Pp. 192. Amsterdam, Oxford and New York : Elsevier Scientific Publishing Company. 1976. Price DflGO; $23.25. Analytical Applications of Complex Equilibria. J. Inczkdy. Ellis Hovwood Sevies in Analytical Chemistvy. Pp. 415. Chichester : Ellis Hor- wood Ltd. Distributed by John Wiley & Sons, Chichester. 1976. Price L17.50; $35.90. Digital Electronics and Laboratory Com- puter Experiments.Charles L. Wilkins, Sam P. Perone, Charles E. Klopfenstein, Robert C. Williams and Donald E. Jones. Pp. viii -$- 283. New York and Lon- don: Plenum Press. 1975. Price $18. Membrane Electrodes. N. Lakshminarayanaiah. Pp. x + 368. New York, San Francisco and London: Academic Press. 1976. Price $34.50; L20. Bibliography of Paper and Thin-Layer Chromatography 1970-1973 and Survey of Applications.Edited by K. Macek, I. M. Hais, J. Kopeck?, V. Schwarz, J . GaspariC and J . ChurAEek. JournaZ of Chvomatogvaphy Supplementavy Volume No. 5, 1976. Pp. xviii + 744. Amsterdam, Oxford and New York : Elsevier Scientific Publishing Company. 1976. Price Dfl200; $76.95. Trace Analysis. Spectroscopic Methods for Elements. Edited by J . TI. Winefordner. Chemical Analysis Sevies, Volume 46.Pp. xii + 484. New York, London, Sydney and Toronto: John Wiley &- Sons. 1976. Price A18; $29.45. Electron Spin Double Resonance Spectro- scopy. Larry Kevan and Lowell D. Kispert. Pp. x + 427. New York, London, Sydney and Toronto : John Wiley & Sons. 1976. Price i 1 8 ; $30.70. Advances in Mass Spectrometry in Bio- chemistry and Medicine.Volume 1. Edited by Alberto Frigerio and Neal Castagnoli. Pvoceedings of the 2nd Ifitevnational Symposium of Mass Spectvometvy in Riochemistvy and Medicine, Mario Negvi Institute fov Phavma- cological Reseavch, Milan, Italy, June, 1974. Pp. xxii + 586. New York: Spectrum Publi- cations, Inc. Distributed by John Wiley & Sons, Chichester. 1976. Price i27.20; $46.40.322 PUBLICATIONS RECEIVED PYOC.Auzalvt. Div. Chem. SOC Modern Fluorescence Spectroscopy. Vol- ume 1. Edited by E. L. Wehry. Pp. xvi + 238. New York and London: Plenum Press. 1976. Price $29.50. Organic Functional Group Analysis by Gas Chromatography. 1'. S. Ma and Athanasios S. Ladas. The Analysis of Ovganic Matevials, Numhev 10. Pp. x + 173. London, New York and San Francisco : Academic Press.1976. Price L6.80; $16.75. A Laboratory Manual of Qualitative Org- anic Analysis. H. T. Openshaw. Pp. xii + 92. London, New York and Melbourne; Cambridge Uni- versity Press. 1976. Price L2.75. The Determination of Sulphur-containing Groups. Volume 2. Analytical Methods for Thiol Groups. M. li. F. Ashworth. The Analysis of Ovganic Matevials, Numbev 2 . Pp. xii + 288. London, New York and San Francisco: Academic Press.1976. Price L9.80; $21.50. Practical High Performance Liquid Chromatography. Edited by C. F. Simpson. Pp. x + 315. London and liheine: Heyden & Son. 1976. Price L9.30; $18.50; DM59.50. Theory and Applications of Molecular Paramagnetism. Edited by E. A. Roudreaux and L. N. Mulay. I'p. xii + 510. New York, London, Sydney and Toronto: John Wiley & Sons.1976. Price k25; $42.60. Handbook of Analysis of Organic Solvents. VAclav Sedivec and Jan Flek. Ellis Hovwood Sevies in Analytical Chemistvy. Pp. 455. Chichester : Ellis Horwood Ltd. Distributed by John Wiley & Sons, Chichester. 1976. Price Ll8; $34.20. Quantitative Analysis by Gas Chromato - Josef NovAk. Clzvomatogva$hic Science Sevies, Volume 5. Pp.x + 218. New York: Marcel Deklter, Inc. 1975. Price SwFr58. graPhY Selected Annual Reviews of the Analytical Sciences Volume 4 Edited by Dr L. S. Bark, University of Salford The fourth volume continues the policy adopted in previous volumes of presenting critical reviews of selected topics in modern analytical science. Each of these reviews embodies the work considered pertinent over the four or five years up to 1974.'Advances in Voltammetric Techniques,' b y B. Fleet and R. D. Jee: Advances in Instrumentation and Recent Applications of Voltammetric Techniques in the Areas of DC Polarography, Pulse Polarogra phy, AC Polarogra p hy, Stripping Vol tammetry. 'High- frequency Electrodeless Plasma Spectrometry, ' by B. L. Sharp: Classification of Plasma Types; Emission Spectrometry- General Considerations; Nebulisers; The Inductively-coupled Radio-frequency Plasma Torch; The Microwave Plasma. 73 pages Price f 9.50 ISBN 0 85990 204 8 Members of The Chemical Society may buy personal copies at the special price of f3.00 provided they order direct and enclose remittance. Obtainable from the Publications Sales Officer, The Chemical Society, Blackhorse Road, Letchworth, Herts., SG6 1 HN

ISSN:0306-1396    

DOI:10.1039/AD9761300321

出版商:RSC    

年代:1976

数据来源: RSC