31.infoExpo 2003, Seminario & Workshop

località: Lugano Hotel Parco-Paradiso

Seminario

Hydrophilic Interaction Chromatography - the ideal alternative for seperatin of polar compounds
Dr. Annette Dibowski YMC Europe GmbH

The separation of strong polar compounds is still a problem, which is not easy to solve in the chromatographic area. In this field HILIC offers a good alternative, because this technique implies a lot of advantages in comparison to standard HPLC methods.
Even strong polar compounds can easily be retained under HILIC conditions, where reversed phase chromatography completely fails.
Additionally HILIC opens new ways for method development, because the elution order may change in comparison to reversed phase chromatography.
Finally HILIC is fully compatible to standard detection techniques as well as LC/MS separations, which is essential for modern HPLC applications.
Therefore HILIC “fills the gap” between the different chromatographic techniques for the separation of polar compounds.

Acryl amid Determination with GC/MS (PCI) in Food
Heiko Helms PerkinElmer Deutschland GmbH

Today, analysis for Acrylamide in food is time consuming. The results in this proposal asked for a way to use Headspace analysis combined with GC-MS for an easier way without losing analytical quality.
Extraction is done similar to existing methods, but no clean up is done anyway. Extract is injected by total vaporization in a HS Sampler, then analyzed by GC-MS ( Methane, PCI).
Is this procedure described as a possible method for polar compounds, which are not typically analyzed by Headspace techniques?
Tecniche di campionamento per l'analisi gascromatografica delle acque
Dr. Manuela Bergna, DANI Instruments

Il problema della presenza nell’acqua di sostanze inquinanti è avvertito in misura crescente non solo dagli addetti ai lavori ma anche dall’opinione pubblica, grazie anche ad interventi di sensibilizzazione sull’importanza di un uso e di una gestione sostenibile delle risorse idriche.
Aumenta quindi, a tutti i livelli, la richiesta di metodologie analitiche adatte ad un controllo costante e sensibile della presenza di queste sostanze inquinanti.
Tra le tecniche analitiche impiegate nell’analisi delle acque,la gascromatografia è largamente utilizzata per la determinazione di sostanze organiche quali residui di pesticidi, di solventi volatili, oli minerali, IPA e PCB.
Diverse tecniche di campionamento possono essere accoppiate all’analisi gascromatografica. Queste offrono il vantaggio di automatizzare le analisi di numerosi campioni e di raggiungere i livelli di sensibilità richiesti dalle normative, ottenendo risultati maggiormente accurati e ripetibili. L’intervento illustrerà alcune applicazioni sull’analisi dell’acqua effettuate con tecniche di campionamento diverse quali il campionamento per spazio di testa statico, Purge & trap o campionamenti in continuo.

Lo scale up in Cromatografia. Dalla purificazione di milligrammi alle centinaia di grammi di campione
Dr. Riccardo Braggio, Alfatech Spa

La purificazione per via cromatografia, continua ad acquisire sempre maggiore importanza in numerosi settori della Chimica Farmaceutica ed in quella dei Prodotti Naturali.
L’approccio più comune da parte di chi si appresta ad usare la Cromatografia Liquida a scopi preparativi, è quello di traslare direttamente il metodo analitico su colonne di maggior diametro.
Questo fatto, ed alcuni preconcetti errati sulla tecnica, ne hanno reso difficile l’applicazione pratica generando erronee valutazioni. Scopo della presentazione è quello di illustrare le caratteristiche di questo potente mezzo di purificazione, chiarendo, possibilmente, le potenzialità ed i limiti della Cromatografia Preparativa.
Dopo aver chiarito brevemente le differenze fra la Cromatografia Liquida Analitica e quella Preparativa, vengono dati alcuni consigli pratici per impostare il lavoro di purificazione.
Vengono, quindi, esaminati i principi teorici della separazione cromatografia e viene mostrato come alcuni parametri influenzino la cromatografia preparativa in particolare modificando la resa e la purezza dei prodotti ottenuti.
In particolare viene esaminato il ruolo dell’Rs sulla purezza delle frazioni ottenibili.
Vengono esaminati i limiti esistenti nella capacità di carico delle colonne sia in termini di diminuzione della resa che in termini di purezza ottenuta.
Questi limiti sono in gran parte superabili attraverso la tecnica del Riciclo e con quella del “Peak Shaving” che vengono approfonditamente descritte.
L’uso delle due tecniche combinate consente di ottenere risultati degni di nota.
Viene , infine, proposto un modello di strumento in grado di impiegare le tecniche descritte in modo automatico.

Visualization of the evaporation process in the hot evaporation chamber of the classical split and splitless GC-injector
Maurus Biedermann Kantonales Labor Zürich

Capillary GC frequently struggles with non-reproducible results. Often the source of the deviations is already at the inlet of the GC system. The evaporation process inside the hot chamber of a split/splitless injector was always subject of speculations. The experiments described below enabled its direct visual observation.
A device imitating an injector made from glass was heated to 200 °C in an oil bath [1]. Perylene served as an indicator of non-evaporated solvent: fluorescence of perylene is strong when in solution, but weak when dry, thus there is non-evaporated solvent as long as fluorescence is visible. The experiments were video-taped and later transferred to the computer, which enabled to study the usually fast processes frame by frame [2].
When evaporation inside the syringe needle is suppressed, e.g. by using a fast autosampler, the sample leaves the needle as a band of liquid [3]. This eliminates discrimination by preferential loss of high boiling components in the needle, but introduces a new problem: the band of liquid is shot past the column entrance without relevant evaporation. The videos show what happens with the liquid as well as what measures are successful in halting the band of liquid and keeping the sample in place for evaporation.
When the syringe needle is allowed to heat up to the injector temperature before the plunger is depressed (hot needle injection), partial solvent evaporation inside the needle causes the thermospray effect: the liquid is nebulized by solvent vapor acting as propellant. The solutes evaporate from small droplets suspended in the glass phase [4,5], i.e. without contacting possibly adsorptive or contaminated surfaces.
The videos show the complexity of the vaporization process in the injector and what the options are when injecting with band formation or thermospray.

[1] K. Grob, M. DeMartin, J. High Resol. Chromatogr., 1992, 15, 335

[2] M. Biedermann, „Visualization of the Evaporation Process during Classical Split and Splitless Injection in GC", CD-ROM, 2000

[3] K. Grob, M. Biedermann, „Video-taped sample evaporation in hot chambers simulating gas chromatography split and splitless injectors II. Injection with band formation“, J. Chromatogr. A, 2000, 897, 247-258

[4] K. Grob, M. Biedermann, „Video-taped sample evaporation in hot chambers simulating gas chromatography split/splitless injectors I. Thermospray injection“, J. Chromatogr. A, 2000, 897, 237-246

[5] K. Grob, M. Biedermann, “The Two Options for Sample Evaporation in Hot GC Injectors; Thermospray and Band Formation. Optimization of Conditions and Injector Design”, Anal. Chem. 2002, 74, 10-16

Workshop GC

GC und GC/MS – GC-Analysis in Seconds or Minutes
Dr. Robert Stoop, Brechbühler AG

GC is an established technique, which is widely spread out in all the labs. Yet not much has been said about the GC Techniques recently although there is still enough development going on worth to be mentioned.
One of these newer techniques is the ULTRAFAST GC that allows cutting GC analysis times down to seconds or a few minutes! ULTRAFAST is not just simple FAST GC. In this workshop, the different techniques conventional, fast and ULTRAFAST GC will be compared with each other. The possibilities of the ULTRAFAST GC method and its application in practice will be further discussed in this workshop.

Gas Generators for the Use in Gas Chromatography
Joyce Link, Milian SA

Gas generators have become a widely accepted substitute for expensive and dangerous gas cylinders in the laboratory. Not only has the safety aspect led people to decide on using the gas generator; it’s especially the high quality with which gas is generated – ultra pure and almost absolutely dry. Be it as feed gas for the FID, ensuring lowest possible background noise, or as carrier gas - it definitely enhances reproducability of your detections.
With the aid of the Parker Balston Gas Generator, we will show you how compact, reliable and easy to maintain today's gas generators can be, and that they fully comply with the laboratory quality standards and regulations

MassLib Makes Better Use of Your Analysis Data
Peter Kofel, MSP Kofel

Often mass spectrometry is used only to determine the molecular weight of a compound and with some coarse argumentation as a complimentary method to other spectroscopic techniques. The reasons are quite obvious: the interpretation of mass spectra appears to be unreliable and painful to the non-specialist. Furthermore the data systems based on library searches are often not suitable if an unknown spectrum has no reference in the library with sufficient similarity and quality.
With this respect MassLib is the exception. The unique combination of searches for fragment masses, neutral loss and structural similarity make MassLib an ideal tool for finding structural information. Even if the spectra of related structures are dissimilar and in cases where the limited amount of a sample permits mass spectrometry only.
For the evaluation of mass spectrometric analyses MassLib allows to make use of internal (e.g. single ion traces) and external (e.g. temperature profiles) traces and reference analyses. The computer assisted comparison of entire analysis runs allows the rapid detection and interpretation of differences even if the analyses compared look very similar at first sight.

Workshop HPLC

Validation of Detectors made easy
Andreas Floderer, infochroma ag

Thanks to their good training, lab technicians know how to replace spare parts in HPLC- and GC Systems and how to check that the systems keeps running conform to regulations.
eg. exchanging a deuterium lamp in an HPLC Detector and testing the correct UV wavelenght
It is important to avoid mistakes and to document each step taken. We will introduce a software which provides HPLC and GC users with an excellent tool.

Examples for the HPLC user are testing:
+ correct flowrate
+ correct gradient
+ correct UV-wavelength
+ linear UV-adsorbtion
+ correct temperature of the column oven
+ correct functioning of the autosampler

With the test for a correct flowrate, we will explain the software and the test report in detail.
You can choose a test to test the advantages of the software yourself.

CreaStab, il software per i vostri studi di stabilità
D. Bimbi, CreaLab sagl.

Da oggi è possibile gestire semplicemente i propri studi di stabilità utilizzando il nuovo software: “CreaStab”.
L’interfaccia “Planning” ci permette di visualizzare (e stampare) immediatamente le analisi di stabilità in scadenza.
CreaStab permette l’accesso controllato attraverso la combinazione User Name e password su due livelli: User e Manager.
Nel log file vengono registrate tutte le azioni svolte: il tipo di azione, il momento in cui è stata svolta, e il nome dell’operatore .
Nel caso in cui fosse necessario modificare dati immessi, questo è possibile solo dal Manager; tale cambiamento richiede una motivazione che viene registrata nel log file.

Tre semplici operazioni per gestire i propri studi di stabilità:
1. PREPARAZIONE :
Creazione
- Specifiche
- Condizioni climatiche
- Tempistiche di analisi
- Lotti in stabilità

2. GESTIONE :
Visualizzazione
- Planning dei lotti da analizzare
Inserimento
- Dati analitici
- Verifica “out of specification”

3. ELABORAZIONE DATI :
Visualizzazione, stampa, esportazione dati
- Certificati d’analisi
- Studi stabilità
- Esportazione dati in Excel
- Trend di degradazione
- Statistiche

Azoto per LC-MS; garantita l’alta risoluzione analitica con l’utilizzo dei generatori “Tailored”; economia e praticità ineguagliabili
Nicola Tunesi, Claind
L’idrogeno, gas indispensabile nella GC; sicurezza, purezza e prestazioni all’avanguardia offerti dai nuovi HG serie 2000
L’uso dei gas nel laboratorio e le direttive CEE
I generatori di gas per un laboratorio moderno

Downscale, Mikro HPLC
Manfred Kunz, GROM Analytik + HPLC GmbH

Only a small number of the common HPLC systems can be used for the Microbore HPLC. At flow rates of < 50 µL / min the necessary performance can not be received with this systems. The increasing of LC/MS applications in the analytical labs provided that there are more and more systems for Micro LC are available.
The first part gives a description of the different techniques for performing low flow rates and their advantages and weaknesses of this techniques. Especially for the users of such systems a procedures will be described for their evaluation.
In the second part an overview about the common available systems will be given.

Micro Trap Technique
Ruedi Schwarz, sertec electronics