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The Concepts Guide presents an overview of the InfinityLab LC/MSD Series and 6100 Series LC/MS mass selective detector, to help you understand how the hardware and software work. 1 Overview of Hardware and Software Learn how the hardware works in the InfinityLab LC/MSD Series and 6100 Series LC/MS instrument, and get a brief introduction to the OpenLAB CDS ChemStation Edition program. 2 Instrument Preparation Learn the concepts you need to prepare the LC and column for an analysis, and to tune the MS. 3 Data Acquisition Learn about setting up methods and running samples. 4 Data Analysis Learn the concepts you need for qualitative and quantitative data analysis with the ChemStation Edition program. 5 Reports Learn about predefined results reports and about setting up custom reports. 6 Verification of Performance Learn the concepts for Operational Qualification/ Performance Verification (OQ/PV) and system verification with the ChemStation Edition program. 7 Maintenance and Troubleshooting Learn about tools that are proved in the ChemStation Edition program to help you maintain your system and diagnose and fix problems. Agilent InfinityLab LC/MSD Series and 6100 Series LC/MS Concepts Guide 3 This page intentionally left blank. 4 Agilent InfinityLab LC/MSD Series and 6100 Series LC/MS Concepts Content 1 Overview of Hardware and Software 9 How the Agilent mass selective detectors work 10 Overview 10 Details 11 Types of data you can acquire 15 Scan versus selected ion monitoring (SIM) 15 Generation of fragment ions: low versus high fragmentor 16 Positive versus negative ions 18 Multiple signal acquisition 19 Ion sources 21 Electrospray ionization (ESI) 21 Agilent Jet Stream 25 Atmospheric pressure chemical ionization (APCI) 27 Atmospheric pressure photoionization (APPI) 29 Multimode ionization (MMI) 30 Introduction to the ChemStation Edition program 31 Overview 31 Reviewing data remotely 33 2 Instrument Preparation 35 Preparation of the LC system 36 Purpose 36 Summary of procedures 36 Setting parameters for LC modules 38 Column conditioning and equilibration 39 Monitoring the stability of flow and pressure 41 Preparation of the MS – tuning 42 Overview 42 Agilent InfinityLab LC/MSD Series and 6100 Series LC/MS Concepts Guide 5 Contents Ways to tune 44 When to tune – Check Tune 45 Autotune 47 Manual tuning 49 Tune reports 51 Gain calibration 52 3 Data Acquisition 55 Working with methods 56 Method and Run Control View 56 Loading, editing, saving and printing methods 58 More on editing methods 59 Running samples 62 Running a single sample 63 Running a sequence 64 Flow injection analysis 67 Monitoring analyses 70 Online signal plots 70 Logbooks 71 Instrument shutdown 72 4 Data Analysis 73 The Data Analysis View 74 Loading and manipulating chromatograms 76 Loading signals 77 Removing signals from the chromatogram display 81 Changing how chromatograms are displayed 81 Working with spectra 83 Displaying spectra 84 Peak purity 85 Performing quantification 86 6 Agilent InfinityLab LC/MSD Series and 6100 Series LC/MS Concepts Guide Contents Integrating peaks 86 Calibration 88 Data review and sequence reprocessing 90 The Navigation Table 90 Batch review 91 5 Reports 93 Using predefined reports 94 Generating reports 94 Report styles 95 Defining custom reports 96 Summary of process 96 Example report templates 96 The Report Layout View 97 6 Verification of Performance 99 The Verification (OQ/PV) View 100 Instrument verification 101 Setting up and running instrument verification 102 Available OQ/PV tests 104 Verification logbook 105 System verification 106 Overview 106 Setting up and running system verification 107 7 Maintenance and Troubleshooting 109 The Diagnosis View 110 Overview 110 Instrument panel 111 Logbooks 113 Maintenance 114 Agilent InfinityLab LC/MSD Series and 6100 Series LC/MS Concepts Guide 7 Contents Early maintenance feedback 114 Maintenance logbook 115 Maintenance procedures 115 Venting and pumping down the MS 116 Diagnosing and fixing problems 117 Symptoms and causes 117 Diagnostic tests for the MS 118 Fixing problems 120 8 Agilent InfinityLab LC/MSD Series and 6100 Series LC/MS Concepts Guide InfinityLab LC/MSD Series and 6100 Series LC/MS Concepts Guide 1 Overview of Hardware and Software How the Agilent mass selective detectors work 10 Overview 10 Details 11 Types of data you can acquire 15 Scan versus selected ion monitoring (SIM) 15 Generation of fragment ions: low versus high fragmentor 16 Positive versus negative ions 18 Multiple signal acquisition 19 Ion sources 21 Electrospray ionization (ESI) 21 Atmospheric pressure chemical ionization (APCI) 27 Atmospheric pressure photoionization (APPI) 29 Multimode ionization (MMI) 30 Introduction to the ChemStation Edition program 31 Overview 31 Reviewing data remotely 33 This chapter provides an overview of the hardware and ChemStation Edition program that comprises the InfinityLab LC/MSD Series and 6100 Series LC/MS systems. The InfinityLab LC/MSD Series consists of two models: LC/MSD XT and LC/MSD. The 6100 Series LC/MS family consists of three models: 6120B, 6130B, and 6150B. 9 1 Overview of Hardware and Software How the Agilent mass selective detectors work How the Agilent mass selective detectors work Overview Mass selective detectors (MSD) analyze ions moving through a vacuum to produce mass spectra. Mass spectra provide valuable information about the molecular weight, structure, identity, quantity, and purity of a sample. MSDs add specificity to both qualitative and quantitative analyses. A quadrupole mass analyzer is Figure 1 shows a diagram of Agilent MSD instrument. The sometimes called a quadrupole ionization of a sample occurs at atmospheric pressure in the ion mass filter or a quadrupole. source that is shown on the left. The Agilent MSDs are compatible with a number of Agilent atmospheric pressure ionization (API) sources. HPLC inlet quadrupole nebulizer capillary mass filter ion optics detector ion source rough split-flow pump turbo pump Figure 1 Block diagram for an Agilent MSD API – atmospheric pressure A common atmospheric sampling interface introduces ions ionization from these ionization sources into the vacuum system of the mass spectrometer. Various ion-optic elements focus and guide the ions through a series of vacuum stages until they reach the quadrupole mass analyzer, which separates the ions. The ions then travel to the detector, where they are recorded as signals. 10 Agilent InfinityLab LC/MSD Series and 6100 Series LC/MS Concepts Guide Overview of Hardware and Software 1 Details Details Figure 2 and Figure 3 show more detailed schematics of the ion paths in an Agilent MSD. After the API source forms ions, the ion-optic elements in the ion transport and focusing region of the system direct the ions toward the quadrupole and the detector. During transit, the ions move from atmospheric pressure (760 torr) at the source to a vacuum in the 10-6 torr range at the quadrupole and detector.