Meeting Abstracts Abstracts of Papers Presented at the 2007 Pittsburgh Conference

86 Pages·2014·7.95 MB·English

HindawiPublishingCorporation
JournalofAutomatedMethodsandManagementinChemistry
Volume2007,ArticleID71943,85pages
doi:10.1155/2007/71943
Meeting Abstracts
Abstracts of Papers Presented at the
2007 Pittsburgh Conference
PeterB.Stockwell
PSAnalytical,ArthurHouse,CrayfieldsIndustrialEstate,MainRoad,Orpington,KentBR53Hp,UK
Received7June2007;Accepted7June2007
Copyright©2007PeterB.Stockwell.ThisisanopenaccessarticledistributedundertheCreativeCommonsAttributionLicense,
whichpermitsunrestricteduse,distribution,andreproductioninanymedium,providedtheoriginalworkisproperlycited.
AUTOMATEDTRACEEXPLOSIVEEXTRACTION OPTIMIZINGSYSTEMPERFORMANCEIN
SYSTEMFORAIRPORTLUGGAGE HAND-HELDMINEDETECTION
AlanDavison
FredyOrnath
ArmyResearchLaboratory,199E.4ThStreetSuiteD,
TraceguardTechnologies,Inc.,P.O.Box4708,
Ft.LeonardWood,MO65473,USA
SegularIndustrialPark,PetachTikva42799,Israel,
GilPerlberg,JehudaYinon,RoyOrnath Effectiveandsafehand-heldminedetectionisdependenton
optimizing the man-machine interface. For this to happen
A system has been designed which is based on an adaptive, the operator must be optimally trained while the detector
flexible, glove-like membrane that forms a smaller volume must be designed to be easy to use. That means it must be
andhermeticenclosurearoundtheinspecteditem(checked simpletooperateinamannerthatthehumaniscapableof
or carryon luggage), with minimal stray air around it. This doing within a practical amount of training, and the infor-
minimizestheairquantitythatneedstobetreated,manip- mation provided by the detector must be reliably accurate
ulated,andexamined,whileincreasingthe“signal-to-noise” and easy for the operator to understand. For humanitarian
ratio. Clean air is introduced in the enclosure by pulsed jet deminers,trainingandmanyhoursofusemayeventuallyen-
nozzles while the air is collected by special suction nozzles. ablefittingthehumantothemachine,assumingamistakeis
Theblowingandsuctionnozzlesaremountedonthemem- notfirstmade.Butforsoldiers,whohavemanyothertasksin
brane,withmaximumefficiencyduetoproximitytothein- whichtheymustalsocontinuouslymaintainskills,thedesign
spected surface. Several compression/decompression cycles ofboththedetectorandthetrainingtaskmustbeassimple
allowextractionofaircarryingtracesofexplosivesfromin- ascanbesafeandeffective.
side the inspected item. The air is then passed through an The Army Research Laboratory in collaboration with
electrostatictraptocollecttheseparticlesandpassthemfi- Carnegie Mellon University, the University of Missouri-
nallytoatraceanalyzer,suchasanionmobilityspectrome- Rolla,andLincolnUniversityhasconductedvariousresearch
ter(IMS).Theautomatedtracecollectioniseffectedwithout studiespertainingtohand-heldminedetection.Theresults
manualintervention,usingadevicethatcollectstheparticles ofthesestudiesareprovidingguidanceforimproveddetec-
usingpneumaticmethodsandmechanicalagitation. tordesign,improvedtrainingtechniques,andbettertraining
Detectiontimeisbelow30seconds/perbaggage.Thesys- toolsandfacilities.Theobjectivesofthesestudieshavebeen
temallowsforremotestandoffoperation,decreasingtherisk tooptimizesoldierperformancewiththedetector.
of blast to personnel, whilst the false positive alarm rate is Thesestudieshavefocusedonmethodsforrejectingclut-
notmorethanthefalsealarmrateofthesensorsystem.This ter,influenceofdistractersonprobabilityofdetection,learn-
is based on testing conducted at Tel Aviv’s Ben Gurion In- ingdecayoverone-tothree-monthintervals,effectivenessof
ternationalAirport,whereover1000piecesofhandluggage computer-based instruction, and potential for supplement-
weretestedusingaSmith’sDetectionIonscan400ETD. ingdetectionwithvisualtechniques.
2 JournalofAutomatedMethodsandManagementinChemistry
Thispresentationwillsummarizethefindingsfromthese injection of the sample, and detection of analytes. Further-
studies and present recommendations for improving Sol- more,itissimpletomanipulatethecellularenvironmentin
dier’shand-heldminedetectionperformance. amicrofluidicspace,allowingforgoodtemporalresolution
for monitoring. Previously, we developed a device that can
OPTIMIZINGTHEIMMOBILIZATIONOFBOVINE maintain living cells in culture and monitor their secretion
PULMONARYARTERYENDOTHELIALCELLSINTO at6-secondintervalsbyanelectrophoresis-basedimmunoas-
POLY(DIMETHYLSILOXANE)MICROCHANNELS say.Thedevicehasbeenappliedtomonitoringinsulinsecre-
tionfromsingleisletsofLangerhansoverperiodsof2hours.
DanaSpence Inthepresentwork,wedescribedevelopmentsthatallowthis
device to be used for monitoring over periods of 1–5 days.
WayneStateUniversity,5101CassAvenue,Detroit,
Previously, long-term continuous monitoring on the chip
MI48202,USA
was limited by degradation of reagents and electrophoresis
buffers. To resolve this problem, in the modified chip, all
A microfluidic-based circulatory vessel comprised of bo-
reagents were continuously perfused into the device with a
vine pulmonary artery endothelial cells (bPAECs) within
gaspressuresystem,soonlyfreshreagentswereusedforanal-
poly(dimethylsiloxane) PDMS-based channels is described.
ysis. The introduction of particulates, which clog the mi-
Here, the optimal concentration, incubation temperature,
crofluidic channels, prevented long-term immunoassay sta-
andperiodofincubationtimeforfibronectinandbPAECs,
bility.Thesourceoftheparticulateswasdeterminedtobea
two components of the immobilization, are described. To
componentofthegaspressuresystemandwasthenreplaced.
optimize the number of viable cells adhered to the chan-
Failureoftheelectricalrelay,whichcontrolledthesamplein-
nels, varying concentrations of fibronectin ranging from
jection,alsohinderedtheimmunoassaystability;thisprob-
1μg/mL to 500μg/mL were incubated in a PDMS-coated
lem was solved by using a relay rated for longer operation
24-well sterile plate, aspirated off, and a cell suspension
(1×109cycles).Withthesemodifications,theimmunoassay
(>50,000cells/mL) was added to each well. The incubation
had a 4% RSD over 24 hours of continuous operation and
time(0to90minutes)andtemperature(25◦Cto37◦C)were
adetectionlimitof0.9nM.Thelong-termmonitoringchip
also examined in a similar manner. For bPAECs, the opti-
willnowbeusedfornovelexperimentsthatrequiremeasure-
mal period of cell incubation on fibronectin-coated PDMS
mentsofslowlydevelopingphenomenaofisletssuchastem-
andtheappropriatedensityofcellsuspensionforconfluency
poralchangesthatresultfromtimeincultureandeffectsof
wereestablished.Resultssuggestthatfibronectinconcentra-
lipids.
tion, as well as incubation temperature, impacts the num-
ber and viability of cells that adhere to the PDMS surface.
Fibronectin concentrationwasdetermined tobeoptimal at ON-SITESPOTSAMPLINGOFWATERUSINGSPME
50μg/mL and a 10% increase in the number of viable cells FIBERSANDPDMSTHINFILMSWITHACONTROLLED
was observed when the incubation temperature was raised AGITATIONTECHNIQUE
to 37◦C. A correlation exists between the number of viable
JanuszPawliszynandZhipeiQin
cells on the PDMS and an increase in the incubation time
of the cells, as well as an increase in bPAEC density. The
DepartmentofChemistry,UniversityofWaterloo,
optimal bPAEC incubation time was determined to be 120
200UniveristyAvenueWest,Waterloo,ON,CanadaN2L3G1
minutes with the bPAEC solution having the highest den-
sity(150,000cells/mL)becomingconfluentinthewellplate
Field sampling is often influenced by many environmen-
withinafewhours,whiledilutionsofthesolutionwerestill
tal variables such as temperature,turbidity, and water flow.
notconfluentafteranovernightincubation.Theincubation
WhenusingSPMEforfieldsampling,manyofthesevariables
timeoffibronectinhaslittleeffectontheaveragenumberof
canbeeliminatedorminimized.SPMEextractionisdepen-
cells that grow on the plate after 15 minutes. These results
dentuponextractionconditionssuchastemperatureandag-
werethenappliedtocreateamorereproduciblebiomimetic
itation. Temperature is not possible to be controlled in the
system using microfluidic technology for studying multiple
fieldbutwecancontroltheagitationofthefiberinthewater
celllinesinamicrochannel.
sample. Once the agitation is controlled, the concentration
of analytes can be quantitated because the thickness of the
AMICROFLUIDICDEVICEFORLONG-TERM
boundary layer, a zone of defined width between the fiber
CHEMICALMONITORINGOFLIVINGCELLS
andthebulkofthefluidwherenoconvectionoccurs,canbe
estimatedbasedonempiricalformulae.Portablehand-held
RobertT.Kennedy
stirringdeviceshavebeendevelopedusingcordlessdrills.A
DepartmentofChemistry,UniversityofMichigan, special“drillbit”wascreatedtoholdanSPMEfiberorapiece
930N.University,AnnArbor,MI48109-1099,USA ofPDMSthinfilmwhicharethetwoextractiontechniques
usedinourexperiments.Comparisonsbetweentheagitated
Microfluidicdevicesarevaluabletoolsforstudyingcellsand fiber,theagitatedthinfilm,thestaticfiber,andthestaticthin
arepotentiallycompatiblewithlong-termcellularmeasure- filmwerecompletedandshowedthattheagitatedthinfilm
ments.Itispossibletointegrateandautomateseveralfunc- hasthefastestextractiontimeandthelargestcapacity.This
tions on one chip, including sample collection from cells, is due to the high surface-to-volume ratio of the thin film
PeterB.Stockwell 3
compared to the SPME fiber. We are able to achieve rapid, [4] M. Vogel and U. Karst, “4-Nitro-7-piperazino-2,1,3-benzox-
reproducibleextractiononsiteusingthehand-heldstirring adiazoleasareagentformonitoringofairborneisocyanatesby
devicewithverylittlecost. liquidchromatography,”AnalyticalChemistry,vol.74,no.24,
pp.6418–6426,2002.
AFULLYVALIDATEDPASSIVESAMPLINGMETHODFOR
AIRBORNELOW-MOLECULARISOCYANATES LOW-COSTHAND-HELDANDONLINESPECTRAL
MEASUREMENTSYSTEMSFORENVIRONMENTAL
MartinVogel,HartmutHennken,andUweKarst MONITORINGAPPLICATIONS
DepartmentofAnalyticalChemistry,InstituteOfInorganic JohnP.Coates
AndAnalyticalChemistry,UniversityofMuenster,
MicroSpectralSensors,284MainStreet,Suite200,Wilton,
Corrensstraße30,Muenster48149,Germany
ME04294,USA
Isocyanates are important compounds in the field of occu-
In 2004, EPA warned against widespread pollution of lakes
pational hygiene. They show severe acute toxicity and have
andriversbymercury,dioxin,PCBs,pesticidepollutionand
alsostrongsensitizingproperties.Sensitizationusuallytakes
othercontaminants.TheEPAadministratorconfirmedthat
at least several weeks of exposure, but then even very low
nearly every time officials check for pollution, they find it.
concentrations below current occupational exposure limits
The Natural Resources Defense Council reported in 2005
(OELs)couldtriggerlife-threateningasthmaattacks.
thatunknownandillicitsewagesourcescontinuetodegrade
As for the determination of isocyanate concentrations
naturalhabitatsandtherebyincreasingtheriskofinfectious
in air, all routine and standard measurements are based on
bacteriological diseases in drinking and recreational waters
active sampling methods. In recent years, passive sampling
resulting in 19950 beach closing/advisory days in 2004—a
methods have proven great effectiveness and reliability for
tenfoldincreasesince1994.
airmonitoringapplicationsformanyairborneanalytes.Re-
Keepingthenation’swatersupplycleanandsafeisofin-
gardingisocyanates,thereareuptonowonlytwofullyval-
creasingconcern,andiscompoundedbytheinabilitytotrace
idatedpassivemethodsformethylisocyanate(MIC)known
illicit contamination sources. EPA is identifying endocrine
fromtheliterature[1,2],aswellasanearlyapproach[3]re-
disruptors from 87000 chemicals. Emerging contaminants
porting a passive dosimeter fortoluene diisocyanate (TDI).
enter waterways through the 90000 municipal, industrial,
Furthermore,amethodfordiffusion-controlledsamplingof
pharmaceutical,andagriculturalwastewatersystems.
TDIandhexamethylenediisocyanate(HDI)usingSPMEde-
Overthenextdecade,ithasbeensuggestedthatpotable
viceshasbeenreported.
waterresources,onaworldwidebasis,willbeamoreimpor-
Inthispaper,wepresentafullyvalidateddiffusivesam-
tantissuethanthecurrentconcernsaboutfossilfuels.Tak-
pling method for the determination of airborne methyl
ing into account all of the above comments, it is becoming
(MIC), ethyl (EIC), and phenyl (PhIC) isocyanates us-
increasinglyimportanttohaveeasilydeployableinstrumen-
ing4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole(NBDPZ)-
tationandsensingsystemsforthemonitoringofallaspects
coated [4] SDB filter tapes as collection material. Val-
ofwaterquality.
idation was carried out by active sampling using 1-(2-
MicroSpectral Sensors has developed a new miniature,
methoxyphenyl) piperazine (2-MP) as derivatizing agent.
multiparameter spectral measurement system as a low-cost
Samplingintervalswerebetween15minutesandmorethan
solution for field-based and online monitoring of environ-
8hours. Sampling rates ranged from 21.0mL/min for MIC
mentalcontaminationthreats.Theseareintendedtoprovide
downto11.5mL/minforPhIC.Thelimitsofquantification
real-time measurements of a wide variety of contaminants.
were1.4ppbforMICand1.3ppbforEICandPhICapplying
Thispaperwillreviewtheapplicationsofthisnewtechnol-
15-minutessamplingperiods.
ogytocurrentwater-qualitymeasurementmethods.
REFERENCES
ANEWAPPROACHTOLABORATORYINFORMATICS
[1] H. Henneken, R. Lindahl, A. O¨stin, M. Vogel, J.-O. Levin, RobertPavlis
and U. Karst, “Diffusive sampling of methyl isocyanate us-
ing4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole (NBDPZ)as LabtronicsInc.,546GovernorsRoad,Guelph,ON,
derivatizingagent,”JournalofEnvironmentalMonitoring,vol.5,
CanadaN1K1E3
no.1,pp.100–105,2003.
[2] P. von Zweigbergk, R. Lindahl, A. O¨stin, J. Ekman, and J.-O.
Alaboratoryusesarangeofinformaticscomponentsinclud-
Levin,“Developmentofadiffusivesamplingmethodfordeter-
ingLIMS,CDS,ELN,andECM/SDMS.Theroleofeachof
minationofmethylisocyanateinair,”JournalofEnvironmental
these components overlaps and it is not always clear which
Monitoring,vol.4,no.5,pp.663–666,2002.
[3] R.J.Rando,Y.Y.Hammad,andS.-N.Chang,“Adiffusesam- solutionisthebest.Forexample,whichsystemdoyouuseto
pler for personal monitoring of toluene diisocyanate (TDI) storechromatographyresults?
exposure—partI:designofthedosimeter,”AmericanIndustrial Eventhoughthesebetter-knownsystemshandlealotof
HygieneAssociationJournal,vol.50,no.1,pp.1–7,1989. the laboratories’ requirements, there are still key areas that
4 JournalofAutomatedMethodsandManagementinChemistry
untilrecentlyhavenoclearsolution.Managingmanualpro- FASTTRACKLIMS
ceduresandautomatingsmallinstrumentsaretwokeyareas.
Other than specific instrument data systems, the com- GeorgeGallatig,ArlieLowers,andDavidDeSchere
mon informatics products available today are not designed
forreal-timemanagement.Theyplayaroleinplanningthe TaratecDevelopmentCorporation,1620WashingtonLane,
work for the laboratory and in storing results, but they do WestChester,PA199382,USA
notgetinvolvedintheactualanalysisprocess.Consequently,
theirabilitytomanageworkflowandcontrolanalysisislim- What is special about fast track LIMS? Rigid adherence to
itedornonexistent.Real-timemanagementofthelaboratory principles of “fast” and “On track” phased implementa-
requiresacompletelynewapproach. tion focused on achievable, priority deliverables, rapid de-
This presentation will examine the role of each of the cisionmaking,constantmonitoringandcommunicationof
common informatics components discussing both their progressagainstdeliverablesandresolutionofissues,andso
strengthsandweaknesses.Itwillthenhighlightkeyareasthat forth.
arestilllackingautomationsolutions.Finally,itwillpresent Laboratory information management systems (LIMS’s)
anewconceptininformaticsthatintegratesthestrengthsof arehighlycomplexsystemsthatsupportmultipleusersand
existing components with new real-time management con- businessprocessesthatcrossorganizationboundaries.LIMS
trolcapabilities.Thisnewconceptredefinestheroleofinfor- interfaceswithamyriadofinstrumentssystemsfordatacol-
maticsinthelaboratory. lectionandhelpsachievebusinessgoalsthroughintegration
withotherbusinesssystems.ImplementationofLIMSisdif-
ficult. The road is littered with LIMS projects that did not
ELECTRONICLABORATORYNOTEBOOKSFOR
quitemeettheirintendedgoals.Projectsarefrequentlylate,
ROUTINEPROCEDURES
runoverbudget,orstopshortofproducingtheresultsthat
DaleSeabrooke wereusedtojustifytheoriginalproject.
FasttrackLIMSisaprovenmethodologythatgetsLIMS
LabtronicsInc.,546GovernorsRoad,Guelph,ON, implementation done quickly and keeps it “on track.” “On
CanadaN1K1E3 track” means that the implementation focuses on the cor-
rectendgoals,isaccomplishedwithefficientuseofbothtime
Mostelectroniclaboratorynotebookshavebeendesignedto
andresources,andproducesanenduringsolutionthatmeets
assistinR&Doperations.Manyofthekeyconsiderationsfor
businessneeds.
these ELNs are based on concepts involving collaboration,
Thispresentationwilldescribetheprinciplesandactiv-
documentation,andprotectionofintellectualproperty.This
ities involved in the fast track methodology. The paper will
type of design however does not lend itself well to the re-
address the full LIMS life cycle starting with requirements,
quirements of automating routine procedures. For routine
vendor selection, design and build, configuration, and data
analyses, there is a need to control the information that is
loadingthroughgoinglive.Thespeakerswilldiscusssomeof
recordedinordertoensurethatitfulfillsrequirementsand
thetypicalpitfallsawaitingaLIMSimplementationandde-
followsstandards.UnliketheR&Denvironment,itisnotac-
scribekeystosuccessorprovenwaysofaddressingthesepit-
ceptable or desirable to record any observation or any data
falls.Acasestudywillbepresentedhighlightingthecritical
thattheanalystfeelsisappropriate.Instead,therequirement
decisionsthatenabledfasttrackimplementationandreview-
isforamuchmorecontrolledsetofdata.
ingbarrierstooptimalexecution.
Inthissession,wewillhighlightkeyconsiderationswhen
investigatinganELNforroutineproceduresanddiscussthe
AUTOMATINGCGMPQCLABORATORIESUSING
benefits that can be realized by utilizing this technology as
AGMPELECTRONICNOTEBOOKSYSTEM
partofalaboratoryinformaticsstrategy.
JohnP.Helfrich
CONNECTINGTHELABORATORYTOTHEENTERPRISE
USINGWEBSERVICES
VelQuestCorporation,25SouthStreet,Hopkinton,
MA01748,USA
DavidShin
ThermoElectronCorporation,18CommerceWay,Suite5000, Pharmaceutical R&D and manufacturing have not changed
Woburn,MA01801 their fundamental paper-based infrastructure in decades.
The principal reason is that science by nature and regula-
One of the key problems laboratories are trying to solve is toryrequirementsresistchange.Recently,industryandFDA
how I make my results available to the people who need have been more aligned with respect to utilizing innova-
them.HowcanIhelpthemtomakedecisions?Laboratories tion and technology to bring manufacturing processes into
can have hundreds of different instrument and equipment the21stcentury.Leadingcompaniesareadoptinganewap-
typesfromdifferentvendorsallwithdifferentsoftwarepack- proach to “automating R&D and compliance,” that is, uti-
ages.ThistalkwilldiscusshowuseofwebservicesandXML lizing innovative technologies (such as ELN strategies) and
cansimplifythisprocessforthelaboratoryandensurequick building quality into the research, quality, and compliance
decisionsforthebusiness. infrastructures.
PeterB.Stockwell 5
The talk will discuss the current situation in cGMP lab asthetimesavingandconvenienceofmultiplespeciesmea-
operationsrelativetoFDAinitiativesinmanufacturingand surementthroughsamplepreparationandanalysisasanin-
thebroadopportunityforelectroniclabnotebookprocesses. tegratedstep.
Thepaperwillprofileaninnovative“method-centric”soft-
ware platform, designed to electronically execute and man- AUTOMATEDUPLCMETHODSDEVELOPMENT:
age laboratory protocols, yielding significant reductions in MONITORINGSELECTIVITYCHANGEBYCONTROLLING
overallmethodexecutioncycletimes,andelectronicallycap- STATIONARYPHASE,ORGANICMODIFIER,PH,
turealldataandmetadatainacommonrepository.Several ANDTEMPERATURE
largepharmaceuticalITinfrastructuredesignexampleswill
beoutlined. EricS.Grumbach,DianeM.Diehl,andJeffreyR.Mazzeo
WatersCorporation,34MapleStreet,Milford,MA01757,USA
EASINGSOFTWAREVALIDATIONAND
IMPLEMENTATIONTHROUGHTHEDEPLOYMENTOF UPLC allows chromatographers to get higher-resolution,
AMODERNSOFTWAREFRAMEWORK faster chromatographic methods by improving system effi-
ciency. In addition to improved efficiency, chemical factors
DavidLeitham
canbemanipulatedtoimprovetheselectivityandretentiv-
ity of a separation. In this lecture, we explore and measure
ThermoElectronCorporation,18CommerceWay,Suite5000,
howfactorssuchaspH,organicmodifier,temperature,and
Woburn,MA01801,USA columnchemistryaffectseparationsinUPLCbycombining
improvedefficiencywithmanipulationsofselectivityandre-
Oneof themost oneroustasksfora regulatedlabissimply
tentivitytodevelophigh-resolutionchromatographicmeth-
takingadvantageoftheirinvestment.Thecostandeffortof
ods.
validatingandimplementinglaboratorysoftwarehaveforced
The automation of this approach is implemented with
laboratoriestoupgradeonlyeverythreetofiveyearstoen-
a new, low-dispersion, 4-position column selection device
sureapositivereturnoninvestment.Byusingnewsoftware
which has been introduced to effectively and efficiently
technology,vendorscandeliversoftwarethatiseasiertoim-
screenmultiplevariables.
plement and validate and provides a real benefit to the end
In this lecture, we discuss the chromatographic effect
users.
of chemical factors on retentivity and selectivity. By under-
standingtheseeffects,wecanformulateasystematicscreen-
SIMULTANEOUSCOEXTRACTIONOFMULTISPECIESOF ingprotocolthatstreamlinesthemethodsdevelopmentpro-
DIFFERENTELEMENTSFROMBIOLOGICALSAMPLES cess.
BYCLOSED-VESSELMICROWAVEEXTRACTIONAND
DETERMINATIONBYINDUCTIVELYCOUPLEDPLASMA
ASYSTEMATICAPPROACHTOCONVERTUPLC
MASSSPECTROMETRYCOUPLEDTOLIQUIDANDGAS
CONDITIONSTOHPLCCONDITIONS
CHROMATOGRAPHY
XiaoweiSunandLorenWrisley
HowardM.Kingston
WyethResearch,AnalyticalandQualitySciences,
DepartmentofChemistry,DuquesneUniversity,600Forbes 401N.MiddletownRoad,PearlRiver,NY10965,USA
Avenue,MellonHall,Room308,Pittsburgh,PA15282,USA
UPLC has gained popularity since its introduction in 2004.
Organometallic species of mercury, lead and tin, and re- UPLC provides faster analysis time and higher efficiency
dox states of chromium play important roles in biological comparedtoregularHPLC.However,amethodthatistruly
as well as environmental processes because they are highly optimizedforUPLCcannotberundirectlyonatraditional
toxic and can be of anthropogenic and/or biogenic origin. HPLCsystem,mainlyduetopressurelimitations.Itcanbea
A simple and efficient coextraction method was developed dilemmaforanalystsorlabmanagerswhendecidingwhich
for simultaneous extraction of different species of mercury, techniquewillbeusedforaroutineanalyticalmethodsince
lead,organotins,andchromiumfrombiologicalsamplesby they are considered two different methods and there is no
using closed-vessel microwave-assisted extraction protocol. easy way to transfer (or translate) methods between UPLC
Thedevelopedextractionmethodwasvalidatedusingcerti- andHPLCtoensure,mostimportantly,equivalentselectiv-
fied reference materials of biological origin and applied to ity.
biological samples. The developed extraction method was AsystematicapproachtocovertUPLCconditionstotra-
validated by implementing EPA method 6800 as a diagnos- ditionalHPLCconditionswillbediscussed.Inthisapproach,
tictoolforspeciestransformationduringextractionand/or DryLab software was used to facilitate translation of UPLC
analysis using ICP-MS coupled with both liquid and gas conditions to traditional HPLC conditions. A combination
chromatography.Thiscoextractionmethodformultispecies offourtemperatureandgradientscoutrunswasperformed
analysisincorporatesmanybenefitsofmicrowaveextraction underUPLCconditions.Theretentiontimesandpeakareas
and method 6800 in terms of speed, low solvent use, accu- ofeachcomponentforeachexperimentalrunwereentered
racy of measurement, sensitivity, relative simplicity, as well into theDryLabsoftwaretoestablish aretention model for
6 JournalofAutomatedMethodsandManagementinChemistry
UPLC conditions. This DryLab retention model for UPLC ANOVELCHIP-BASEDSENSINGSYSTEM
wasverifiedbyactualverificationrunstocomparetothose DEVELOPEDFORHAND-HELDANDONLINE
predicated by DryLab. Next, the column parameters dwell SPECTRALMEASUREMENTS
volumeandflowratewerechangedfromUPLCparameters
totraditionalHPLCconditionswithintheDryLabsoftware JohnP.Coates
topredictseparationperformance.
In summary, our experiments showed that (1) DryLab microSpectralSensors,284MainStreet,Suite200,Wilton,
can be used to accurately optimize UPLC separations and ME04294,USA
(2) can accurately translate UPLC conditions to traditional
HPLC conditions and predict retention behavior very well The concept of a “spectrometer on a chip” has been dis-
(providedthattheselectivityofUPLCandHPLCcolumnsis cussed now for many years. Although certain specialized
thesame). measurement systems have been developed featuring cus-
tomizedelectronics,therehasnotbeenanyformofgeneral-
purposeinstrumentationbasedonachip-basedopticalspec-
COMBINATIONOFNEWLYDEVELOPED trometer.
TECHNOLOGYANDCOMMERCIALDETECTION A miniaturized spectral sensing system has been devel-
EQUIPMENTFORSIMULTANEOUSRAPIDACCURATE opedbasedonanopticalchipassemblymeasuringapprox-
DETECTIONOFCHEMICALWARFAREAGENTSAND imately8mm×1mm.Thesensor,basedona128-element
BIOLOGICALTOXINS optical array, is capable of providing spectral data from the
UVtothenearinfrared.Thedevicehasbeenintegratedinto
YasuoSeto,HirotakaUzawa,IsaacOhsawa,Kouichiro aspectralmeasurementenginethatincludessolidstatelight
Tsuge,MasayukiIzumi,MiekoKanamori-Kataoka, sources,on-boardsignalacquisition,dataconditioning,and
NaoyaEzawa,NobuoNakano,RyojiSekioka, spectral data extraction. The entire package has been de-
TakeshiOhmori,TetsuyaKawabe,YasuakiTakada, signed to be accommodated on a single board system with
andYasuoTakayama accompanyingelectronicsforinformationdisplayandcom-
munications.Thiscompactsystemdoesfeatureconventional
NationalResearchInstituteofPoliceScience, optics and is designed to be constructed from inexpensive
6-3-1Kashiwanoha,Kashiwa,Chiba277-0882,Japan molded parts. The result is an optimized, versatile sensing
system that can be easily integrated into different measure-
In crisis and consequence management against biological mentplatforms.
andchemicalterrorism,monitoring,detection,andidentifi- Thispaperwilldiscussthespectralsensingconceptand
cationareimportantforpreventionofterrorismoccurrence itsapplicationtospectralabsorptionandfluorescence-based
and minimization of damage. Among terroristic weapons, measurements.Initscurrentmanifestations,thespectralen-
chemicalwarfareagents(CWAs)andbiologicaltoxins(tox- gineisappliedtohand-heldandonlinesystemsthatfeature
ins) show toxic effect within one day, and so on-site detec- integratedsamplehandling.Theon-boardintelligencepro-
tion is desirable. We have evaluated commercially available vides the storage of a large number of methods that can be
on-sitedetectionequipmentforCWAsandtoxins,andelu- applied to a host of industrial, environmental, and biologi-
cidated shortcomings of the present on-site detection sys- calapplications.Examplespresentedwillincludebothwater-
tem conducted by first responders: low sensitivity against basedandorganicchemistries.
gaseousCWAsandtoxins,highfalsepositivefrequency,and
tediousoperation.Toovercomethedifficultyinreliableon- FROMLABORATORYTOPRODUCTION
site detection activity, we have developed three new tech- IMPLEMENTATIONONNEARINFRARED
nologies:monitoringtapemethod(MTM),counterflowin- SPECTROSCOPYFORONLINEDETERMINATIONOF
troduction atmospheric pressure chemical ionization mass MOISTUREINFLUIDBEDDRYERS
spectrometry(CFI-APCI-MS),andsugar-basedchipbiosen-
sor method (biosensor). MTM enables sensitive (LOD: sub PromitDas,GaryGolnick,andRossC.Herrold
mg/m3)andaccuratedetectionofbloodandchokingagents
within 1minute, using portable multiarray diffusion-type CDIPharma,2633FoundationDrive,SouthBend,
apparatus. CFI-APCI-MS enables very sensitive (LOD: sub IN46628,USA
μg/m3) and continuous monitoring of volatile (nerve gas
andblisteragent)andnonvolatile(vomitagentandteargas) It has been demonstrated that near infrared spectroscopy
CWAs,usingion-traptypeanalyzer.Biosensorenablessensi- (NIRS)isanidealtechnologyformoisturedeterminationin
tive(subn/mLlevel)detectionofricinandbotulinumtoxins, fluid bed dryers for the pharmaceutical industry. There are
usingspecificcarbohydrateligandsandsurfaceplasmonres- numerouspublicationstosupportthis.However,theactual
onancemeasurement.Bycombiningthesenewlydeveloped implementationinaproductionenvironment,tothebestof
technologiesandcommerciallyavailableequipmentsuchas ourknowledge,hasnotbeendemonstrated.Thispaperde-
ion mobility spectrometer, it is possible to detect thorough scribes in detail the several stages required for a successful
CWAsandtoxinssensitively,rapidly,andaccuratelywithout installation,fromfeasibilitytestinginalaboratoryenviron-
tediousoperation. mentthroughtothevalidationoftheentireprocess.
PeterB.Stockwell 7
DEVELOPINGROBUSTCHEMOMETRICTOOLS is often needed to maximize the ranges of several parame-
FORONLINESPECTROSCOPICDETERMINATIONOF ters that affect a tablet property. The aim of this work is to
“PHARMACEUTICS”:ACALIBRATIONTRANSFERAND find out an accurate and effective way of maximizing sev-
QUALITYOFDESIGNSTUDY eral parameter ranges simultaneously for a tablet property
development.
DongXiang,JasonTeelucksingh,RichardVivilecchia, Inthiswork,anaccuratemultivariatemodelwasfirstes-
RosarioLoBrutto,andYusufSulub tablishedtocorrelateatabletpropertywithalltheparame-
tersthatcouldaffecttheproperty.Threemethodswerethen
NovartisPharmaceuticals,OneHealthPlaza, used to maximize the ranges of all the effective parameters
Building401/B244D,EastHanover,NJ07936,USA sothatthedesiredtabletpropertycouldalwaysbeachieved
within the calculated ranges. The first method used Monte
Over the years, near infrared (NIR) spectroscopy has been Carlosimulationtoobtainalargeamountofsyntheticdata
coupled with multivariate techniques to determine concen- fortheextractionofparameterranges.Thesecondmethod
trationofactiveingredientsandexcipientsinpharmaceutical usedafunctionoptimizationalgorithmwiththemultivari-
drug products. Typically, quantitative aspect of chemomet- atemodelastheobjectivefunctiontoobtaintheparameter
rics analysisinvolves the generation of multivariate calibra- ranges.Thelastmethodusedresponsesurfacemethodology
tionmodelsfromasetofdatacollectedonaparticularNIR withpolynomialmodelstoobtaintheparameterranges.The
instrument. results of these three methods were compared for accuracy
Whenimplementingchemometrics-basedalgorithmsfor andeaseofuse.
online spectroscopic systems, it is critical that the dataset
of the calibration model be representative exhibiting the
full range of variations expected for the eventual unknown AUTOMATEDPHMEASUREMENTSOFPURGEAND
sample. The variations could be any spectroscopically sen- TRAPWATERSAMPLESFORUSEPAVOCMETHODS
sitive parameters, such as instrumental differences, instru-
mental drift, and chemical or physical properties of drug LauraChambers,JoanKillgore,andMichaelL.Duffy
substance and excipients. However, due to the difficulty,
if not impossibility, in incorporating foreseeable variations OIAnalytical,P.O.Box9010,151GrahamRoad,
intotheoriginalcalibrationmodel,solelyrelyingonsimple CollegeStation,TX77842-9010,USA
chemometrics-basedalgorithmsisrisky.Itisessentialforthe
pharmaceutical industry to adopt the development of spe- Many USEPA methods require that all drinking water and
cialized calibration transfer(SCT) algorithms as well as us- waste water samples be preserved with acid during the col-
ingthesealgorithmstoevaluateanyspectralvariancesinthe lectionprocesstopHlessthan2priortoanalysisforvolatile
data. organiccompounds(VOCs)bypurgeandtrap(P&T).Water
Inthisresearch,varioustechniqueswillbeevaluatedon sample preservation prevents degradation prior to analysis,
their efficiency and effectiveness in handling the problems andeachanalyticalmethoddescribesauniquepreservation
encountered during calibration transfer. The data analysis technique.Someofthemethodsrequiringacidpreservation
will be based on datasets collected on multiple NIR instru- prior to analysis are USEPA methods 502, 524, 624, 5030,
ments over a period of weeks. Spectral variances will be and8260.OtherregulatoryVOCmethods,suchastheMas-
investigated mainly based on measurement of solid dosage sachusetts volatile petroleum hydrocarbon (VPH) method,
fromsamples. offertheoption ofpreservingthesamplebyraisingthepH
ofthesampleabove11.
MULTIVARIATEPARAMETERRANGES Fornearlythirtyyears,theprocessofmeasuring,record-
MAXIMIZATIONFORTABLETPROPERTY ing, and reporting each sample’s pH level has been an en-
OPTIMIZATIONINTHEDEVELOPMENTOF tirely manual procedure. The technician or chemist must
APHARMACEUTICALFORMULATION open each sample vial, measure the pH manually using ei-
therpHindicatorstripsorapHprobe,recordthemeasure-
HushengYang ment in a logbook, and then include the measurements in
thefinalclientreport.Forhigh-throughputlaboratorieswith
AstraZenecaPharmaceuticals,1800ConcordPike, multipleP&Tinstrumentsanalyzingsamples24hourseach
Wilmington,DE19850,USA day, this practice can be extremely time-consuming, labor-
intensive,andexpensive.
Apharmaceuticaltabletusuallycarriesseveraldesiredprop- This poster describes a new instrument that fully auto-
erties to facilitate the delivery of the active pharmaceuti- mates the entire process of measuring, recording, and re-
cal ingredient (API). Since many tablet properties are of- portingthepHlevelforallVOCwatersamplestoverifythat
tenaffectedbyseveralparametersinrawmaterialsandpro- the pH level meets the requirements specified in regulatory
cesses, pharmaceutical companies have started using mul- methods.Thenewinstrumentimproveslaboratoryproduc-
tivariate analysis increasingly to achieve desired properties tivityandprofitabilitybyeliminatingthelaborandmaterials
in the development of a tablet formulation. To accommo- requiredformanualmeasurementofpHlevelsofVOCwater
date the most variability and flexibility in a formulation, it samples.
8 JournalofAutomatedMethodsandManagementinChemistry
REAL-TIMEMONITORINGOFPOLYMERHEATCURING ONLINEHPLC+HRGCCOUPLING:ANEW,FULLY
BYDIAMONDATRSPECTROSCOPY AUTOMATEDMETHODFORTHEDETERMINATIONOF
PESTICIDESINVEGETABLESAMPLES
JosephP.Lucania
JosepM.Gibert,AriadnaGalve,andRogerGibert
HarrickScientificProducts,Inc.,P.O.Box277,141Tompkins
Avenue(2ndFloor),Pleasantville,NY10570-3138,USA KONIKInstruments,12221Sw129Ct.,Miami,FL33186,USA
Epoxies were first introduced commercially in the early Determinationoforganiccontaminantsisregulatedbygov-
1950’s for the aerospace industry and are now widely used ernmentsallovertheworldandhasbeenincludedaspriority
for a variety of applications, including manufacturing of pollutantsintheEuropeanUnionlists.Pesticidesconstitute
commercialvehicles,electronics,inks,andvarnishes.Epox- averyimportantgroupofthesecompoundsowingtotheir
iesconsistoftwocomponents:aresinandacuringagentor hightoxicityandtheirextendeduseinagriculturalpractice.
hardener, which are tailored for specific properties such as The standard method for the analysis of pesticides in
adhesion,elasticity,andhardness.Forthebestperformance, vegetablesamplesischromatographywithselectivedetectors
the two components are mixed and cured under controlled andeventuallyGC-MS.Duetothecomplexmatrices,com-
conditions. plicated sample cleaning procedures are needed, previously
It is important to have real-time methods of analyzing to the HRGC analysis. Classical methods consist in a pesti-
theepoxycuringprocesstodeterminetheoptimumcuring cideextractionwithethylacetatefromthevegetable;thenthe
conditions for a given epoxy, for quality-control purposes, supernatantisevaporatedtodrynessandfinallydissolvedto
andtobetterunderstandthekineticsandunderlyingchem- obtainthesolutionreadytoinjectintotheGC.
icalprocesses.Spectroscopicmethodsforexaminingepoxies Inthiswork,anewapplicationofthepatentedTOTAD
curinginrealtimearenotcommonsincemanyepoxiesare interfaceforonlinecouplingHPLC-HRGCispresented.The
not readily removed from the windows or crystals used for interfacecouplinganHPLCtoanHRGCintheKONIKK2
transmissionorATRmeasurements. HPLC+HRGCsystemallowsthedirectanalysisofpesticides
TheintroductionofthediamondATRcrystalnowmakes infruitsandvegetables.
real-timemonitoringofepoxiescuringfeasible.Diamondis Thepesticidesareextractedfromthesample,previously
extremelyhardsothebondedepoxycansimplybescrapped ground, by a simple stirring and with a few milliliters of
off.Thispaperexaminesthecuringofanepoxyundercon- organic solvent placed directly in the injection vial. After
trolledelevatedtemperaturesinrealtimeusinganewheated the extraction, the supernatant is injected directly into the
diamondATR. HPLC system and the fraction of interest is transferred to
the HRGC by using the interface. With the addition of the
KONIK Robokrom HPLC autosampler and the full con-
ALOW-COSTAUTOMATICGRAVIMETRICTITRATION
trol through the Konikrom software, the complete analy-
SETUPFORCOLLEGELABORATORY
sis can be easily automated and performed in a few min-
utes, limiting the use of solvents while protecting sample
AlexanderY.Nazarenko
integrity.
The extraction step and the HPLC and HRGC parame-
ChemistryDepartment,SUNYCollegeatBuffalo,
terswereoptimizedtoobtainamultiresiduemethodwiththe
1300ElmwoodAvenue,Buffalo,NY14222,USA
selectivityandsensitivityrequiredforthelegislation.Finally,
themethodwasappliedtorealsamplesandresultscompared
With widespread availability of electronic balances, a novel intermsofselectivityandsensitivitywiththestandardmeth-
simpleapproachtogravimetrictitrationsbecomesanattrac- odsofextraction.
tive alternative to usual syringe-based automatic titrators.
ThetestedsetupconsistsofelectronicbalanceswithRS-232
or USB connection to the PC, a vessel for titrant solution, NEWMASSSPECTROMETRICSYSTEMFOR
deliverysystem,andanappropriatedetectorthatisalsocon- COMBUSTIONENGINEDEVELOPMENT:ULTRAFAST
nected to the same PC via suitable data logging device. A IN-CYLINDERMEASUREMENTOFOILEVAPORATION
numberofdetectorsforvarioustypesoftitrationweretested:
apHelectrode,apAgelectrode,Ptelectrodeforredoxtitra- SvenKrause,GerhardMatz,andMarcusGohl
tions,andafiberopticsprobeconnectedtotheCCD-based
spectrophotometer. Simultaneous collection of the mass of HamburgUniversityofTechnology,Harburger
titrantvesselsandcorrespondingdetectorreadingsproduces Schlossstrasse20,Hamburg21079,Germany
satisfactory titration curves suitable for automatic titration
withthree-digitprecision. Caremissionstandardsaregettingmorestringentinthefu-
Severalvariantsofdeliverysystemarediscussed.Modifi- ture.
cationsoftheusualtitrationproceduresaredescribed. To reduce the emission from combustion engines, the
Thesuggestedexperimentalsetuppresentsalow-costop- highlydynamicprocesshastobeinvestigatedinordertoun-
tionforautomatictitrationinacollegelaboratory. derstandthegenerationofpollutantsbetter.Thismeansthat
PeterB.Stockwell 9
overtime;adialysismembranewasaddedtotraptheenzyme
ontheelectrode.Theenzyme,glucoseoxidase(GOx),which
×102 is highly specific for •-D-glucose, was directly immobilized
40
onto the Pt electrode surface through two different immo-
35
30 bilization methods. An electrostatic/surface adsorption and
−1n)25 a polymer entrapment method were both used to immobi-
mi20
( lize the enzyme to the Pt RDE electrode. Glucose was de-
M15
RP10 tectedat650mVversusAgwirepseudo-referenceelectrode
usingathree-electrodeconfigurationincludingaPtwireas
360 720 1080 theauxiliaryelectrode.Experimentalconditionssuchasde-
Degreecrankangle tection potential, pH, temperature, and electrode rotation
DSP
rate were optimized for the electrostatic/surface absorption
method. The surface area of the electrode was determined
using chronocoulometry. The specificity of the GOx RDEE
for•-D-glucoserelativetosweetenersstructurallycloseto•-
D-glucosewasalsostudied.
ACKNOWLEDGMENT
Figure1
The research was financially supported by the Natural Sci-
enceSummerStudentResearchprogramatBenedictineUni-
thegascompositioninsidethecylinderhastobemonitored versity.
onlineforeachcombustioncycle.
Part of the online measuring system under develop-
EVALUATIONOFREAL-TIMEIMMUNO-PCR
ment is the Lubrisense 1200 mass spectrometer equipped
ASSEMBLAGESFORTHEFORENSICIDENTIFICATION
with a CFD optimized high-temperature direct inlet. The
inlet-systemconsistsofatransfercapillary,twodifferential- OFSEMENSTAINS
pressure stages, a heating system, and a pressure control
GeorgeDuncanandShaniKagen
device. Together with a high-speed data acquisition system
(12.5kHz), this system enables crank-angle-resolved moni-
DivisionofMath,Science,andTechnology,
toring of oil evaporation in the combustion chamber over
NovaSoutheasternUniversity,3301CollegeAvenue,
thefullspeedtorquerangeofanengine.Rapidonlinemea-
Ft.Lauderdale,FL33314,USA
surements will yield further information to understand the
processgeneratingpollutants.
Theidentificationofabiologicalfluidstainatacrimescene
as a semen stain is often critical to the assessment of the
DEVELOPMENTANDOPTIMIZATIONOFAGLUCOSE crime. This is particularly true in date rape cases, where
OXIDASE-MODIFIEDROTATINGDISKELECTRODE thevictimwasdruggedorincapacitatedandhavenodirect
memoryofasexualassault.Ifthereisnosperminasample,
AngelaA.PeverlyandNiinaJ.Ronkainen identificationofabiologicalfluidstainassemenisdifficult.
Allsemenstains,eventhosedevoidofsperm,willcontainthe
DepartmentofChemistry,BenedictineUniversity, proteinprostatespecificantigen,orPSA.PSAisatitshigh-
5700CollegeRoad,Lisle,IL60532-0900,USA est level in semen compared to other body fluids. This in-
vestigationcombinestheuseofthechemicalspecificityasso-
Enzyme electrodes combine the high sensitivity of electro- ciatedwithimmunotechniqueswithoutstandingsensitivity
chemicaldetectionwithspecificityoftheenzymeforitssub- attained in real-time PCR. Antibodies specific for PSA are
strate. Enzyme electrodes have gained popularity in analy- immobilized to surface of a vessel. When sample is intro-
sisofclinical,environmental,andfoodsamplesduetobeing duced,PSAinteractingwiththeboundantibodyisthenim-
relatively simple, inexpensive, and easy to prepare. Enzyme mobilized.AseconddetectionantibodywithacoupledDNA
electrodesalsoproviderapidanalysis,easilyregenerate,and moleculeisaddedwhichbindstothetotheimmobilizedpro-
arereusable.Addingarotationtotheelectrodeprovidescon- tein target. The sample vessel is then washed to free all un-
tinuousstirringofthebulksolutionandfastertransportof boundreagentsandtheDNAisamplifiedanddetectedwith
theanalytetotheelectrodesurfaceresultinginshorterdetec- afluorescenttag.Thereal-timePCRwasperformedtoam-
tiontimesandfasteroverallanalysis.However,rotatingdisk plifyanddetectfluorescentlytaggedDNA.Thereisnoneed
enzymeelectrodes(RDEEs)arelesscommonlystudiedand toquantitatetheDNA;simplythepresenceofthepreviously
notcommerciallyproduced.Rotatingdiskelectrodes(RDEs) immobilizedDNAindicatedthepresenceofPSA.Usingthree
modified with glucose oxidase (GOx) were constructed as different assemblage strategies provided by TATAA Biocen-
working electrodes for the amperometric detection of •-D- ter,thisstudycomparestheefficacyoftheseassemblagesin
glucose. The rapid rotation causes the enzyme to leach off detectingPSAinsemensamplesdevoidofsperm.
10 JournalofAutomatedMethodsandManagementinChemistry
THEDETECTIONOFSUGARSBY favorthatprocess.Becausethesedimentenvironmentinsalt
ELECTROGENERATEDCHEMILUMINESCENCEWITH marshesisexceedinglycomplicated,itispertinenttoinves-
RUTHENIUM(II)TRIS-BIPYRIDYLATGOLDANDGLASSY tigatetheconversionofinorganicmercuryintoorganomer-
CARBONELECTRODESINAFLOW-STOPTHINLAYER cury species. A fully automated GC coupled to atomic flu-
CELLSYSTEM orescencespectrometerwillbedescribedforthedetermina-
tionofmethylmercuryinsedimentsandsaltmarshplants.
NormanE.SchmidtandJacobS.Beveridge
NOVELAPPROACHINTHEPROFILINGOF
DepartmentofChemistry,GeorgiaSouthernUniversity,
VOLATILEORGANICCOMPOUNDSINWATER
P.O.Box8064,Statesboro,GA30460,USA
UTILIZINGTHEPURGEANDTRAPAUTOSAMPLER
The electrochemiluminescence (ECL) of Ru(bpy) 2+ was
3 TeriDattilioandEdPrice
studied in the presence of sugars at gold (Au) and glassy
carbon (GC) working electrodes having a surface area of TeledyneTekmar,4736SocialvilleFosterRoad,Mason,
7.06mm2. In an oxidative-reduction mechanism similar to OH45040,USA
that of Ru(bpy) 2+-Triproplyamine (TPA), a sugar reacts
3
with Ru(bpy) 2+ whose excited state (Ru(bpy) 2+∗) emits EPA methods 524.2 and 624 outline the general criteria
3 3
lightat610nm.Usingcyclicvoltammetryinaflow-stopthin for volatile organic compounds in water and wastewater
layercellanalysissystem,anECLsignalisobservedfroman- analysis. In recent years, laboratories have run into an in-
alytesolutioncontainingRu(bpy) 2+,Triton-X,buffer,anda strumental barrier in their efforts to increase throughput
3
sugar.AtbothAuandGCelectrodes,alinearECLresponse and productivity for the analysis of Volatile Organic Com-
is observed with increasing sugar concentration. A limit of pounds (VOCs). Conventional purge and trap technology
detection (LOD) of approximately 1mM was found for all hadreachedalimitwherethespeedcouldnotbeincreased
sugarsstudied.Solutionswerepreparedina1Mphosphate furtherwithoutseverelyaffectinganalyticalperformanceand
buffer pH 11, 1.0 × 10−8M Ru(bpy) 2+, and 0.01/0.02% quality. This paper compares the standard purge and trap
3
(v/v)TX-100. technologyandthenewtekmarpurgeandtrapshowingthat
reduced run time can be achieved while maintaining EPA
compliancewithimproveddataquality.
DETERMINATIONOFMERCURYSPECIESIN
PORTUGUESESALTMARSHESUSINGCAPILLARYGC:
ATOMICFLUORESCENCESPECTROMETRY NEWAPPROACHINTHEPROFILINGOFVOLATILE
ORGANICCOMPOUNDSINSOILUTILIZINGTHEPURGE
WarrenT.Corns,DerekW.Bryce,EduardaPereira, ANDTRAPAUTOSAMPLER
MiguelPardal,MonicaValega,andPeterB.Stockwell
TeriDattilioandEdPrice
PSAnalytical,ArthurHouse,CrayfieldsIndustrialEstate,
MainRoad,Orpington,KentBr53Hp,UK TeledyneTekmar,4736SocialvilleFosterRoad,Mason,
OH45040,USA
Salt marshes located near to industrialized areas can act as
EPAmethodsforthedeterminationofvolatileorganiccom-
natural sinks for trace metals. Anthropogenic metals, as-
poundsinsoilfollowingmethod5030and8260parameters
sociated with suspended particulate matter, can be trans-
can be a challenge when trying to ensure the fastest possi-
portedbytidalcurrentsandtrappedbyvegetationwithsub-
bleruntimewithoutsacrificingyouranalyticalintegrity.Two
sequentincorporationintosediments.Plantrootscaninter-
mainaspectsthatareoftencompromisedwhenoptimizinga
actwiththesurroundingsediment,exudingoxygen,andor-
purgeandtrapconcentratorandautosamplerarecarryover
ganic compounds that influence the distribution and avail-
and low-end sensitivity. Teledyne Tekmar is offering a new
abilityoftracemetals;however,theamountofmetalstaken
approach to purge and trap optimization that is achieving
up by the plants is dependent on the metal availability in
unprecedented performance. Data presented demonstrate
thesediment,andthisismodifiedbytherootactivity.Oxy-
advances in analytical abilities without sacrificing any data
genationofupperestuarinesedimentsdecreasesrapidlywith
integrity.
depth due to the consumption of oxygen in the oxidation
processoftheorganicmatter;however,saltmarshsediments
receiveanadditionalinputofoxygeninthesubsurfacelayers AUTOMATEDDISSOLUTION/REACTION
throughthewell-developedaerenchymaofsaltmarshplants MONITORINGINAVESSELSAMPLEDBYANEW
(halophytes) which transports oxygen from leaves to roots “SIPPING”AUTOSAMPLER
and consequently to the surrounding sediments. This sup-
SteveE.Hobbs
plyofoxygencanaltersignificantlytheredoxstatusofsed-
imentswithstrongrepercussionsonthebiogeochemistryof EksigentTechnologies,5875ArnoldRd,Dublin,
nutrientsandtraceelements,namely,mercury.Themethy- CA94568,USA
lation of mercury in salt marsh sediments is poorly docu-
mented,althoughabundantmicroorganismsandstrongre- Afastmethod forreal-time reactionmonitoring is demon-
doxgradientsbetweenrootsandsurroundingsedimentsmay stratedusingcapillarychromatographyandanewautomated