Dionex MSQ Bedienungsanleitung

Document No. 031871

Revision 02

October 2003

Hardware

MSQ™

Printed in the United States of America.

This publication is protected by federal copyright law. No part of this publication may be copied or

distributed, transmitted, transcribed, stored in a retrieval system, or transmitted into any human or computer

language, in any form or by any means, electronic, mechanical, magnetic, manual, or otherwise, or disclosed

to third parties without the express written permission of Dionex Corporation, 1228 Titan Way, Sunnyvale,

California 94088-3603 U.S.A.

DISCLAIMER OF WARRANTY AND LIMITED WARRANTY

THIS PUBLICATION IS PROVIDED “AS IS” WITHOUT WARRANTY OF ANY KIND. DIONEX

CORPORATION DOES NOT WARRANT, GUARANTEE, OR MAKE ANY EXPRESS OR

IMPLIED REPRESENTATIONS REGARDING THE USE, OR THE RESULTS OF THE USE, OF

THIS PUBLICATION IN TERMS OF CORRECTNESS, ACCURACY, RELIABILITY,

CURRENTNESS, OR OTHERWISE. FURTHER, DIONEX CORPORATION RESERVES THE

RIGHT TO REVISE THIS PUBLICATION AND TO MAKE CHANGES FROM TIME TO TIME IN

THE CONTENT HEREINOF WITHOUT OBLIGATION OF DIONEX CORPORATION TO

NOTIFY ANY PERSON OR ORGANIZATION OF SUCH REVISION OR CHANGES.

TRADEMARKS

Chromeleon is a registered trademark of Dionex Corporation.

Cone Wash, M-Path, MSQ, and Xcalibur are trademarks of Thermo Electron Corporation.

Microsoft is a registered trademark of Microsoft Corporation.

Q-tip is a trademark of Chesebrough-Pond’s, Inc.

Teflon, Vespel, and Viton are registered trademarks of E.I. du Pont de Nemours and Company.

PRINTING HISTORY

Revision 01, July 2002

Revision 02, October 2003

The products of Dionex Corporation are produced under ISO 9001 accredited quality management systems.

Published by Technical Publications, Dionex Corporation, Sunnyvale, CA 94086.

Chapter 1

Introducing the MSQ1.

Introducing the MSQ.................................................................................................................1-i

Introduction ....................................................................................................................................1-1

System Overview............................................................................................................................1-2

What Is Mass Detection?...................................................................................................1-4

Exterior Features of the MSQ............................................................................................1-5

The Source–An Introduction to API Techniques ...........................................................................1-8

Electrospray.......................................................................................................................1-9

Atmospheric Pressure Chemical Ionization.....................................................................1-13

Source Fragmentation......................................................................................................1-16

Cone Voltage Ramping ...................................................................................................1-18

Polarity Switching ...........................................................................................................1-19

Application of API Techniques .......................................................................................1-20

The Self-Cleaning Source: Cone Wash ........................................................................................1-23

Introduction .....................................................................................................................1-23

Functional Description ....................................................................................................1-24

The Reference Inlet System..........................................................................................................1-25

Introduction .....................................................................................................................1-25

Functional Description ....................................................................................................1-25

The Mass Analyzer and Detector .................................................................................................1-26

The Vacuum System.....................................................................................................................1-27

The Data System...........................................................................................................................1-28

Software...........................................................................................................................1-28

Raw Data .........................................................................................................................1-30

Raw Data Types...............................................................................................................1-31

____________________________MSQ Hardware Manual _____________________________ 1-i

Introducing the MSQ

Introduction ____________________________________________________________________________

1-ii____________________________ MSQ Hardware Manual ____________________________

Introducing the MSQ

___________________________________________________________________________ Introduction

Introduction

The MSQ™ MS detector has been specifically designed and engineered for

liquid chromatographic detection using Atmospheric Pressure Ionization

(API) and Mass Spectrometry (MS) technology. These technologies can

provide sensitive and selective detection of organic molecules.

Interfacing High Performance Liquid Chromatography (HPLC or LC) and

MS provides the separation scientist with one of the most powerful

analytical tools available. Both LC and MS have developed to a point

whereby they represent two of the most important techniques in

characterizing and detecting organic compounds. Although the potential

benefits of interfacing LC to MS have been clearly recognized for many

years, producing a truly automated “connect-and-use” interface has proven

to be a challenging task.

Atmospheric Pressure Ionization (API) techniques now provide highly

sensitive detection using conventional to capillary LC flow rates on bench-

top MS detector systems. LC/MS works with typical solvent compositions,

whether the separation is achieved by isocratic or gradient elution.

Historically, LC/MS has been compatible only with volatile buffer systems

using modifiers such as trifluoroacetic acid, formic acid, and acetic acid.

Phosphate buffers, although extensively used in LC separations, were not

suited to LC/MS due to rapid blocking of the ion sampling region caused by

the deposition of involatile phosphate salts. The self-cleaning API source

allows for extended periods of operation in LC/MS with chromatographic

buffers such as phosphates or ion-pairing agents and samples in dirty

matrices.

API using Electrospray (ESI) or Atmospheric Pressure Chemical Ionization

(APCI) interfaces has proved to be invaluable in meeting sensitivity

requirements in quantitative methods. It can also provide structural

information, which is complementary to techniques such as NMR and infra

red spectroscopy.

This introduction focuses on the principal components of the system.

___________________________MSQ Hardware Manual ____________________________ 1-1

Introducing the MSQ

System Overview ________________________________________________________________________

System Overview

The MSQ MS detector is an integral part of the LC detection system. Key

points of the system are:

The sample is introduced into the ion source using an LC system,

possibly through a column.

•

In an API MS detector, the part of the source where ionization takes

place is held at atmospheric pressure, giving rise to the term

Atmospheric Pressure Ionization (API).

In ESI, the sample is ionized in the liquid phase, while in APCI,

ionization occurs in the gas phase. In both cases, efficient desolvation is

needed to remove the solvents from the sample.

Ions, now in the gas phase, are passed through the mass analyzer and are

collected at the detector.

The detected signal is sent to the data system and stored ready for

processing.

LC Column

Separation

LC System

Sample

introduction

Ion Source

Ionization &

transmission

Mass Analyzer

Sorting of ions

Detector

Detection

of ions

Data System

Windows NT

Molecular weight information

Structural information

Positive identification

Quantitative information

Turbomolecular

& rotary pumps

Figure 1-1. The key components of the MSQ API LC detection system

1-2 ___________________________ MSQ Hardware Manual ____________________________

Introducing the MSQ

_______________________________________________________________________System Overview

The main features of the MSQ MS detector are:

Dual ESI/APCI orthogonal probe•

•

Self-cleaning API-LC/MS interface

M-Path™ triple orthogonal source

Quadrupole

mass analyzer

Square

quadrupole

RF lens

Rotary

pump

Split flow

turbomolecular

pump

Entrance cone

From HPLC

Orthogonal sample

introduction probe

Cone wash

Exit cone

Figure 1-2. Schematic diagram of the MSQ API inlet, analyzer, and

detector system

The LC eluent is ionized at the API probe and the resulting ions are focused

into a square quadrupole RF lens. The quadrupole mass analyzer filters the

ions before detection.

___________________________MSQ Hardware Manual ____________________________ 1-3

Introducing the MSQ

System Overview ________________________________________________________________________

What Is Mass Detection?

Mass detection is a very powerful analytical technique used in a number of

fields, including:

Identification of unknown compounds•

•

Quantitation of known compounds

Determination of chemical structure

The basic function of an MS detector is to measure the mass-to-charge ratio

of ions.

The unit of mass used is the Dalton (Da). One Dalton is equal to 1/12 of the

mass of a single atom of carbon-12. This follows the accepted convention

that an atom of carbon-12 has exactly 12 atomic mass units (amu). The MS

detector does not directly measure molecular mass, but the mass-to-charge

ratio of the ions. Electrical charge is a quantized property and so can exist

only as an integer; that is, 1, 2, 3, and so on. The unit of charge used here (z)

is that which is on an electron (negative) or a proton (positive). Therefore,

the mass-to-charge ratio measured can be denoted by m/z. Most ions

encountered in mass detection have just one charge. In this case, the mass-

to-charge ratio is often spoken of as the “mass” of the ion.

1-4 ___________________________ MSQ Hardware Manual ____________________________

Introducing the MSQ

_______________________________________________________________________System Overview

Exterior Features of the MSQ

This section highlights the exterior features of the MSQ. The parts labeled

here may be referred to in later chapters of this manual or other manuals

supplied with the MSQ.

Status light

Figure 1-3. Front view of the MSQ

Figure 1-3 shows the front view of the MSQ. The main feature is the status

light.

___________________________MSQ Hardware Manual ____________________________ 1-5

Introducing the MSQ

System Overview ________________________________________________________________________

Table 1-1. Instrument status light

Instrument Status Light

Vented Red

Venting Red

Pumping down Flashing yellow

Under vacuum (above

vacuum trip)

Red

Under vacuum (ready

for use)

Yellow

Operate on (MSQ in

use)

Green

Source enclosure open Red

The vacuum trip is the pressure below which it is safe to switch on the

voltages in the source. When the instrument is functioning normally, the

status light will go from flashing yellow to solid yellow and Operate can be

switched On. If the pressure in the instrument rises above the operating

pressure, the status light turns red to indicate that the pressure is above a

safe level. See the chapter Shutting Down and Restarting the System for

information on pumping down the MSQ.

Figure 1-4 shows the MSQ with the doors open. The source enclosure and

reference inlet are now visible.

Source

enclosure

Reference

inlet

Figure 1-4. The MSQ with the doors open

1-6 ___________________________ MSQ Hardware Manual ____________________________

Inhaltsverzeichnis

Andere Dionex Laborausrüstung Handbücher

Dionex

Dionex IONPAC AG9-SC GUARD COLUMN Bedienungsanleitung

Dionex

Dionex RF-2000 Bedienungsanleitung

Dionex

Dionex UltiMate 3000 Benutzerhandbuch

Dionex

Dionex ICS-900 Bedienungsanleitung

Dionex

Dionex ICS-90 Bedienungsanleitung

Dionex

Dionex TCC-100 Bedienungsanleitung

Dionex

Dionex ProPac WCX-10 Montageanleitung

Dionex

Dionex P680 Bedienungsanleitung

Dionex

Dionex ICS-90 Bedienungsanleitung

Dionex

Dionex UltiMate 3000 Series Bedienungsanleitung

Dionex

Dionex ICS-3000 Bedienungsanleitung

Dionex

Dionex ICS-2100 Bedienungsanleitung

Dionex

Dionex DX-120 Bedienungsanleitung

Dionex

Dionex As Bedienungsanleitung

Dionex

Dionex P680 Bedienungsanleitung

Dionex

Dionex ICS-1000 Bedienungsanleitung

Dionex

Dionex UltiMate 3000 Benutzerhandbuch

Dionex

Dionex P680 Bedienungsanleitung

Dionex

Dionex AS-HV Bedienungsanleitung

Beliebte Laborausrüstung Handbücher anderer Marken

Qiagen

Qiagen DML 3000 Bedienungsanleitung

Queensgate

Queensgate NANOSCAN OP400 Programmierhandbuch

Conviron

Conviron GEN1000-GE Bedienungsanleitung

Parr Instrument

Parr Instrument 4560 Bedienungsanleitung

IKA

IKA IC control Bedienungsanleitung

Integra

Integra DOSE IT Bedienungsanleitung

Agilent Technologies

Agilent Technologies 5800 ICP-OES Bedienungsanleitung

Endress+Hauser

Endress+Hauser Cleanfit CPA875 Bedienungsanleitung

NI PXI-5422 Handbuch

Collomix

Collomix Aqix Bedienungsanleitung

SPEX SamplePrep

SPEX SamplePrep 6875 Freezer/Mill Series Bedienungsanleitung

Ocean Insight

Ocean Insight FLAME-NIR+ Bedienungsanleitung

Parker

Parker ALIGN-MG-NA Bedienungsanleitung

BD 644787 Bedienungsanleitung

DENTAURUM

DENTAURUM Compact Megaplus Bedienungsanleitung

Biuged Laboratory Instruments

Biuged Laboratory Instruments BGD 626 Bedienungsanleitung

VWR

VWR SAS Super IAQ Bedienungsanleitung

illumina

illumina MiSeqDx Bedienungsanleitung