Front matter

 

作者:

 

期刊: Analyst  (RSC Available online 1979)
卷期: Volume 104, issue 1242  

页码: 073-078

 

ISSN:0003-2654

 

年代: 1979

 

DOI:10.1039/AN97904FP073

 

出版商: RSC

 

数据来源: RSC

 

摘要:

iv SUMMARIES OF PAPERS I N THIS ISSUE Septembev, 1979Summaries of Papers in this IssueIonic Polymerisation as a Means of End-point Indicationin Non- aqueous Thermometric Titrimetry.Determination of AcidsPart X. Acrylonitrile Indicator Reactions in theThe mechanism of the reaction marking the end-point when acrylonitrile isused as the indicator reagent in the thermometric titration of acids withsolutions of potassium hydroxide and alkoxides in alkanols has been investi-gated. Two indicator reactions occur : cyanoethylation of alcohols andanionic polymerisation of the acrylonitrile. The relative contribution ofthe two reactions is shown to depend on the nature and concentration ofalcohols in the titrand solution. Cyanoethylation is more important withrespect to end-point sharpness, when primary and secondary alcohols arepresent, and polymerisation predominates in the presence of tertiary alcohols.Anomalous titration values obtained in the determination of thiols andsulphanilamide can be explained by the effect of the structure of the samplecompound on the reversibility of its reaction with acrylonitrile.The experimental findings are used to devise combinations of titrand solventsand titrants leading to “ideal” titration curves.Keywords : Non-aqueous thermometric titrimetry ; end-point indication ; ionicpolymerisation ; acrylonitrile indicator reactions ; weak acid determinationE.J. GREENHOW and L. A. DAJER DE TORRIJOSDepartment of Chemistry, Chelsea College, University of London, Manresa Road,London, SW3 6LX.Analyst, 1979, 104, 801-811.Identification and Determination of Titanium Sulphide andCarbosulphide Compounds in SteelAs part of the experimental work to identify titanium compounds formed tocontrol sulphide morphology in high-strength low-alloy steels, heats withspecial additions of titanium were melted.It was determined that fivetitanium compounds could be distinguished from one another by differentialthermal analysis - evolved gas analysis techniques. Further, by analysingresidues obtained by using both the acid and the ester - halogen methods ofdissolving the matrix, it was possible to quantify the results for the fivetitanium compounds.The results showed that every experimental heat or experimental alloyexamined contained Ti,C,S, and that one sample contained both Ti,C,S,and y-Ti,S.Another unidentified titanium sulphide was thought to bepresent in one of the steels.Keywords : Titanium compounds ; high-strength low-alloy steel ; diflerentialthermal analysis ; evolved gas analysis ; ester - halogen extractionW. R. BAND1 and GEORGE KRAPFUnited States Steel Corporation, 125 Jamison Lane, Monroeville, Pa. 15146, USA.Analyst, 1979, 104, 812-821Se@tembcr, 1979 THE ANALYST VORGANICS ANALYSIS USING GASCHROMATOGRAPHY/MASSAND PROCEDURES MANUALby W.L. Budde and J.W. Eichelberger,Environmental Monitoring and Support Laboratory,US Environmental Protection Agency, Cincinatti.A practical guide for scientists, managers, andtechnicians who perform or contract to performanalyses of organic pollutants in water, air,sediment, or fatty tissue samples. It emphasizesquality control and the versatility of the powerfulgas chromatography/mass spectrometry tech-nique.In Press approx.242 pages0250 4031 8 8 approx. $22.00/f 1 1 .OOPublished by Ann Arbor Science Inc., and dis-tributed by John Wiley & Sons Ltd.SPECTROMETRY - A TECHNIQUESARCHEOLOGICAL CHEMISTRY:A Sourcebook on the Applications ofChemistry to Archeologyby Z. Goffer, Soreq Nuclear Research Centre,Yavne, Israel.A description of the ways in which chemistrycan beused as an aid in the study of archaeology. Itpresents a unified treatment that includes not onlymethods and techniques, but case histories as well.Results obtained from laboratories and theirinterpretation are emphasized and there isdiscussion of such topics as: ancient technologyand materials, decay and restoration, dating,prospecting, ancient temperatures and palaeo-climate, and authentication of antiquities.(Analytical Chemistry Series Vol.55)In Press approx. 390 pages0471 05156 X approx. $33.20/f 16.70INTRODUCTION TO POWDERSURFACE AREAby S. Lowell, Quantachrome Corporation.A highly specialized book - written by a leadingauthority - which provides a concise introductionto the theory and experimental methods used tostudy the surface area and porosity of solidsurfaces. Part 1 covers the important theoriesassociated with the measurement of surface area,along with the factors that affect it.Part 2 describesand compares various experimental methods.In Press appiox. 200 pages0471 04771 6 approx. $23.90/f 12.05KIRK-OTHMER ENCYCLOPEDIA OFCHEMICAL TECHNOLOGY 3rd Ed.VOl. 7Editorial Board: H.F. Mark and D. Othmer, both ofthe Polytechnic Institute of New York;C.G. Overberger, University of Michiganand G.T. Seaborg, University of California,Berkeley; Executive Editor: M. Grayson;This volume - covering Copper Alloys toDisinfectants and Antiseptics - spans the 15-yeargap between the previous edition and the presentone and brings thasubjects covered completely upto date. The new Third Edition has been completelyrewritten and updated. Two hundred and fifty newsubjects are included reflecting the growth andchanges in chemical technology through the1970s.In addition the new edition emphasizes major topicsof current concern to all industrial and appliedchemists.Some areas in which coverage has beenexpanded include chemical engineering, coatingsand inks, ecology and industrial hygiene, energyconversion and technology, plastics and elasto-mers, semiconductors and electronic materials,and water supply, purification, and reuse. TheThirdEdition also includes: approximately 1000 new orrevised articles by over 1200 distinguishedspecialists - both SI and Imperial units; ChemicalAbstracts Service’s Registry Numbers; and interimindexes to be supplied with every fourth volume.In Press approx. 900 pages0471 02043 5 approx. $1 20.00/f60.00(subscription price)(single-volume price) approx.$150.00/f 75.00Associate Editor: D. EckrothVi SUMMARIES OF PAPERS IN THIS ISSUE September, 1979Correction System for Spectroscopic Determination ofTrace Amounts of Cadmium Using the Atomic Faraday Effectwith Electrothermal AtomisationThe effect of background absorption of radiation on the signal obtained inFaraday-eff ect atomic spectroscopy has been overcome by comparing theenergies transmitted when the optical polarisers are in crossed and parallelconfigurations. Two systems were developed: one was a static system inwhich a Glan prism was used to divide the optical beam into two beams oforthogoually polarised radiation that were detected by two photomultipliers ;the other system used a rotating prism to rotate the plane of polarisation ofthe optical beam and a single photomultiplier with time-sharing electronicsto separate the required signals.Cadmium in a starch matrix was deter-mined using the spectral line a t 228.8 nm and losses of incident radiation ofup to 99% were corrected successfully.Keywords : Atomic spectroscopy ; electrothermal atomisation ; Faraday effect ;cadmium determination ; background correctionK. KITAGAWA, T. KOYAMA and (the late) T. TAKEUCHIDepartment of Synthetic Chemistry, Faculty of Engineering, Nagoya University,Furo-cho, Chikusa-ku, Nagoya, Japan.Analyst, 1979, 104, 822-830.Determination of Aluminium, Calcium, Iron and Magnesium inSewages and Sewage Effluent by a Rapid ElectrothermalAtomic-absorption Spectroscopic MethodThe methods currently used for the determination of aluminium, calcium,iron and magnesium in sewages and final effluent are time consuming.Arapid electrothermal atomic-absorption spectroscopic procedure utilisinghomogenisation of samples as the only pre-treatment has been compared withdigestion methods followed by flame atomic-absorption spectroscopic analysisin a statistically designed experiment. Low-sensitivity (secondary absorp-tion) lines were used for the electrothermal atomic-absorption analysis. Thetime saved by the use of this method is substantial and it could be usedadvantageously for routine analysis.Keywords Electrothermal atomic-absorption spectroscopy ; aluminium,calcium, iron and magnesium determination ; sewages and sewage ejluent ;pe-treatment by homogenisation ; low-sensitivity linesM.J. T. CARRONDO, J. N. LESTER and R. PERRYPublic Health and Water Resource Engineering Section, Civil Engineering Depart-ment, Imperial College of Science and Technology, London, SW7 2AZ.Analyst, 1979, 104, 831-836September, 1979 SUMMARIES OF PAPERS I N THIS ISSUEDetermination of Nitrate in Raw, Potable and Waste Waters byUltraviolet SpectrophotometryviiA method is proposed for the determination of nitrate in raw, potable andwaste waters using ultraviolet spectrophotometry. The use of an activatedcarbon filter at an elevated pH eliminates interference from organic matter,i.e., substances commonly assumed to be responsible for the related absorb-ances a t 275 and 210nm.The procedure also removes the interferences ofseveral cations that are precipitated out of solution. The development workleading up to the proposed method is discussed with reference to the relevantbehaviour towards organic matter and the nitrate ion of activated carbonmaterials. The method has a limit of detection of 0.006 mgl-1 N and atotal standard deviation of 0.016mg1-I N at a nitrate concentration of1.05 mg 1-l N in potable water. No statistically significant difference wasdetected between the proposed method and an established automated methodfor a wide range of samples.Keywords : Nitrate determination ; water ; waste water ; ultvaviolet spectro-Photometry ; activated carbonP. J. RENNIE and A. M. SUMNERNorth West Water Authority, Southern Division, Allport Road/Bridle Road, Brom-borough, Wirral, Merseyside, L62 6AB.and F.B. BASKETTERNorth West Water Authority, Directorate of Scientific Services, Dawson House,Great Sankey, Warrington, WA5 3LW.Analyst, 1979, 104, 837-845.Combined Gas Chromatography - Chemical-ionisation MassSpectrometry of Some Phthalate EstersA sample mixture of seven phthalate esters was analysed using combinedgas chromatography - chemical-ionisation mass spectrometry (GC - CIMS) .Separation of the various components of the mixture was effected by gaschromatography and subsequent identification by chemical-ionisation massspectrometry using methane and isobutane as reagent gases.Comparison of electron-impact (EI) spectra and the CI spectra was under-taken in order to illustrate the advantage of CIMS over EIMS in identifyingthese phthalate esters. CIMS with isobutane gives abundant quasi-molecularions, [M + HI+, with no adduct ions formed, in contrast to CIMS withmethane, and thus provides a means of distinguishing between isomericphthalate esters.Keywords : Phthnlate ester analysis ; gas chromatography - chenaical-ionisntionmass spectrometryJ. B. ADDISONAtlantic Regional Laboratory, National Research Council of Canada, 141 1 OxfordStreet, Halifax, N.S., B3H 321, Canada.Analyst, 1979, 104, 846-852

 

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