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Journal of Automatic Chemistry, Vol. 17, No. 3 (May-June 1995),
pp. 119-122
products
P.S. Analytical Ltd and Inchcape Testing Services
Since its formation in 1983, P.S. Analytical has
beenco-operating with its customers to solve complex
analyticalproblems. One of its initial clients was Inchcape
TestingServices in St. Helens who were one of the first companiesto
purchase the PSA Hydride Vapour Generator. Thisproduct and its
successors have been in continual use atInchcape Testing
Services.
In response to the increasing demand for lower and
lowerdetection limits for analytes such as mercury,
selenium,antimony and arsenic in environmental samples,
especiallygroundwaters, Inchcape has sought to enhance
itscapability in this area. Staff at St. Helens spent manyhours
evaluating alternative methods for this work. Afterthese tests and
co-operation with P.S. Analytical, Inchcapeagreed to purchase the
combined Merlin Excaliburinstrument. This allows a highly flexible
construction withextensive capabilities to analyse the various
elements indifficult matrices and with a high degree of accuracy
andprecision, even at sub ppb levels.
Inchcape Testing Services has the specific aim of beingthe most
skilled and innovative team of professionals inenvironmental
analytical measurement. Purchasing theP.S. Analytical Merlin
Excalibur instrumentation notonly provides quality instrumentation
for the job but alsoadds to the considerable resources of P.S.
Analytical’sapplications expertise.
Literature on the P.S. Analytical product range is availablefrom
P.S. Analytical, Arthur House, Unit 2.03 CrayfieldsIndustrial Park,
Main Road, St Pauls Cray, Orpington, KentBR5 3HP, UK. Tel.: 01689
891211; fax: 01689 896009.
Injbrmation about Inchcape Testing Services is available.from
Ken Hepburn, Technical Manager, Inchcape TestingServices
Environmental Laboratories, Lancots Lane, St. Helens,Merseyside WA9
3ES, UK..
Atomic-emission detector
Hewlett-Packard has published an index of HP
5921Aatomic-emission detector (AED) application notes andscientific
articles. The index is a resource for chemists toobtain information
on how the HP 5921A AED can beused to solve analytical Challenges;
it contains resourceintbrmation on subject areas that include the
following:
(1) Sulphur, oxygen, lead, nickel, vanadium, iron andboron in
the petroleum industry.
(2) Process impurities in the petrochemical and
chemicalindustries.
(3) Hydrocarbons, pesticides, organometallics and haz-ardous
waste in air, water and soil environmentalsamples.
(4) Characterization of unknown compounds in foods,flavours and
fragrances.
(5) Stable isotope labels in metabolite studies.
(6) Simplified quantitation using
compound-independentcalibration.
The index is available free of charge (quote 5963-6601E)fromPMG
Logistics, Attn. Petra Butter, P.O. Box 533, 2130 AMHoofddorp, The
Netherlands.
Analysis of VOCs in water
Perkin-Elmer has published a new application note whichdiscusses
the Japanese Standard Headspace Methodfor Analysisof VOCs in Water.
It summarizes and explains the simpleand highly productive static
headspace GC/MS procedureincluded in new regulations covering water
quality testing.It includes details of the instrumentation and
analyticalconditions, a method summary listing target VOCs,
andchromatograms and results tables illustrating replicateanalyses.
The advantages of headspace over purge-and-trap systems for
environmental water analysis are alsodiscussed.
Forfurther information, contact Perkin-Elmer Limited, Post
OffceLane, Beaconsfield, Bucks HP9 1QA, UK. Tel.: 01494 679269:fax:
01494 679332.
Clenbuterol screening
Fisons Instruments VG Organic have released newinformation on
clenbuterol screening in a new applicationnote: An Improved Method
For Clenbuterol Screening UsingHigh Resolution Selected Ion
Recording. Methodology whichextends the use of GC-MS by improving
the specificityof the technique using the high resolution
capabilities ofa magnetic sector mass spectrometer is described.
Usedas an anti-asthmatic and tocolytic drug in the treatmentof both
humans and animals, clenbuterol is a stimulantof the nervous system
and a fl2-agonist. Together withother -agonists, it also exhibits
growth stimulatoryeffects, leading to enhanced muscle and decreased
fatdeposition. Consequently, clenbuterol is used to stimulategrowth
in farm animals, and by athletes seeking enhancedperformance from
the protein anabolic response to thedrug. Such abuse within sport
is attracting the attentionof various sporting authorities, and
thus requires preciseinvestigation and monitoring.
Dosage is typically in the gg/kg range of human
bodyweight--therefore a sensitive but specific method is neededto
check for the presence of clenbuterol. The proceduredescribed in
the application note is sufficiently specific tobe used for the
analysis of heavily contaminated urinesamples which have undergone
enzymatic hydrolysis.
For more information contact IAS, Queens Avenue,
Maccleeld,Cheshire SKIO 2BN, UK. Tel.: 0162543434&fax: 01625
434335.
119
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New products
Pharmacokinetic study using HPLC/MS/MS
Fisons Instruments VG Organic’s Quantitative HPLC/MS/MS In
Support OfA Pharmacokinetic Study has recentlybeen announced. Mass
spectrometry has long beenemployed as a highly sensitive and
specific tool forpharmaceutical studies, and its use in this field
has beenwell documented. The greater prominence ofLC/MS/MSis
rapidly becoming evident from drug discovery throughmetabolism and
toxicological studies to drug manufacture.An explanation tbr this
increased application is theintroduction of the atmospheric
pressure ionizationtechniques, electrospray (ES) and atmospheric
pressurechemical ionization (APcl), in addition to improvementsin
computer technology. Electrospray is an extremelypowerful method
used in the analysis of thermally labilecompounds due to the
relatively mild ionizing nature ofthis interface. This is
specifically important in the areasof drug metabolism and
pharmacokinetics, where com-monly occurring metabolites such as
glucuronides andsulphates are encountered.
Formerly, ionization techniques, such as thermospray
andplasmaspray, caused these conjugated metabolites tofrequently
revert to their aglycones, losing all theirmolecular mass
intbrmation. Electrospray is more sensitivethan fast atom
bombardment and thermospray due to thegreatly decreased level of
background ions and its higherionizing efficiency. Besides their
high sensitivity andspecificity, the atmospheric pressure
ionization techniquesare also so reproducible and robust that they
lendthemselves readily to automation. These highly
beneficialligatures are described in Fison’s new literature, in a
studywhich uses HPLC/MS/MS in support of drug discovery.
For more information contact IAS, Queens Avenue,
Macclesfield,Cheshire SKIO 2BN, UK. Tel.: 01625 434343; fax:
01625434335.
SEM developments
Oxtbrd Instruments Scientific Research Division produceslarge
movement, custom produced stages for the SEM(Scanning Electron
Microscope). This is particularlyimportant, for example, for the
semiconductor industry,where stages can be produced that hold
watirs withdiameters up to 12 inches, for techniques such as
DRT,probing and EBIC. Stages can also be built for
otherapplications, including electron beam lithography and
theexamination oflarge and heavy samples, such as engineer-ing
components. Ifthe SEM chamber is too small, replace-ment chambers
can also be supplied.
Detailed specifications are, naturally, dependant on
theindividual design but typically will offer sub-micronprecision.
Technologies available include microsteppingmotor drive with
software controlled and co-ordinatestorage, piezo electric
movements, linear encoders, a laserinterferometer system and
microprobing.
In addition, the company also produces a wide range ofstandard
and custom stages for the SEM and TEM, whichinclude heating
cooling, and tensile facilities.
All Oxford Instruments customers now have free andunlimited
access to the company’s specialist engineeringand applications
support hotline.
For further information contact Oxford Instruments
ScientificResearch Division, Old Station Way, Eynsham, Witney,
OxonOX8 1FL. Tel.: 01865 882855," fax." 01865 881944.
Net Communication
The benefits of the Internet have now been realized
foranalytical chemists with the creation of LabNET, adedicated
global platform providing a plethora of facts onthe latest product
and technological developments.
LabNET goes on-line in May 1995. It is an uniqueinteractive
response mechanism giving access to manu-facturers throughout the
world. Clear step-by-stepinstructions guide visitors quickly
through to their selectedareas where exciting graphical and textual
data may beanalysed, down loaded, printed or re-visited as often
asrequired. Direct links to companies ofyour choice are
alsoavailable, enabling you to discuss enquiries via e-mail forthe
cost of a telephone call.
LabNET information is available on the 01799 516610or e-mail
[email protected].
Thermal analysis applications
Three new thermal analysis application notes are availablefrom
Perkin-Elmer.
PETAN 54--Epoxy Cure Characterization using SimultaneousDynamic
Mechanical Analysis-Dielectric Analysis DMA-DEAdescribes recent
developments in polymer compositemanufacturing which have resulted
in higher quality andlower cost epoxy composites. The method and
instru-mentation used to simultaneously characterize the
curingprocess of epoxy using the Perkin-Elmer DMA 7eDynamic
Mechanical Analyzer with the cup and platemeasuring system and the
Micromet Instruments EumetricSystem 11 Microdielectrometer are
outlined.
PETAN 55-Prepreg Cure Characterization using SimultaneousDynamic
Mechanical Analysis-Dielectric Analysis DMA-DEAlooks at the effects
of batch-to-batch material variabilityand changes in the curing
process on final quality of partsmade from thermosetting prepregs.
The note outlines thesimultaneous characterization of the
mechanical anddielectric curing process of an EPON 828 prepreg
usingthe Perkin-Elmer DMA 7e Dynamic Mechanical Analyzerwith the
parallel plate measuring system and theMicromet Instruments
Eumetric System Micro-dielectrometer.
PETAN 56--Determination of the Curing Kinetics of an
EpoxyAdhesive using Isothermal DSC Kinetics Software outlines
theuse of DSC isothermal software for the 7 Series/UNIXsystem to
obtain the curing parameters for an epoxyadhesive.
Forfurther information, contact Perkin-Elmer Limited, Post
OffceLane, Beaconsfield, Bucks HP9 1QA, UK. Tel.: 01494 679269;fax:
01494 679332.
120
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New products
Electrospray LC/MS analysis
An application note from Fisons Instruments VG Organicof
Altrincham, Cheshire, describes the development of aselective and
sensitive method for detecting glycopyrrolate,a quaternary ammonium
anticholinergic drug banned inhorseracing due to its respiratory
enhancing properties.Eleclrospray LC/MS Analysis of Glycopyrrolate
in Equine Sportdescribes a rapid and reliable technique
appropriateglycopyrrolate quantification at the low ng/ml level
usingthe closely related mepenzolate bromide as
internalstandard.
Abuse of glycopyrrolate has caused great concern tohorseracing
authorities worldwide, with several positivecases having been
detected. Administration of the drugusually takes place by
intravenous or intramuscular routesat low levels (approximately 4
pg per kg). Excretion inurine is rapid, taking place in less than
eight hours, andpredominantly in the form of the parent drug.
AlthoughELISA kits are commercially available for this purpose,and
provide an ettctive preliminary screening proceduretbr drug
control, the kits are insufficiently selectivedrug detection in
sport, where it is mandatory to identifythe drug present in the
body fluid under test.
Mass spectrometry, however, offers high selectivity, andwhen
coupled with the appropriate ionization method forthe sample under
scrutiny, also provides high sensitivity.Initial mass spectrometric
methods developed for glyco-pyrrolate involved base hydrolysis of
the drug, tbllowedby methylation of the cyclopentylmandelic acid
thusproduced, and subsequent GC/MS detection of thismethyl ester.
The various developed methodologies basedon this approach have been
used to confirm the adminis-tration to horses of glycopyrrolate in
drug controlprogrammes in equine sports.
Detection of the drug at the Horseracing ForensicLaboratory is
currently made using an on-line LC/MSmethod. However, with the
advent of electrosprayionization (ES) mass spectrometry has come
the oppor-tunity tbr the development of an on-line LC/MS
methodcapable of identitk/ing the intact parent drug, and thusthe
ability to bypass laborious and time-consumingdcrivatization
procedures. Renowned in the biopolymerfield, electrospray
ionization’s reliability and capacity toanalyse thermally labile
lower molecular weight com-pounds has ensured its increasing
application in thedetection and identification ofdrugs and their
metabolites.
Copies from IAS, Queens Avenue, Maccleeld, CheshireSKIO 2B./V,
UK. Tel.: 01625 43434. fax: 01625 434335.
Flexible MIS and industrial control
Bristol Babcock has announced the formation ofPronexus,its new
Software Technologies Division. Pronexus aims toprovide industry
with the most open, flexible and scaleablebusiness solutions tbr
Management Intbrmation Systems(MIS) and industrial control
applications. Pronexus willbe dedicated to the development of ’next
generation’software products, based on the concept of open
systemsand connectivity and incorporating leading edge
softwaretechnologies such as object-oriented relational
databases,
global standards compliance, hardware and softwareplatform
independence, database access through standards(for example, SQL
and ODBC) and advanced X-Windows operator graphics.
Details from Pronexus, Worcester Road,
Stourport-on-Severn,Worcestershire D Y139A T, UK. Tel.: 01299
824119;fax. 01299824118.
Portable pH meter
Radiometer’s PHM201 Portable pH Meter allows labor-atory
standard measurements to be taken in the field. ThePHM201
automatically recognizes the buffers used forcalibration--users
have a choice of IUPAC buffers,technical buffers meeting DIN 19267
or buffers pH 4, 7and 10. There is then the option of single or
dual pointcalibration. The last calibration is also
automaticallystored to enable electrode performance comparison.
During actual reading, the AUTOREAD thnction locksthe meter onto
the signal as soon as it is stable. Measure-ments can also be real
live with the aid of a stabilityindicator. The measurement range
runs from -9 to + 23pH units (millivolt measurement optional) with
aresolution of0.01 and accuracy of
___0.01 after calibration.
There is a continuous range of information availablevia the
display including prompts tbr the calibrationparameters and when to
change buffers. The PHM201operates off" battery or mains.y
For more information contact Ed Lemon at Radiometer Lld,
TheManor, Manor Royal, Crawley, West Sussex RHIO 2PY. Tel."01293
517599; fax." 01293 531597.
Mercury Measurement at PITTCON ’95
At the 1995 Pittsburgh Conference in New Orleans, P.S.Analytical
introduced several new products to extendtheir atomic fluorescence
range. Mercury continues to be amajor focus of PSA’s customers and
the new mercuryspeciation system based on gas chromatography,
coupledto atomic fluorescence (GC AFS) is the world’s first
thllyconfigured instrument to analyse organo-mercury com-pounds.
The system allows rapid analysis of soils,sediments and water
samples to ascertain their organo-mercury profile. The methods
provide sample extractionswhich avoid masking any mercury compound
presentsuch as diethyl mercury. The system provides detectionlevels
which are better than pg for diethyl mercury.
As a further extension ofits product range, P.S. Analyticalhas
introduced two new instruments for on-line mercuryanalysis. The PSA
10.223 Liquid On-Line System meetsclients’ needs in the
chlor-alkali, chemical or effluentindustries. It uses the wide
linear dynamic range of theMerlin Detec{or to analyse such
difficult samples on arepeat cycle basis. Systems have already been
installed inEurope to monitor effluents 24 hours a day. PSA has
alsointroduced a new Sir Galahad on-line gaseous monitor.
Further information from Professor Peter Slockwell,
P.S.Analytical, Arthur House, Unit 2.03 Crayfields Industrial
Park,Main Road, St Pauls Cray, Orpington, Kent BR5 3HP, UK.Tel.:
01689 891211; fax: 01689 896009.
121
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New products
Derivative spectroscopy
The theory of derivative spectroscopy is described in anew
application note tiom Hewlett-Packard. The notereviews the
fundamental mathematical relationshipsbetween analyte concentration
and measured absorbancethat are used to calculate first and
higher-order derivatives.It describes the optical, electronic and
mathematicalmethods of obtaining derivative spectra, and outlines
theadvantages of the mathematical techniques.
Computer-generated examples are used to illustrate thefeatures
and applications ofderivative spectroscopy. Theseexamples show how
resolution can be increased, howbackground absorbance and scatter
can be eliminated,and how broad absorbing bands and background
matricescan be suppressed.
The application note is available from PMG Logistics, Alln.Pelra
Butler, P.O. Box 533, 2130 AM ttoofddorp, TheNelherlands.
122
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