January, 19731 SUMMARIES OF PAPERS I N THIS ISSUEThe Direct Complexometric Determination of Metals in UnusedLubricating Oils and Additives by Automatic Non-aqueousPotentiometric TitrationMethods are described for the determination of calciuni, barium, zincand magnesium in any combination in additive concentrates and unusedlubricating oils. The samples are dissolved in a mixed aqueous - organicsolvent and titrated directly with 1,2-bis(2-aniinocthoxy)ethanc-NNN”’-tetraacetic acid [ethylene glycol bis( 2-aminoethyl) tetraacetic acid ; lS(;‘l‘A]or 1,2-diaminocyclohexane-NNN’N’-tetraacetic acid (DCTR), the end-pointsbeing indicated by metal ion sensitive electrodes. I3y use of a maskingagent and the appropriate buffer solutions the individual metals in anycombination can be determined following a maximum of three titrations.The results are compared with those obtained by established procedures.The accuracy of the complexometric methods is comparable with that o festablished wet-chemical methods, but the former are up to ten times fastcrand are therefore suitable for blending control.J.N. WILSON and C. 2 . MARCZEWSKIThe British Petroleum Company Limited, T 3 P ICesenrch Centre, Chert ,cy I C o m I ,Sunltury-on-Thames, Middlesex.Analyst, 1973, 98, 42-48.viiThe Direct Determination of Mercury by Atomic-absorptionSpectrophotometry at 184.9 nm by Using a Nitrogen- separatedNitrous Oxide - Acetylene FlameA modified atomic-absorption spectrophotonieter with a nitrogen-purgedoptical path has been used for the direct determination of mercury by atomic-absorption spectrophotometry, by using a nitrogen-separated pre-mixednitrous oxide - acetylene flame and electrodeless discharge lamp source.The high transparency of the fuel-rich flame below 200 nni permits the useof the principal resonance line of mercury at 184.9 nni for its determination.The sensitivity (for 1 per cent. absorption) enhancement obtained by using thisline rather than the 253-7-nm line is fifty-fold; detection limits for rnercury(1)and mercury(I1) of 0.02 p.p.m.and 0.05 p.p.m. are achieved in aqueoussolution.G. F. KIRKBRIGHT, T. S. WEST and P. J. WILSONChemistry Department, Irnpcrial College, London, SW7 2AY.Analyst, 1978, 98, 4!)-52.A Cold Vapour Technique for the Determination of Mercury inGeological Materials Involving its Reduction with Tin(I1)Chloride and Collection on Gold WireA technique for the determination of mercury in geological matcrials isdescribed in which mercury liberated from the sample by tin(ll) chloride iscollected on gold-wire clippings and determined by flameless atomic absorptionafter heating the gold in an easily constructed resistance furnace.Ihringthe heating stage the stream of air used to carry the atomic mercury vapouris diverted through a by-pass. The method gives a five-fold increase insensitivity over reduction with tin(I1) chloride alone and is free from non-atomic-absorption interferences when single-beam detectors are used. Thedetection limit is 0.001 pg of mercury and the coefficient of variation for0.080 pg of mercury is 3-9 per cent.P.C. HEAD and R. A. NICHOLSONInstitute of Geological Sciences, Geochemical Division, 64-78 Gray’s Inn Road,London, WClX 8NG.Analyst, 1973, 98, 63-66January, 19731 THE ANALYST ixCLASSIFIED ADVERTISEMENTST& ra& for classifid advertisewnts i s 369 a lint (or spaceequtvaient of a Line) with an extra charge of lop for theuse of a Box Number. Semi-displayed classifiedadvtrtisemenls arc €4 for single-column inch.Copy for classijied advertisements required not later thanthe r8th OJ the month preccding date of publication whichis on the 16th of each month. Advertisements should beaddressed to J . Arthur Cook, 9 Lluyd Square, London,WCIX 9MA. Tel.: 01-837 6315APPOINTMENT VACANTINSTRUMENTAL METHODS ANALYSTTo be responsible for the administration and operation of instrumentalnicthods of chemical analysis including U.V.emission and X-Raycwission and diffraction techniques.Tlit. successful candidate should hold an H.N.C. or above qualificationi i i cither chemistry or physics and should have previous experienceof this type of work and a knowledge of application to both metallica r i d nonmetallic samples.The Company can offer an attractive salary to the right candidate; i d fringe benefits available include four weeks annual holiday tothose aged 25 or above, contributory superannuation schrmc andtrw life assurance.Applications should he made i n writing giving details of age, qualifica-tions and experience to:John MasonINTERNATIONAL COMBUSTION LTD.Sinfin Lane, Derby DE2 9GJANALYSTrequired byThe EAST AFRICANPESTICIDES CONTROL ORGANISATIONto establish a small analytical laboratory for the veri-fication of pesticide contents of selected technicaland formulated pesticides.The successful candidatewill be a member of EAPCO which meets bi-annuallyto promote the safe and effective use of pesticidesand enforce conditions for the sale and proper use ofefficient and appropriate pesticide-products in EastAfrica.Candidates must have a good Honours degree inChemistry plus at least 4 years post-graduate ex-perience in Pesticide Chemistry. Knowledge of methodanalysis of major pesticides is essential. Salary is ina range of approxlmately €2890- €4050 at present rateof exchange.A Gratuity of 25% of total salary drawnis payable on completion of service.The post descrlbed is partly financed by Britain’sprogramme of a!d to the developing countries ad-ministered by the Overseas Development Admin-istration of the Foreign and Commonwealth Office.Apply toCROWN AGENTSM. Division, 4, Millbank, London,SWlP 3JDfor application form and further particulars statingname, age, brief details of qualifications and ex-perience and quoting reference number M3€/720450/AA D.~~LECTURES & COURSESUNIVERSITY OF SOUTHAMPTONDEPARTMENT OF CHEMISTRYAPPLICATIONS OF I’HO‘TOCHEMlS1’RYThe following self-contained short coursI’s driilirig with sonw appli-cations of photocheniistry arc open to m y applicwt.7th-12th January 1973 13iiviroiiinc.iit;iI arid Aii;ilvtic;il Aslwcts25th-30th March 1953 Polymvr Photochc.rriistry1st-6th April 1973 Iniagc,-forrning i’rocrssrsThe above courses are rcsitleiitial.In addition this followiiig shortcourses, offered as part of an M.Sc. programinc., arc opeii to partici-pants although in these cases accominotfatioii caiiriot I)v arr;uigc.tl.22nd-26th January 1973 Inorganic Photochrrnistry29th January-?rid FebruaryI973 Photochvmical Syri thrsis12th-16th February 195919th-ZSrd February 1973For furthrr details contact5th-9th February 1973 PhotobiologyPhotochemistry of DyrstuflsPhotochfwistry in thc Solid StatcDr. D. Phillips (A),1)epartinc:iit of Ch(-iiiistry,’The Univcmity,Southairiptori SO!) 6NH.BINDINGHave your back numbers of The Analyst boundin the standard binding case.Send the parts and the appropriate index(es)together with a remittance for f2.40 to:W. Heffer & Sons Ltd.Cambridge EnglandBOOKSM ON OG RAPHSREPRINTSorders for all publications ofthe Society (except journals)should be sent direct or througha bookseller to-THE SOCIETY FORANALYTICAL CHEMISTRYBook Department9/ I0 Savile Row,London, WIX IAx THE ANALYST [January, 1973ANALYTICAL CHEMISTRYSECTION MANAGERto join the Process Research Department of our General Chemicals Division at Widnes.Key tasks include thc development and application of analytical tccliiiiqucs to ;L witlc rangeof organic and inorganic compounds and liaison between I<cscarch ant1 I’rotluction units through-out the Division on matters relating to analytical methods.The man appointetl will be directlyrcsponsible to Mr C. Whalley, the current President of the Socicty for Analytic;iI Chemistrya n t l the Analytical Division of the Chemical Society.Candidates must have a sound knowledge of modern analytical procedures a n t 1 particularlyof instrumental methods. They must be able to rccognise the potcntinl ol thc Intwt tlcvclopnicntsi n analytical chemistry; some experience in managing ;t team o l gratluatcs mi(1 assistants iscsscntial.11 competitive starting salary is offered together with all the usual 1)cnclits of a I)rogressivecompany, including generous removal assistance where appropriatc.Applications, quoting reference LA.90, and giving details of ctlucation an(1 car(wr to (la tc,shoultl l)c ;ttltlressed t o :The Divisional Personnel ManagerLAPORTE INDUSTRIES LTDGeneral Chemicals DivisionMoorfield Road, Widnes, Lancs.WA8 OHESENIOR ANALYSTI<oche Products Limited have an opening for a Senior Analyst to be responsiblc for the analyticallaboratory work in their Dalry, Ayrshire factory. This laboratory provides qua1 ity controlinformation on raw materials and final products in synthetic vitamin and drug manufactures a tthis site ; it also offers some analytical service to the plant control antl investigation lahoratories.Applicrtnts must therefore have a t least fivc years’ postgraduate training ant1 experience in thisticltl (i.c.PhL, level) preferably in pharmaceutical chemistry, antl have hat1 experience in control0 1 staff. The person appointed will be required to take charge of a team o f some 16 assistants.ICoche l’roclucts Limited is a member of an international Swiss-bnsctl group of pharmaceuticala n t 1 chemical companies, and the conditions of service arc those to bc cxpcctctl from such anorganisation.Write i n confidence, quoting. rcfcrencc ’r J , for an application forln a n ( l further information, to theI )ircxtor o f Personnel a t :ROCHE PRODUCTS LIMITED15 MANCHESTER SQUARE LONDON W1M 6AJanuary, 19731 THE ANALYST xiBUREAU OF ANALYSEDSAMPLES LTD.NEW SAMPLESChemical StandardsNo. 384 Hycomax I11 Permanent Mag-net AlloyNo. 387 Nimonic 901 Alloy (12% Cr,60/, Mo) Also available asspectroscopic standard.No. 389 High Purity Magnesite stand-ardised for B,03No.390 High Tensile Brass (BS 2874CZ 114)announce the issue of the followingSpectroscopic StandardsNos. 666-670 Nodular Irons contain-ing increments of C, Si,Mn, S , Ni and MgFor further details please write to:-NEWHAM HALL, NEWBY,TS8 9EAor Telephone 0642 37216MI DD LES B ROU G HI TE ESSl D E, EN G LAN D.DECEN NlAL INDEXESTO THE ANALYST1906-1915t .. f2.101916-1925* . . f2.101936-1945* . . €2.101946-1955* . . €51956-1965" . . €6.75Bound in cloth boardst Paper boundObtainable fromThe Society for Analytical ChemistryBook Department9/10 Savile Row,London, WIX IAFSPECIALIST ABSTRACTJOURNALSpublished bySCIENCE AND TECHNOLOGY AGENCYAtomic Absorption and FlameEmission Spectroscopy AbstractsVol.5, 1973, bimonthly S24X-Ray Fluorescence SpectrometryAbstractsVol. 4, 1973, quarterly €24Thi n-Layer Chromatography AbstractsVol. 3, 1973, bimonthly S24Gas Chromatography-MassSpectrometry AbstractsVol. 4, 1973, quarterly $37Nuclear Magnetic ResonanceSpectrometry AbstractsVol. 3, 1973, bimonthly €30Laser-Raman Spectroscopy AbstractsVol. 2, 1973, quarterly €30X-Ray Diffraction AbstractsVol. 1-2, 1973, quarterly €30Neutron Activation Analysis AbstractsVol. 2-3, 1973, quarterly $30Electron Microscopy AbstractsVol. 1, 1973, quarterly S30Liquid Chromatography AbstractsVol. 1, 1973, quarterly €30Electron Spin Resonance SpectroscopyAbstractsVol.1, 1973, quarterly S30Sample copies on request from:SCIENCE AND TECHNOLOGY AGENCY,3 DYERS BUILDINGS, HOLBORN,LONDON, E.C.1, ENGLAND01-405 932xii SUMMARIES OF PAPERS I N THIS ISSUEThe Atomic-absorption Spectrophotometric Determination ofTotal Aluminium in Steel after its Dissolution in a Pressure BombA method is described for the determination of 0.001 to 0.14 per cent.of total aluminium in irons and steels, which does not involve fusion of anoxide residue. The iron or steel is completely dissolved by first subjectingit to conventional treatment with acid in an open beaker and then to attackby acid in a PTFE-lined bomb a t 200 "C. The oxide residue is completelydissolved by attack in the bomb with hydrochloric acid alone or with a mixtureof hydrochloric and hydrofluoric acids, the latter solvent being preferred.Iron(II1) is extracted from the solution of steel, 6 M in hydrochloric acid,with isobutyl methyl ketone and aluminium is then extracted from the aqueousphase buffered a t pH 4-7 with acetylacetone. The concentration of aluminiumin the organic phase is determined by atomic-absorption spectrophotometrywith a nitrous oxide - acetylene flame.Good results were obtained for thedetermination of aluminium in eleven standard irons and steels.J. B. HEADRIDGE and ALAN SOWERBUTTSDepartment of Chemistry, The University, Sheffield, S3 7HF.Analyst, 1973, 98, 57-64.[January, 1973A Study of the Variation with pH of the Solubility and Stabilityof Some Metal Ions at Low Concentrations in Aqueous Solution.Part IAtomic-absorption spectrophotometry has been used to determine traceamounts of metal ions in aqueous solution and to investigate the effect ofpH upon their stability, solubility and adsorption.It was found that for thefifteen metal ions investigated, namely those of aluminium, calcium, cobalt,chromium, copper, iron, magnesium, manganese, molybdenum, nickel, lead,strontium, titanium, vanadium and zinc, a pH of 1.5 or less was necessaryto ensure that all of these metal ions remained in solution a t low levels ofconcentration.A. E. SMITHImperial Chemical Industries Limited, Mond Division, Research and DevelopmentDepartment, Winnington Laboratory, Northwich, Cheshire, CW8 4D J.Analyst, 1973, 98, 65-68.Determination of Oxygen in Semiconductor Materials with aCryogenically Pumped Spark- source Mass SpectrometerA liquid helium cryogenic pump, which is mounted directly on to theion-source chamber of the mass spectrometer, is described.Base pressuresdown to about 8 x 10-10 torr are rapidly obtained within 1 hour of thecommencement of cryogenic pumping and pressures of about torr aremaintained during the analysis. The analytical blank for oxygen is shownto be directly dependent on the residual gas pressure in ths ion-sourcechamber and with liquid helium cryogenic pumping the blank for the deter-mination of oxygen in germanium is not more than 0.02 p.p.m.a. (parts permillion atomic).The quantitative performance of the method has been evaluated byusing germanium and silicon samples that had previously been analysedby infrared spectrophotometry.A mean standard deviation of 19 per cent.was obtained from measurements of oxygen present in silicon covering therange 11 to 35 p.p.m.a. The method has also been applied to the determinationof oxygen and carbon in indium phosphide, and satisfactory agreement a tthe 0-1 p.p.m.a. level has been found with results independently obtainedby gamma-photon activation analysis.J. B. CLEGG, I. G. GALE and E. J. MILLETTMullard Research Laboratories, Redhill, Surrey.Analyst, 1973, 98, 69-74January, 19731 THE ANALYST xiiiANNUAL REPORTSONANALYTICAL ATOMICSPECTROSCOPYVolume 1 , I W lTHIS comprehensive and critical reportof developments in analytical atomicspectroscopy has been compiled frommore than lo00 reports received fromworld-wide correspondents who areinternationally recognised authorities inthe field and who constitute the Editor-ial Board.In addition to surveyingdevelopments throughout the worldpublished in national or internationaljournals, a particular aim has been toinclude less widely accessible reportsfrom local, national and internationalsymposia and conferences concernedwith atomic spectroscopy.Volume 1 covers the year 1971.204 pagesPrice $5000Members of The Chemical Society may buypersonal copies at the special price of S.3-00.Obtainable from-THE SOCIETY FOR ANALYTICALCHEMISTRY,(Book Depart men t) ,9/10 Savile Row, London, W1X 1AFMONOGRAPHSFOR TEACHERSModernAnalyticalMethodsby D.BETTERIDGEand H. E. HALLAMModern Analytical Mefhods is one of TheChemical Society's series of paperbackmonographs which present concise andauthoritative accounts of selected welldefined topics in chemistry for those whoteach the subject at 'A' level and above andfor students of further and higher education.It discusses the principles underlying themost important methods of quantitative andqualitative analysis used today. Samplesfor analysis may arise from diverse sourcesand contain a variety of molecules orelements at various levels of concentration.Thus separation methods, organic reagents,nuclear, electrochemical, spectroscopic andtitrimetric methods are amongst those dealtwith in some detail. Within the bounds ofelementary algebra, equations are developedwhich show how the optimum conditions forthe application of a method may be deducedand conditional constants are usedthroughout.The numerous illustrationssupport the text by clarifying principles or byexemplifying important methods which aredealt with briefly because they do not involvenew principles.234pp 75 diagrams S2.00(CS Members €1.50)ISBN 0 85186 759 6Orders enclosing the appropriateremittance, should be sent to:The Publication Sales Oficer, TheChemical Society, Blackhorse Road,Letchworth, Herts SGS 1HN.For information on other titles in the serieswrite to: The Marketing Officer,The Chemical Society, Burlington House,London W1 V OBNxiv SUMMARIES OF PAPERS IN THIS ISSUEThe Determination of Oxygen and Carbon in Indium Phosphideby High-energy Gamma-photon ActivationHigh-energy gamma-photon activation has been used for the determina-tion of carbon and oxygen in single-crystal indium phosphide a t concentrationsin the range 0.01 to 0.1 p.p.m. m/m and less than 0.05 p.p.m. m/m, respectively.J. S. HISLOP, T. J. WEBBER and D. R. WILLIAMSAnalytical Sciences Division, Atomic Energy Research Establishment, Harwell,Didcot. Berkshire.Analyst, 1973, 98, 75-76.[January, 1973PARTICLE SIZE ANALYSIS1970THE Society for Analytical Chemistry has published i n this book all papers presented atthe Second Particle Size Analysis Conference, held in Bradford in September 1970, andthe full discussions on them.The 35 papers cover all aspects of research i n t o the subject, basically covering the4-year period since the f i r s t conference was held i n Loughborough i n 1966, and includeplenary lectures by the late Professor H. Heywood and by Professor K. Leschonski.The volume i s a companion to “Particle Size Analysis” - the report of the First Con-ference, also published by the Society.Pp. x + 430Price €7975Obtainable from-THE SOCIETY FOR ANALYTICAL CHEMISTRY,(Book Department),9/10 Savile Row, London, WIX IAFMembers of The Chemical Society may buy personal copies at the special price of f6.2