February , 1983 SUMMARIES OF PAPERS IN THIS ISSUEDetermination of Lead in Whole Blood by Electrothermal Atomic-absorption Spectrometry using Graphite Probe AtomisationAtomisation from a pyrolytic graphite probe, placed in a hot and constant-temperature HGA 70 furnace, was used for the direct determination of leadin diluted whole blood. Substantial reductions in the classical vapour-phaseinterference effects by up to 2% m/V magnesium chloride and calcium chlorideand 1.5% wz/V sodium chloride allowed the use of aqueous standard solutionsfor analytical calibration. Good agreement with national (UK) mean valueswas obtained for the analysis of quality control blood samples. The analyticalprecision is equivalent to that with conventional atomisation, but withimproved sensitivity.ixKeywords : Lead determination ; whole blood analysis ; electrotlaermal atomisa-tion ; atomic-absorptio n spectrometry ; probe atomisationSHREE K.GIRI, CHARLES J. SHIELDS, DAVID LITTLEJOHN andJOHN M. OTTAWAYDepartment of Pure and Applied Chemistry. University of Strathclyde, CathedralStreet, Glasgow, G1 1XL.Analyst, 1983, 108, 244-253.Analysis of Used Lubricating Oils for Wear Metals by WavelengthDispersive X-ray Fluorescence SpectroscopyAnalysis of used lubricating oils for wear metals by X-ray fluorescence spectro-scopy has always been difficult when the deterinination of many elements hasbeen required. Problems have been mainly caused by the nature of the sample,selection of standards and presentation of samples and standards to theinstrument in a suitable form.The method described largely overcomes theseproblems, is simple and convenient to use and is suitable for a wide range oflubricating oils. Repeatability is good and readily available standards can beused for calibration purposes. A correlation programme has been carried outusing flame atomic-absorption and direct-reading emission spcctroscopy onchromium, tin, lead, copper and iron.Keywords ; Wear metals ; lubricating oils ; wax medium ; X-ray fluorescencespectroscopyEDWARD SEARLE and CHRISTOPHER M. THOMPSONResearch laboratory, London Transport Executivc, 566 Chiswick High Road, London,W4 5RR.Analyst, 1983, 108, 254-260X SUMMARIES OF PAPERS I N THIS ISSUEDetermination of Lead in Soil by Graphite Furnace Atomic-absorption Spectrometry with the Direct Introduction of SlurriesFebruary, 1983A simple procedure is described whereby 5-20mg of a powdered soil aremixed with 25 ml of water and, while stirring, 20-pl aliquots of the slurryare pipetted into a graphite furnace electrothermal atomiser.Calibrationwith aqueous standards gives the total lead concentration of the soil. Thisis much simpler than the complex hydrofluoric acid digestion proceduresnormally required to obtain complete recoveries from soil. The over-allprecision of the analysis (8% relation standard deviation) is adequate forthis application, as is the sensitivity. A characteristic concentration ( A =0.0044) of 0.5 pg 1-1 is equivalent to 0.62 pg g-1 soil in a typical slurry.Keywords Lead determination ; soil analysis ; solid-sample introduction ;electrothermal atomisation ; atomic-absorption spectrometryKENNETH W.JACKSONDepartmentS1 1WB.of Chemistry, Sheffield City Polytechnic, Pond Street, Sheffield,and ALAN P. NEWMANDepartment of Geography and Environmental Studies, Sheffield City Polytechnic,Wentworth Woodhouse, Rotherham, S62 7T J.Afialyst, 1983, 108, 26 1-264.Re-usable Sampling Tubes for Monitoring Airborne MercuryVapour Concentrations : Sample Collection and Analysis byCold Vapour Atomic-absorption SpectrometryA re-usable sampling tube with silvered alumina as the collection medium isused to monitor concentration levels of airborne mercury vapour. Thedevice is ideally suited for personal sampling over long or short periods andits mercury blank is negligible.Analysis is by cold vapour atomic-absorptionspectrometry, using thermal desorption to release the mercury from thesampling tube for subsequent measurement, and a novel and convenientmeans has been devised for altering the measurement range of the analyticalsystem. A detection limit of 3 ng, equivalent to 0.5 pg m-3 for a 6-1 airsample, has been achieved but this could easily be improved further bymaking small modifications to the analytical apparatus. The sampling andanalytical procedures have been validated by comparing results obtained forsamples from mercury standard atmospheres and for factory samples withthose obtained by established procedures.Keywords : Airborne mercury vapour ; silvered alumina ; re-usable samplingtube ; cold vapour atomic-absorption spectrometryMARK TAYLORHealth and Safety Executive, London and Home Counties North Field ConsultantGroup, 14 Cardiff Road, Luton, LU1 1PP.Analyst, 1983, 108, 265-276February, 1983 THE ANALYST xiCOMPUTERS IN AUTOMATION ANDLABORATORY MANAGEMENTThe 5th Summer School ofAutomatic Chemical AnalysisA residential course at the University of Sussex,Falmer, Brighton, England.10th to 15th July 1983For the past four years this highly acclaimed coursehas been held at the Universiw College of Swansea.The new venue will provide an opportunity toexpand the scope of the course while retaining theproven format which includes a balanced mixtureof theory, practice and personal tuition.The programme will include lectures, tutorials andpractical sessions on the following broad topics:AutomationComputingData handlingManagementMicro-electronicsDetailed information and registration forms from:The 5th Summer School ofAutomatic Chemical Analysis,176A North View Road,London, N8 7NB.England.A Handbook ofICP SpectrometryM Thompson, Imperial College, London,andJ N Walsh, King's College, London.This important new book, the first t o bedevoted entirely t o inductively coupledplasma atomic emission spectrometry (ICPAES),reviews the theory and practice of this impres-sive analytical technique.Beginning with a review of the developmentof ICPAES, its analytical characteristics andadvantages and the instrumentation used, thebook goes on t o concentrate on how thetechnique can be applied t o the geological andenvironmental sciences.Appendices summarize the determination ofthe elements and list all publications concernedwith geological and environmental analysis byICPAES.Publication June 1983c.23Opp ISBN 0 2 16 9 1436 1 c.f 35.00 netBlackie Et Son LtdBishopbriggsGlasgow 664 2NZUK1 Scientific, educational, medical andindustrial laboratory equipment, servicesand supplies.2 Medical electronics.3 Analytical, Biochemical and ResearchInstrumentation.4 Electronic measuring and testingequipment.5 Measurement control systems andinstrumentation.IT ALLADDS UPTOTHE INT€RNATIONALLABORATORY SHOWi nco r po ra t i ng La bex and La bTec h no logy14 - 17 June 1983.€arts Court, London.Opening times: 14th-16th June. . . .0930 - 173017th June. . . .0930 - 1600Or anised by:Industrial an% Trade Fairs Limited,Radcliffe House,Blenheim Court,&-& Solihull, West Midlands B912BGTel: 021-70s 6707. Telex: 337073. r - i - - - - - - - - - m - Please send me further details on Tectronica '83. 7I NAME II COMPANY II ADDRE55 II A 2 1I Post to: Industrial and Trade Fairs Limited, Radcliffe House, IBlenheim Court, 5olihull, West Midlands B91 2BG England.A203 for further information.- - - - - - - - - - - - - . J ISee page xviii A207 for further information. See page xviixii SUMMARIES OF PAPERS I N THIS ISSUE February, 1983Extraction of Metals from Soils and Sewage Sludges byRefluxing with Aqua RegiaThe analysis of soils for total metal content using various acid digestionprocedures and flame atomic-absorption spectroscopy has been investigated.Refluxing with aqua regia was more effective than digestion in an open vesseland produced results comparable to those obtained by bomb digestion, themost vigorous method used.Refluxing with aqua regia extracted at least80% of the total chromium, copper, lead and manganese from sewage sludgesand sludge-treated soils. Analysis of the uncontaminated Canadian Referencesoils showed that a similar proportion of the total cadmium, iron and zincwas also extracted. Results for the analysis of six typical Scottish topsoilswere in agreement with the conclusions obtained with the Canadian soils.Keywords ; Trace metal determination; soils ; sewage sludges ; acid digestions ;atomic-absorption spectro$hotometryMICHAEL L.BERROW and WINNIE M. STEINDepartment of Spectrochemistry, The Macaulay Institute for Soil Research, Craigie-buckler, Aberdeen, AB9 2Q J.Analyst, 1983, 108, 277-285Febrzcary, 1983 THE ANALYST xiiiThe Market Leader for ICP Sourcesand AccessoriesNEW f I950 per unitA m t e d Hydride GeneratorRapid analysisof As, Bi, Sn, Sb, Se, Te, Ge, Hg, & Pb. Detectionlevels in region of . l PPB for above elements. Stable contin-uous hydride generation allows greater precision and relia-bility. Simplevisual checking of instrument performance.Sample levels measuredagainst background.Easy and simpleto interface to any plasmaor atomic absorption instrument.Additional pumpingchannel available for introductionof HzOz orIodide solution. Stand-alone or remote operation fromcomputer or auto sampler.Plasma-Therm ICPSources, which have become the standardof the industry are ideal sources for macro or trace, single ormultielement analysis. The heart of each system is a crystalcontrolled RF generator (27.1 2 or 40.68 MHz) designed forstability, reliability. serviceability, simplified control and safety.Automatic power control; impedance matching; and preciseflow meter control of plasma, auxiliary, and nebulizing gasesensure high spectroanalytical stability and reproducibility. Allsystems are easily adapted to most commercial spectro-meters.The recently introduced Compact Single Phase 40 MHzSystems available as 1 KW and 2KW versions offer increasedstability, reliability and performance.PlASMAmTHERM LTD213 Kangley Road Lower Sydenham sE26 5AR Tel: 01-778 6798A202 for further information.See Page xviiiSecond-hand -Copies? -RSC members have the advantage thatthey may subscribe to this journal at amost attractive discount price.The convenience of having yourpersonal copy, rather than borrowinga library copy, is obvious but there aremany other advantages of member-ship. Details of membership will besent if you write 200 in one of theboxes on the Reader Enquiry Servicepage.BUREAU OF ANALYSEDSAMPLES LTDannounce the availability ofNEWCERTIFIED REFERENCEMATERIALSfor twelve trace elementsinNICKEL BASE ALLOYSBCS/SS 345 for normal trace levelsBCS 346/SS 346A for enhancedtrace levelsFor full details write, telephoneor telex to:BAS Ltd., Newham Hall, Newby,Middlesbrough, Cleveland, TS8 9EATelephone: Middlesbrough 31 721 6Telex: 587765 BASRIDA200 for further information.See page xviii A209 for further information. See page xviixiv THE ANALYST Febrzlayy, 1983Analytical Sciences MonographsNo. 4 ElectrothermalAtomisation for AtomicAbsorption Spectrometryby C. W. FullerSince the introduction of atomic absorptionspectrometry as an analytical technique, by Walsh,in 1953, the use of alternative atomization sourcesto the flame has been explored.At the present timethe two most successful alternatives appear to bethe electrothermal atomiser and the inductively-coupled plasma. In this book an attempt has beenmade to provide the author's views on the historicaldevelopment, commercial design features, theory,practical considerations, analytical parameters of theelements, and areas of application of the first ofthese two techniques, electrothermal atomisation.Hardcover 135pp 0 851 86 777 4f 18.00 ($34.00) RSC Members fl3.50No. 5 Dithizoneby H. M. N. H. IrvingThe author of this monograph, who has beenclosely associated with the development ofanalytical techniques using this reagent for manyyears, and who has made extensive investigationsinto the properties of its complexes, has gatheredtogether a body of historical and technical data thatwill be of interest to many practising analyticalchemists.Hardcover 11 2pp 0 851 86 787 1f12.50 ($24.00) RSC Members f9.50No.6 lsoenzyme AnalysisEdited by D. W. MossThis monograph attempts to draw together the mostimportant experimental techniques which haveresulted from the modern recognition that enzymesfrequently exist in multiple molecular forms. Thismonograph also indicates the advantages andlimitations in isoenzyme studies of these modernexperiments.Brief Contents:Multiple Forms of Enzymes; Separation of MultipleForms of Enzymes; Selective Inactivation of MultipleForms of Enzymes; lmmunochemistry of MultipleForms of Enzymes; Catalytic Differences betweenMultiple Forms of Enzymes, Methods of ObtainingStructural Information, Selection of Methods ofAnalysis.Hardcover 171 pp 0 85186 800 2f12.00 ($23.00) RSC Members f9.00No.7 Analysis of AirbornePollutants in WorkingAtmospheresThe Welding and SurfaceCoatings Industriesby J. Moreton and N. A. R. FallaThis Monograph covers the following:Part I The Welding Industry: Airborne Pollutantsin Welding; Sampling of Welding WorkshopAtmospheres; Analysis of Welding Fumes andPollutant Gases.Part II The Surface Coatings Industry: Origin ofAirborne Pollutants in the Surface CoatingsIndustry; Collection and Analysis of GaseousAtmospheric Pollutants in the Surface CoatingsIndustry; Collection and Analysis of ParticulateAtmospheric Pollutants in the Surface CoatingsIndustry; Future Trends Relating to Sampling andAnalysis in the Welding and Surface CoatingsIndustries.Hardcover 192pp 0 85186 860 6f15.00 ($29.00) RSC Members f12.00No.8 The Sampling of BulkMaterialsby R. Smith and G. V. JamesThe literature of analytical chemistryexhaustively covers the many techniques nowavailable to the analyst.feature common t o a l l analyses, is in contrastonly sparsely documented. Comparatively feworiginal papers on this subject have beenpublished in the last fifty years; there are veryfew reviews available, and perhaps as a resultsampling is badly neglected in most instructionalcourses in analytical chemistry. ThisMonograph will go some way towards filling agap in the literature and should stimulateinterest in the development of sampling as afield of study.Brief ContentsIntroduction; Glossary of Terms; Establishment of aSampling Scheme; Sampling Theories; Apparatusfor Sampling; Sampling Methods; Appendices 1-4.Hardcover 200pp 0 851 86 81 0 Xf16.50 ($32.00) RSC Members f10.75Orders:RSC Members should send their orders to:The Membership Officer, The Royal Society of Chemistry30 Russell Square, London WC1 B 5DTAll other orders should be sent to:The Royal Society of Chemistry, Distribution Centre,Blackhorse Road, Letchworth, Herts. SG6 1 HNSampling, the oneThe Royal Society ofChemistrFebruary, 1983 THE ANALYST xvWiley Heyden J O U R ~ - _Announcing a new quarterly journalComputer En hanced CES SpectroscopyAn International JournalEDITOR-IN-CHIEF: REGIONAL EDITORS:Dr.H.A. Willis NORTH AMERICA: JA PA N:4 Sherrardspark Road, Professor G. Levy, Professor S. Sasaki,Welwyn Garden City,Herts, AL8 9JP, Syracuse University, School of Materials Science,England. Bowne Hall, Tempaku - Cho,EDITORIAL ADVISORY BOARDU.K.: Dr. A. Braithwaite, Nottingham, Dr. A. Carrick,Manchester, Dr. A.F. Fell, Edinburgh, Dr. B.J. Millard,BerkhamsteadU.S.A.: Professor R.E. Dessy. Blacksburg. Virginia,Professor P. Griffiths, Riverside, California,Dr. T . Hirschfeld, Livermore, California, ProfessorF. McLafferty, New York, Dr. R. Shaps. Philadelphia,Pennsylvania, Professor C.L. Wilkins, Riverside. California,Department of Chemistry,New York, NY 132 7 0.USA.To yohashi Institute of Technology,TOYO Lashi, Japan.GERMANY: Dr. W. Brernser, Ludwigshafen.Dr. K. Holland-Moritz, KolnJAPAN: Professor S. Minarni, Osaka, Dr. Y. Kudo,TokyoRUSSIA: Professor V.A. Koptyug. NovosibirskAIMS AND SCOPEComputer Enhanced Spectroscopy is devoted to therapid publication of papers describing novel practicalwork in which the performance of a spectrometer or achromatograph/spectrometer combination is enhancedwith a computer. Contributions centre on minicomputersand microcomputers, their application in the control andoperation of spectrometers, the acquisition andevaluation of data, the relevant software and user-developed programmes and the associated hardwareand interfaces. Papers on more sophisticated computersand spectrometers will also be welcome, especiallywhere the object is to interrelate the output of a numberof instruments or to involve data bases and SpectraCollections, or where there are implications for thesmaller installation.Short communications and Lettersto the Editor are also invited so that an interchange ofideas and results can be established. Reviews on topicsof special interest will be included.PAPERS APPEARING IN EARLY ISSUESH. Abe, T. Fujiwara, T. Nishimura, T. Okujama, T. Kidaand S. SasakiRecent advances in structure elucidation systems'CHEMICS'.J.D. Lipscornbe and R.W. SaloElectron Paramagnetic Resonance Spectrometer DataAccumulation and Reduction system for microcomputersR.S. Stradling, P.A. Ryan and J.D.WoodAutomated control of a mass spectrometer using a centralminicomputer and distributed microprocessors.H.D. Kronfeldt and S. WasserothComedy: A microcomputer based system for controllingpulsed dye laser experiments.D. Bianchi, F. Cavatorta and G. LenziData acquisition and spectrometer control with aRockwell AIM 65 microcomputer.D. Michailovic, J.F. Ryan and W.J. SiersternaA multipurpose computer interface for a scanning opticalspectrometer.P.L. Mains and M.J. HughesUsing a Hewlett-Packard minicomputer for the processingof gamma ray spectra from neutron activation analysis.A.F. Mehlkopf, A. Bax, J. Schmidt and T.A. TiggelrnanDesign, control system and software organisation ofmultipurpose nmr spectrometers.M . Carleer and J.P.WalgraeveMicroprocessor synchronisation of multichannel analyserto a monochromator.Subscription details: quarterly f50.00/$110.00A. Wiley Heyden journal published by John Wiley andSons Ltd.For a specimen copy and/or further informationplease write to the most convenient address below~~A201 for further information. See page xviixvi THE ANALYST February, 1983The Royal Society of ChemistrySpecialist Periodical ReportsEnvironmentalChemistry Vol. 2Senior Reporter: H. J. M. BowenThe first volume of this series was published in1975 and emphasized environmental organicchemistry whereas this second volume is deliber-ately slanted towards inorganic chemicals,covering the broad fields of the atmosphere andthe hydrosphere, soils, and human diets.Reviewers of all these subjects agree that far toolittle information is available on the chemicalforms of the elements in environmental reservoirs,thus laying down a challenge to analyticalchemists.A broad review of mycotoxins is how-ever included partly to redress the balance ofinorganic topics.Brief Contents :Inorganic Particulate Matter in the Atmos-phere :Methods of Sampling and Analysis; GeneralPhysical and Chemical Composition of Particu-lates; Characteristics of Emissions from SpecificSources; Atmospheric Transport and Dispersionof Particulates; Removal of Particulates from theAtmosphere; Effects of Airborne and DepositedParticulates; Future Research Needs and Con-clusions;The Elemental Content of Human Diets andExcreta :Outline of Ingestion, Absorption, Excretion;Met h odolog ica I Problems, In puts, 0 u tpu ts,Deficient Concentrations, and Oral Toxicities ofthe Elements;The Elemental Constituents of Soils:The Alkali Metals: Lithium, Sodium, Potassium,Rubidium, and Caesium; The Alkaline EarthElements: Beryllium, Magnesium, Calcium,Strontium and Barium; Titanium, Zirconium, andHafnium; Vanadium, Niobium, and Tantalum;The Lanthanides or Rare Earth Elements, andYttrium and Scandium; Molybdenum andTungsten; Chromium, Manganese, Iron, Cobalt,and Nickel; Copper, Zinc, and Cadmium; TheNoble Metals; Mercury; Boron, Aluminium,Gallium, Indium, and Thallium; Carbon, Silicon,Germanium, Tin, and Lead; Nitrogen, Phos-phorus, and Sulphur; Hydrogen and Oxygen;The Halogens: F, CI, Br, and I; Arsenic, Selenium,Antimony, and Bismuth; Thorium and Uranium;Radionuclides, Organic Soils;M ycotoxi ns :Biogenesis of Mycotoxins; The Importance ofMycotoxins in the Environment; Analysis ofMycotoxins; Occurrence in Food and AnimalFeed; Metabolism and Mode of Action of Myco-toxins; Control of Mycotoxins in the Food Chain;Occurrence, Distribution, and ChemicalSpeciation of some Minor DissolvedConstituents in Ocean Waters :Individual Elements; Additional Aspects ofChemical Speciation;Hardcover 301 pp 0 851 86 765 0Price f33.00 ($63.00) RSC Members f19.00Still available:Volume 1.Hardcover 21 2pp 0 851 86 755 3Price f15.50 ($30.00) RSC Members f7.50Special Package Price (Vols 1 & 2)Non-RSC Members only f39.00 ($75.00)Miscellaneous PublicationsThe Periodic Table ofthe ElementsThe Royal Society of Chemistry has produced acolourful wall chart measuring 125cm x 75cmcovering the first 105 elements as they existtoday.Each group is pictured against the same tintedbackground and each element, where possiblephotographed in colour and discussed withregard to its position in the hierarchy of matter.Additional information for each element includeschemical symbol, atomic number, atomic weightand orbits of electrons.This chart is particularly useful for both teachersand students and would make a worthwhileaddition to any establishment.Price f2.20 ($4.00) RSC Members f1.00Teacher Members f4.60 for 10Prices for The Periodic Table subject to VAT in the UK~~RSC members should send their orders to: The Royal Society of Chemistry, The Membership Officer, 30 RussellSquare, London WC1 B 5DT.Non-RSC members should send their orders to: The Royal Society of Chemistry,Distribution Centre, Blackhorse Road, Letchworth, Hens SG6 1 HN. Z,!M *The Royal Society of ChemistryBur lington HouseLondon W1V OBFe braary , I983 THE ANALYST xviiAnnual Reports on AnalyticalAtomic Spectroscopy Vol. 11Edited by M. S. Cresser and 6. L. SharpThis volume reports on current developmentsin all branches of analytical atomic emission,absorption and fluorescence spectroscopywith references to papers published andlectures presented during 1981. Much of theinformation is in tabular form for ease ofreference.Brief ContentsAtomization and ExcitationArcs, Sparks, Lasers and Low-pressure Dis-charges; Plasmas; Flames; ElectrothermalAtomization; Vapour Generation;InstrumentationLight Sources; Optics; Detector Systems;Instrument Automation; Complete Instru-ments; New Commercial Instruments;MethodologyNew Methods; Detection Limits, Precision andAccuracy; Standards and Standardization;ApplicationsChemicals; Metals; Refractories and MetalOxides, Ceramics, Slags, Cements; Minerals;Air Analysis; Water Analysis; Soils, Plants andFertilizers, Foods and Beverages; Body Tissuesand Fluids;Hardcover 388pp 0 85186 707 3Price f48.00 ($88.00) RSC Members f32.00RSC members should send their orders to: The Royal Society of Chemistry, The Membership Officer,30 Russell Square, London WClB 5DT.Non-RSC members should send their orders to: The RoyalSociety of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 1 HN. ,,~”.~The Royal Society of ChemistryBurlington HouseLondon WIV OBNNotice to SubscribersSubscriptions for The Analyst, Analytical Abstracts andAnalytical Proceedings should be sent to:The Royal Society of Chemistry, Distribution Centre,Blackhorse Road, Letchworth, Herts., SG6 I HN, EnglandRates for 1903 (including indexes)u K/Eire USA... 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