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Micromass Quattro Ultima User Manual

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Quattro Ultima
User's Guide
Code: 6666511
Issue 3
© Micromass Ltd.
Micromass UK Limited
Floats Road
Wythenshawe
M23 9LZ
Tel: +44 161 945 4170 Fax: +44 161 998 8915
Tudor Road
Altrincham
WA14 5RZ
Tel: +44 161 282 9666 Fax: +44 161 282 4400
http://www.micromass.co.uk
The instrument is marked with this symbol where high voltages are
present.
The instrument is marked with this symbol where hot surfaces are
present.
The instrument is marked with this symbol where the user should refer to
this User's Guide for instructions which may prevent damage to the
instrument.
Warnings are given throughout this manual where care is required to avoid personal
injury.
If the instrument is used in a manner not specified by the manufacturer, the protection
provided by the equipment may be impaired.
This manual is a companion to the MassLynx NT User's Guide supplied with the
instrument.
All information contained in these manuals is believed to be correct at the time of
publication. The publishers and their agents shall not be liable for errors
contained herein nor for incidental or consequential damages in connection with
the furnishing, performance or use of this material. All product specifications, as
well as the information contained in this manual, are subject to change without
notice.

Table of Contents

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Micromass Quattro Ultima Specifications

General IconGeneral
BrandMicromass
ModelQuattro Ultima
CategoryLaboratory Equipment
LanguageEnglish

Summary

Safety Information and Symbols

High Voltage Warning Symbol

Symbol indicates the presence of high voltages on the instrument.

Hot Surfaces Warning Symbol

Symbol indicates that the instrument has hot surfaces.

Refer to Manual Symbol

Symbol indicates user should consult the guide to prevent instrument damage.

General Safety Warnings

Warnings for personal injury avoidance and proper instrument use.

Hardware Specifications

Dimensions

Physical dimensions of the instrument with a diagram.

Weights

Weight specifications for the instrument, data system, and pumps.

Lifting and Carrying Precautions

Safe Lifting Guidelines

Warnings and guidelines for safe lifting and handling of the instrument.

Power, Environment, and Cooling Specifications

Power Requirements

Electrical voltage and current specifications for the instrument and pumps.

Environmental Specifications

Ambient temperature, heat dissipation, and humidity limits.

Water Cooling System

Specification for heat dissipation into water for cooling the system.

Exhaust and Gas Venting Requirements

Rotary Pump Exhaust Venting

Requirement to vent rotary pump exhaust to atmosphere via fume hood or vent.

API Gas Exhaust Venting

Venting API gas exhaust to atmosphere; caution about connection to rotary pump exhaust.

Gas Supply Requirements

Nitrogen Gas Supply

Specification for dry, oil-free nitrogen supply and tubing requirements.

CID Gas Supply

Specification for Argon as collision gas and required pressure.

Instrument Description Overview

System Components and Capabilities

Overview of the Quattro Ultima MS-MS system and its coupling capabilities.

Ion Path and Detection Process

Description of ion flow through source, quadrupoles, and detector system.

Vacuum System Operation

Pump Configuration Details

Details of rotary and turbomolecular pumps used for vacuum generation.

Vacuum Measurement and Interlocks

Vacuum measurement gauges and system interlocks for protection.

Ionisation Techniques Overview

Atmospheric Pressure Chemical Ionisation (APCI)

Description of APcI mechanism, sample vaporization, and flow rates.

Electrospray Ionisation (ESI)

Description of ESI mechanism, charged droplets, and flow rates.

Nanoflow Electrospray

Nanoflow interface for low flow rate ESI and sensitivity gains.

Sample Inlet Description

How samples are introduced via liquid pumping systems and capillaries.

Mass Spectrometry Operating Modes

MS Operating Modes

Explanation of MS1 and MS2 modes for basic MS analysis.

MS-MS Operating Modes Summary

Summary of four MS-MS scan functions: Daughter Ion, Parent Ion, MRM, Constant Neutral Loss.

Daughter Ion Spectrum Analysis

Daughter Ion Spectrum Applications

Typical applications like structural elucidation and method development.

Daughter Ion Spectrum Example

Example spectrum illustrating daughter ion analysis.

Parent Ion Spectrum Analysis

Parent Ion Spectrum Applications

Applications for structural elucidation and complementary data.

Parent Ion Spectrum Example

Example spectrum illustrating parent ion analysis.

Multiple Reaction Monitoring (MRM)

MRM Principle and Applications

MRM for high sensitivity screening and applications.

MRM Example and Output

Example of MRM transition monitoring and chromatogram output.

Constant Neutral Loss Spectrum Analysis

Spectrum Generation and Interpretation

How the spectrum is generated and what it represents.

Data System and MassLynx NT Software

PC-Based Data System Function

Role of PC data system and MassLynx NT in instrument control.

Front Panel Connections

Gas Line Connections

Connection of PTFE gas lines for desolvation and nebuliser gases.

Electrical Connections

Electrical connections for ESI capillary, APcI discharge pin, and ESI/APcI heaters.

Front Panel Controls and Indicators

Status Display Overview

Description of Vacuum and Operate LEDs indicating instrument status.

Vacuum LED Status Indicators

Table detailing states and indications for the Vacuum LED.

Operate LED Status Indicators

Table detailing states and indications for the Operate LED.

Flow Control and Valves

Flow Control Valves

Needle valves for gas control and caution for CID Gas valve.

Divert / Injection Valve

Optional valve for injection or switching solvent flow, pneumatically operated.

Rear Panel Connections

Event Out Outputs

Outputs for peripheral connection, switchable voltage or contact closure.

Contact Closure Inputs

Inputs for external devices to start sample acquisition.

Analog Channels Input

Analog inputs for simultaneous data acquisition from detectors.

Rear Panel Data System Connections

MUX Connector

6-way connector for instrument to MUX control base.

Data System Connector

RJ45 connector for instrument to data system via network cable.

Rear Panel Gas and Water Connections

Water Connections

Water usage for turbomolecular pump cooling.

Nitrogen Gas Inlet

Connection for nitrogen supply, tubing requirements, and caution.

Rear Panel Exhaust, Power, and Control Connections

Exhaust Venting Requirements

Requirements for venting rotary pump and gas exhausts; caution on combining lines.

Power Cord and Mains Switch

Requirements for power cord connection and mains switch function.

Fuses and Rotary Pump Control

Fuse information and rotary pump control via data system.

ESD Earth Facility Connection

Connection for grounding to prevent electrostatic discharge.

Internal Layout - Electronics

Power Supplies Configuration

Location and quantity of power supplies for various instrument components.

Key Electronic PCBs Location

Diagram showing location of Transputer, Analogue, Control, Scan Control, and RF Control PCBs.

Main Electronics Modules

Power Supplies and RF Generators

Details on low/high voltage power supplies and RF generators.

Control and Sequence PCBs Functions

Functions of Pumping Logic PCB and Power Sequence PCB.

Processor and Interface PCBs Functions

Functions of Transputer Processor Card, Analogue PCB, and Control PCB.

Scan and RF Generator Control PCBs

Functions of Scan Control PCB and RF Generator Control PCBs.

Internal Mechanical Components

Source and Analyser Housings

Description of source housing, analyser housing, and detector assembly.

Pumps and Vacuum Gauges

Details on turbomolecular pumps, Pirani, and Active Inverted Magnetron gauges.

Air Filter Location

Location of the air filter at the front of the instrument.

Routine Procedures: Start-Up

Start-Up Preparation Steps

Preparing instrument after inactivity: checking oil, connecting gases.

Routine Procedures: System Checks

Rotary Pump and Data System Connections

Verifying connections for rotary pump control, data system, and mains supplies.

Exhaust Venting and Power On Procedure

Checking exhaust connections and switching on the instrument.

Routine Procedures: Software Startup

Data System and MassLynx Startup

Steps for switching on the data system and launching the tune page.

Pumping Procedure

Rotary and Turbomolecular Pump Operation

Initiating pump down, monitoring vacuum status, and gas ballast valve operation.

Vacuum Monitoring and Instrument Readiness

Analyser Pressure Measurement

Monitoring analyser pressure using Penning gauge and gauge life caution.

Startup After Overnight Shutdown

Starting instrument after overnight standby, checking vacuum LED.

Electrospray Operation: Probe Preparation

Corona Discharge Pin Setup

Steps for fitting/removing corona discharge pin and connecting gas lines.

Electrospray Operation: Probe Setup

Connecting Probe and Setting Temperatures

Connecting probe, setting source/desolvation temps, launching tune page.

Source Operation Warnings

Warnings for operating source without enclosure and handling hot components.

APCI Operation: Probe Preparation

Corona Discharge Pin Installation

Steps for installing APcI corona discharge pin and connecting gas lines.

APCI Operation: Probe Setup

Connecting APcI Probe and Setting Temperature

Connecting APcI probe, setting source temperature, launching tune page.

APCI Operation Warnings

Warnings about operating source without enclosure and hot components.

Instrument Operation

Entering Operate Mode

Steps to enter operate mode via MassLynx, setting gas flows and temperatures.

Vacuum Protection Overview

Instrument protection against vacuum faults like pump malfunction, pressure, or temperature.

Transient Pressure Trip Protection

System response to pressure surge: voltage shutdown and amber Operate LED.

Vacuum Fault Handling

Pump Fault Conditions

Consequences of pump fault: stop pumping, flashing red Vacuum LED, extinguished Operate LED.

Power Failure Procedure

Steps for power failure and subsequent restart.

Tuning and Calibration Procedures

Tuning Information Reference

Reference to Tuning section and specific tuning for ionisation techniques.

Calibration Information Reference

Reference to Mass Calibration section.

Data Acquisition and Processing Reference

Reference to Data Acquisition and MassLynx NT User's Guide.

MS-MS Operation Setup

Worked example for daughter ion acquisition: tuning, parent ion selection, fragmentation.

Parent Ion Selection for Sensitivity

Importance of accurately finding parent ion mass for daughter ion analysis sensitivity.

MS-MS Operation: Fragmentation

Setting Daughter Ion Scan Parameters

Adjusting Mass and Span, using Argon as collision gas.

Optimizing Fragmentation Parameters

Adjusting Entrance, Collision, Exit, and collision gas pressure.

Shutdown Procedures

Emergency Shutdown Protocol

Steps for immediate shutdown: power off and LC isolation.

Overnight Shutdown Steps

Leaving instrument unattended: switching off LC pumps and nitrogen gas.

Complete Shutdown Procedure

Extended Period Shutdown Steps

Steps for extended shutdown: venting, exiting software, power off.

Rotary Pump Oil Management

Procedure for draining rotary pump oil if instrument is off for over a week.

Automatic Startup and Shutdown Files

Startup and Shutdown File Locations

Location and naming of automatic startup and shutdown files used by MassLynx.

Using the Shutdown Editor

Accessing and modifying automatic startup/shutdown procedures.

Shutdown Editor Configuration Options

Error and Batch Shutdown Configuration

Options for immediate shutdown on error, after batch, or after time delay.

Auto Control Tasks Page

Defining sequences of operations within the Auto Control Tasks page.

Managing Shutdown Tasks

Adding, Inserting, and Modifying Tasks

Procedures for adding, inserting, and modifying tasks within the shutdown editor.

Deleting Tasks from Editor

Methods for deleting individual or all tasks from the shutdown editor.

Shutdown Editor Toolbar Functions

Toolbar Button Equivalents and Purpose

Mapping toolbar buttons to menu equivalents and their purpose.

Managing Startup and Shutdown Files

Loading Startup and Shutdown Files

Steps to open existing startup or shutdown files using the open file dialog.

Saving Startup or Shutdown Files

Procedures for saving startup/shutdown files, including new and overwrite options.

Printing Startup and Shutdown Files

Using the Print Dialog

How to print startup and shutdown files using the print dialog.

Creating and Running Startup/Shutdown Files

Creating New Files

How to create a new startup or shutdown file using the New option.

Running and Stopping Files

Procedures for running and stopping automatic startup and shutdown files.

Tuning the Instrument

Tuning Overview and Objectives

Importance of tuning and calibration before data acquisition for mass accuracy.

Tuning Parameter Adjustments

Adjusting parameters in Source and Analyser menus, optimizing collision energy.

Tune Page Operations

Displaying and Printing Tune Information

How to display the tune page and print tune information.

Experimental Record and Parameter Saving

Tuning parameters stored in data files and saving/restoring parameter settings.

Managing Tuning Parameter Files

Saving Tuning Parameter Settings

Saving current tuning parameters to a file, including overwriting existing files.

Restoring Tuning Parameter Settings

Procedure to restore saved tuning parameters from a file.

Peak Display Modification

Selecting and Displaying Peaks

Using Peak Editor to select peaks and adjust Mass, Span, and Gain.

Changing Tune Mass and Range

Methods for changing tune mass and range using mouse or direct entry.

Adjusting Peak Display Parameters

Changing Peak Span

How to change the span of a peak using mouse or direct entry.

Adjusting Peak Gain

Methods for adjusting peak gain by double-clicking or direct entry.

Customizing Display Appearance

Changing Peak Display Colors

Using popup menu to change peak colors and customize plot appearance.

Adjusting Trace Count and Interpolation

Changing number of visible traces and adjusting color interpolation.

Display Options: Trace, Intensity, Grid

Trace Display Options

Options for displaying peak outline, fill, or min/max data points.

Intensity and Grid Display Options

Options for relative/absolute intensity, normalized data, and grid lines.

AutoTune Functionality

Running the AutoTune Process

How to run AutoTune for APcI/ESI modes and define setup parameters.

AutoTune Levels and Process Steps

Explanation of full vs. maintenance AutoTune and parameter initialization.

AutoTune Parameter Checks

Parameter Validation and Tuning Steps

Checks by AutoTune: parameter definition, readbacks, beam detection, focus, ion energy, resolution.

Ion Mode Selection

How to select the required ionisation mode from the Ion Mode menu.

Tuning Controls: Scope, Gas, and Ramps

Scope Parameter Adjustment

Controlling scan time and inter-scan delay for tune peak display updates.

Gas Control and Cone Voltage Ramp Setup

Turning gases on/off and setting up cone voltage ramps.

Tuning Controls: Collision Energy and Zero Level

Collision Energy Ramp Setup

Setting up a collision energy ramp by defining values at two masses.

Resetting the Zero Level

Repositioning zero or baseline by reinitialization to compensate for offsets.

Controlling Readback Display

Readback Display Options

Options for displaying readbacks continuously, hidden, or only when differing from defined values.

Ion Optical System Voltages

Source and Ion Tunnel Voltages

Typical voltages for ES/APcI probes, sample cone, and ion tunnels.

Analyser Voltages

Typical voltages for RF Lens, Aperture, and Ion Energy.

Data Acquisition: Starting an Acquisition

Acquisition Methods

Single sample from tune page, multiple samples from MassLynx screen.

Starting Acquisition from Tune Page

Easiest way to acquire data, allowing parameter control and start/stop.

Data Acquisition Parameters

File Naming and Project Setup

Parameters for data file naming, directory, and project creation.

Acquisition Function Types

Types of acquisition functions: MS, MS2, Daughter, Parent, Neutral Loss, Neutral Gain.

Data Formats and Mass Range Specification

Data formats (Centroid, Continuum, MCA) and specifying mass range (Start/End Mass).

Multiple Sample Acquisitions

Setting up a Sample List

Using MassLynx sample list editor for quantitative analysis.

Starting Multi-Sample Acquisition

Steps to start multi-sample acquisition, including sample list dialog options.

Acquisition Processes and Automated Analysis

Pre-Run and Post-Run Processes

Running tasks before/after acquisition (e.g., switching off gases).

Automated Sample List Processing

Using Quantify Samples dialog for integration, calibration, and quantification.

Quantify Samples Dialog Options

Quantification Task Configuration

Options for integrating samples, calibrating standards, quantifying, printing reports.

Project and Sample Range Settings

Setting the project for data acquisition and defining the sample range for analysis.

Monitoring Data Acquisition

Acquisition Status Display

Acquisition status shown on MassLynx screen, MS panel, and status bar.

Acquisition Status Window

Displaying scan-by-scan statistical reports of acquisition progress.

Real-Time Chromatogram Update

Viewing chromatogram in real-time during acquisition via Display menu.

Real-Time Spectrum Update

Viewing spectrum in real-time during acquisition via Display menu.

Instrument Data Thresholds

Data Pre-processing Parameters

Parameters controlling data pre-processing before sending to computer.

Setting Data Thresholding Options

Specifying data types for acquisition/discarding, and parameter download.

Data Thresholding Parameters Explained

MaxEnt and Profile Data Settings

MaxEnt requirements and controls for profile data (Baseline Level, Points per Dalton).

Centroid and SIR Data Settings

Settings for centroid data (Minimum centroid height) and SIR data (SIR Baseline Level).

Ion Counting Threshold Settings

Threshold Application and Calculation

Setting intensity level below which data points are ignored, applied to all acquisitions.

Threshold Value Recommendations

Guidance on setting Ion Counting Threshold values for optimal noise removal.

Profile Data: Spike Removal

Spike Identification and Removal

How spikes are distinguished and removed by averaging neighbours.

Spike Removal Parameter Settings

Parameters for spike removal: Use Spike Removal, Min Spike Intensity, Spike Percentage Ratio.

Spike Removal and Analog Data

Spike Removal Processing Impact

Spike removal processing impact on acquisition rates and parameter settings.

Analog Data Acquisition Settings

Setting number of samples per second for analog data.

System Manager Communications Status

Checking communications status between MassLynx software and the embedded PC.

Acquisition Control

Stopping an Acquisition

Methods to halt an acquisition from the tune page or MassLynx screen.

Function List Editor Introduction

Purpose of function list editor for setting up scan sequences during acquisition.

Function List Editor Interface

Simple Function List Example

Example of a simple function list with time scale display.

Complex Function List Example

Example of a complex list with multiple SIR functions and selection.

Function List Editor Operations

Function List Editor Toolbar

Toolbar buttons for creating, opening, saving, and printing function lists.

Adding New Functions

How to add new functions using toolbar buttons or the Function menu.

Managing Function List Entries

Modifying and Copying Functions

Steps to modify existing functions or copy them using edit menu options.

Removing and Reordering Functions

Procedures for removing functions and changing their order in the list.

Function List Settings: Solvent Delay and Analog Channels

Setting Solvent Delay Period

How to set a solvent delay period to prevent solvent peaks from eluting.

Analog Channel Configuration

Acquiring and storing analog data from external units like UV detectors.

Function List File Management

Saving Function Lists

Procedures for saving current function lists, including overwriting existing files.

Restoring Function Lists

How to restore previously saved function lists from file.

Full Scan Function Setup

Mass Range and Retention Time Settings

Setting start/end mass and start/end time for acquisition.

Cone Voltage and Method Settings

Using tune page cone voltage and specifying ionization mode and data type.

Full Scan Data Types and Scan Speed

Data Types: Centroid, Continuum, MCA

Explanation of Centroid, Continuum, and MCA data types and their storage.

Scan Duration and APcI Probe Settings

Scan Time, Inter-Scan Delay, and APcI Probe Temperature settings.

Setting up a Selected Ion Recording (SIR) Function

SIR Function Editor Overview

Editor for entering masses, dwell times, and inter-channel delay times for SIR.

SIR Channels Configuration

Entering up to 32 masses to monitor, with dwell and cone values.

SIR Function Parameters

Modifying SIR List Entries

Double-clicking to display values, changing Mass, Dwell, Cone, and sorting.

Method and Retention Window Settings

Inter Channel Delay, Repeats, Span, and Retention Window (Start/End) settings.

Setting up MS-MS Scanning Functions

Daughter Ion Scan Setup

Setting up Daughter scan using MS1 for parent mass and MS2 for fragment mass range.

Parent Ion Scan Setup

Setting up Parent scan using MS1 to scan and MS2 for fragment mass.

MS-MS Scan Types: Parent, MS2, Neutral Loss

Parent Ion Scan

Looking for the parent of a fragment, scanning MS1 over a range.

MS2 and Neutral Loss Scan

MS2 mode for resolving, Neutral Loss for detecting specific neutral fragments.

Collision Energy Settings

Setting Collision Energy Value

Specifying collision energy in electron volts for the collision cell.

Applying Collision Energy Ramp

Setting up a collision energy ramp by defining values at two masses.

MS-MS Function Setup: MRM and Survey

Setting up MRM Function

Setting up MRM functions similar to SIR, monitoring MS-MS transitions.

Setting up Survey Function

Using Survey scans to search for precursor ions.

Survey and MS-MS Template Pages

Parameter Setup Pages

Pages for setting parameters for MS and MS-MS scanning during survey.

MS to MSMS Switching Criteria

Switching Conditions Definition

Criteria for switching from MS to MSMS based on TIC or Intensity thresholds.

Precursor Selection Methods

Automatic, Include Masses Only, and Include Masses and Automatic precursor selection.

Precursor Inclusion and Data Handling

Detected Precursor Inclusion Options

Auto exclude, Always include, and Include after time options.

Data Handling for Survey Scans

Discarding uninteresting survey scans to save disk space.

MSMS to MS Switching Method

Switch Method Options

Default method or After Time method for stopping MSMS functions.

Switch Criteria Definition

Defining when MS scanning resumes based on conditions and threshold values.

Including and Excluding Masses for MS-MS

Mass Range Entry for Inclusion/Exclusion

Entering mass ranges and individual masses to include or exclude from MS-MS scans.

Monitoring Acquisitions Status

Automatic Switching Status Dialog

Display showing precursors currently running during an acquisition.

Mass Calibration Introduction

Calibration Process Overview

Overview of calibration process, including ES and APcI calibration.

Reference Information for Calibration

Reference to calibration solutions and their preparation.

Mass Calibration Overview

Automated Mass Calibration Process

How MassLynx NT performs automated calibration using reference compounds.

Required Calibration Types

Static, scanning, and scan speed compensation calibrations for MS1 and MS2.

Performing a Mass Calibration

Calibration Steps

Steps: Tuning, selecting reference file, starting automatic calibration, checking report.

Electrospray Calibration Introduction

Sensible to calibrate over a wide mass range using NaI/RbI for ES.

Electrospray Calibration Preparation

Reference Compound Introduction Methods

Using injector loop or infusion pump for reference compound introduction.

Tuning for Electrospray Calibration

Setting Multiplier, source/ion energy parameters for unit mass resolution.

Instrument Threshold Parameters for Calibration

Parameter Checks Before Calibration

Checking parameters like data acquisition mode and scanning speeds.

Profile Data Settings for Calibration

Setting Profile Data to Compressed and 16 Points per Dalton for low mass calibration.

Calibration Options and File Management

Accessing Calibration Options

Selecting Calibration > Calibrate Instrument from the tune page.

Selecting and Removing Reference Files

Selecting reference files and removing current calibrations to ensure a clean state.

Calibration Parameters Setup

Automatic Calibration Check Parameters

Setting limits for missed peaks and standard deviation for successful calibration.

Span Correction and Range Checks

Options for Span Correction and Acquisition Calibration Ranges checks.

Calibration Parameter Details

Peak Match and Intensity Threshold

Peak Match parameters (window, error) and Intensity threshold for data inclusion.

Polynomial Order for Curve Fit

Selecting polynomial order (1-5) for calibration curve fitting, with recommendations.

Mass Measure Parameters for Calibration

Parameters for Continuum/MCA Data

Settings for Mass Measure when continuum or MCA data are acquired for calibration.

Centroiding Parameters for High Scan Speeds

Adjusting centroiding parameters for high scan speeds to maintain resolution.

Performing a Mass Calibration

Calibration Types Selection

Selecting static, scanning, and scan speed compensation for MS1 and MS2.

Calibration Acquisition and Verification Options

Checking Acquire & Calibrate and Acquire & Verify options for calibration process.

Complete Calibration Procedure

Types and Process Selection for Full Calibration

Checking all calibration types (Static, Scanning, Scan Speed Comp.) for MS1 and MS2.

Acquire, Calibrate, and Print Report Options

Selecting options in the Process area to perform and report the calibration.

Calibration Acquisition Parameters

Setting Acquisition Parameters

Configuring mass range, run time, and data type for calibration.

Scan Parameters and Run Duration

Setting scan parameters and ensuring adequate run duration.

Calibration Scan Speed Settings

Static Span and Dwell Time Settings

Setting static span size around reference peaks and dwell time.

Slow and Fast Scan Time Settings

Determining scan speeds for scanning calibration and scan speed compensation.

Starting the Mass Calibration Process

Calibration File Acquisition Order

Order in which calibration files (STATMS1, SCNMS1, FASTMS1 etc.) are acquired.

Calibration Report and Status Message

Display of status messages and printed calibration reports upon completion.

Instrument Calibration Report Details

MS1 Calibration Plots

Plots for MS1 Static, Scanning, and Scan Speed calibrations.

MS2 Calibration Plots

Plots for MS2 Static, Scanning, and Scan Speed calibrations.

Checking the Mass Calibration

Viewing Calibration Details

Accessing calibration reports to view spectra and mass differences.

Manual Peak Matching Verification

Examining peak matching and highlighting matched peaks in expanded regions.

Calibration Failure Analysis

Reasons for Calibration Failure

Causes: no peaks, missed peaks, incorrect mode, threshold/window settings, wrong file.

Troubleshooting Calibration Failures

Interpreting Missed Peaks

Checking report for missed peaks and identifying potential causes.

Accepting or Rejecting Calibration

Checking peak matches and deciding to accept or cancel the calibration.

Detecting Incorrect Calibration

Causes of Incorrect Peak Matching

Parameters leading to incorrect matching: threshold, error, window, std deviation.

Handling Contamination and Background Peaks

Strategies for dealing with contamination peaks affecting peak matching.

Manual Calibration Adjustments and Saving

Manual Peak Matching Editing

Excluding or including peaks manually via the calibration report.

Saving Successful Calibration

Saving a fully calibrated instrument state for future recall.

Calibration Verification Process

Performing Calibration Verification

Performing verification instead of full recalibration, checking scanning acquisition.

Verification Setup and Procedure

Accessing dialogs, setting parameters, and starting verification procedure.

Calibration Verification Report

Verification Results Display

Display of verification results without changing instrument calibration.

Electrospray Calibration with PEG

PEG Spectrum Characteristics

Understanding PEG spectrum, doubly charged ions, and effects of ammonium acetate/cone voltage.

APCI Mass Calibration Introduction

APCI Calibration Overview

Complete mass calibration using APcI and reference compound preparation.

APCI Procedure Steps

Procedure requires multiple steps due to short residence time of reference solution.

APCI Calibration Preparation and Options

Reference Compound Introduction for APcI

Using injection loop and solvent delivery system for APcI reference introduction.

APCI Calibration Options Selection

Accessing options, selecting reference files, and removing current calibrations.

Selecting APcI Calibration Parameters

Recommending Polynomial order 2 for Curve Fit in APcI calibration.

Performing APcI Mass Calibration

Static Calibration Setup

Setting up static calibration for MS1, checking Acquire & Calibrate.

APCI Acquisition Parameters Setup

Default parameters for APcI reference file (pegh1000.ref), including mass range and data type.

APCI Data Acquisition for Calibration

Static Calibration Data Acquisition

Acquiring data using STAT file name, injecting reference solution.

Manual Calibration Check

Advisability of checking calibration manually whether successful or failed.

Manual APcI Calibration

Performing Manual Calibration

Using chromatogram window and Process, Combine Spectra to determine scan numbers.

Manual Calibration Report and Verification

Selecting Static calibration type and MS1, entering scan ranges, displaying report.

Troubleshooting Manual Calibration

Insufficient or Incorrect Peak Matching

Referring to Calibration Failure section for peak matching issues.

Printing and Accepting Manual Calibration

Printing Calibration Report

Printing the calibration report from the report display.

Accepting the Calibration

Selecting OK from the calibration report to accept the calibration.

Scanning Calibration and Scan Speed Compensation

Acquiring Data for Scanning Calibration

Acquiring two data files at slowest and fastest speeds for scanning calibration.

Scan Speed Settings and Data Type

Setting Scan From/To, Scan Time, Inter Scan Delay, and Data Type.

Manual Scanning Calibration

Manual Scanning Calibration Procedure

Selecting Scanning type and MS1, entering start/end scans from report.

Comparing Spectra for Match Verification

Comparing acquired and reference spectra to ensure correct peak matching.

Scan Speed Compensation and MS2 Calibration

Scan Speed Compensation Procedure

Procedure using fast scanning file (FASTMS1) for scan speed compensation.

Calibrating MS2

Performing calibration for MS2 by acquiring data in MS2 mode instead of MS1.

Mass Calibration Failure Analysis

Manual Calibration Failure Detection

Judging calibration success by examining on-screen report; no warning message.

Causes of Manual Calibration Failure

Reasons for failure: no peaks, missed peaks, incorrect mode, threshold settings, wrong reference file.

Troubleshooting Manual Calibration Failures

Interpreting Missed Peaks in Manual Calibration

Checking report for missed peaks and identifying causes like low threshold or window settings.

Handling Contamination in Manual Calibration

Dealing with contamination peaks affecting peak matching and potential solutions.

Manual Calibration Adjustments and Saving

Manual Peak Matching Editing

Excluding or including peaks manually via the calibration report.

Saving Calibration Settings

Saving calibrated states for different ionisation modes or future recall.

Manual Calibration Verification

Performing Manual Verification

Setting up scanning acquisition and accessing calibrate dialog for verification.

Verifying Calibration Parameters

Setting peak matching parameters and selecting verification options.

Calibration Verification Results

Verification Report Display

Display of verification results without changing instrument calibration.

Electrospray Ionisation Introduction

ESI Interface and Probe Description

Description of Z-spray source, electrospray probe, and optional nanoflow interface.

ESI Process and Applications

How mobile phase becomes aerosol spray, and applications for various analytes.

Electrospray Sample Delivery Methods

Syringe Pump and Reciprocating Pump Operation

Common methods for delivering sample, including injection valve use.

Infusion Pump and Solvent Recommendations

Using infusion pump, mobile phase composition, and solvent degassing.

Electrospray Flow Rate Checks

Periodically Checking Flow Rate

Method for checking flow rate from solvent delivery system and monitoring back pressure.

Post-column Splitting in Electrospray

Splitting for Sample Saving

Recommendation to split flow post-column to approximately 200 µl/min for saving samples.

Split Ratio Adjustment

Adjusting split ratio by back pressure in waste line, and incorporating UV cell.

Electrospray Flow Modes

Megaflow Electrospray Operation

Enabling flow rates from 200 µl/min to 1 ml/min using microbore columns.

Changing Flow Mode Tubing

Using correct tubing (1/16" o.d., 0.007" i.d. peek) for megaflow operation.

Electrospray Operation: Initial Setup

Source Assembly and Gas Connection

Ensuring source assembly, nitrogen supply, and exhaust liner are correctly fitted.

Optimizing for Low Flow Rates

Importance of exhaust liner and baffle for optimal intensity and stability at low flow rates.

Checking the Electrospray Ionisation (ESI) Probe

Probe Connection and Flow Check

Connecting probe to pump, checking liquid flow at tip, and turning on nitrogen.

Nebulisation and Probe Tip Adjustment

Adjusting probe tip for complete nebulisation and checking capillary alignment.

Electrospray: Obtaining and Optimizing Ion Beam

Obtaining the Ion Beam

Changing ionisation mode, setting desolvation gas flow, liquid flow, and temperature.

Tuning and Optimizing Ion Beam

Optimizing parameters using a representative analyte sample.

Probe Position Adjustment for Ion Beam

Adjusting probe position (in/out, sideways) for optimal sensitivity and stability.

Electrospray Source Gas Controls

Probe Position Optimization Details

Further details on probe position adjustment and considerations for higher liquid flow rates.

Nebuliser and Desolvation Gas Control

Optimizing nebulisation by fully opening Nebuliser valve and adjusting Desolvation Gas flow.

Electrospray Source Gas and Temperature Settings

Desolvation Temperature and Gas Flow Guide

Table relating solvent flow rate to Desolvation Temp and Gas Flow Rate.

Cone Gas and Purge Gas Function

Role of Cone Gas in reducing cluster ions and Purge Gas for removing solvent vapour.

Electrospray Source Restrictor Adjustment

Restrictor Function and Adjustment

How restrictor affects source pressure and sensitivity, and adjustment precautions.

Electrospray Source Operating Parameters

Source and Probe Temperature Settings

Typical and maximum source temperatures, APcI probe temperature settings.

Capillary and Sample Cone Voltages

Optimal voltage ranges for capillary and sample cone for electrospray.

Electrospray Ion Optical Parameter Tuning

RF Lens and Aperture Voltages

Adjusting RF Lens 1/2 and Aperture voltages for sensitivity and fragmentation.

Mass Resolution and Ion Energy Optimization

Optimizing mass resolution and ion energy for peak shape and resolution.

Megaflow Electrospray Operation

Megaflow Setup Adjustments

Adjustments for megaflow: drying gas, desolvation temp, source temp, probe position.

Removing the Electrospray Probe

Steps to safely remove the probe from the source, including deselecting Operate.

Sample Analysis and Calibration Guidelines

Sample Preparation and Concentration

Ensuring samples are dissolved, filtered, and using optimal concentrations.

Reference Samples for Analysis

Examples of reference samples like myoglobin and PEG for calibration.

Typical Electrospray Ion Samples

Positive Ion Sample Types

List of common sample types analyzed in positive ion mode.

Negative Ion Sample Types

List of common sample types analyzed in negative ion mode.

Chromatographic Interfacing with Electrospray

Microbore and Capillary Column Interfacing

Interfacing 1mm columns, using syringe pumps, and solvent mixing.

2.1mm and 4.6mm Column Interfacing

Interfacing 2.1mm/4.6mm columns, UV detector use, and solvent considerations.

LC-MS Sensitivity Enhancement Strategies

Improving LC-MS Sensitivity

Increasing sensitivity via LC (columns, trace enrichment) and MS (narrow scan, SIR).

Nanoflow Electrospray Overview

Nanoflow Interface Capabilities

Performing ESI at 5-1000 nl/min using glass capillary or Nano-LC options.

Installing the Nanoflow Interface

Interface Components and Rotation

Description of nanoflow end flange, manipulator, stage, and rotation procedure.

Probe and Source Enclosure Removal

Steps for removing probe and glass tube, warning about exposed heater.

Nanoflow Interface Installation Steps

Probe Flange and Cone Gas Nozzle Setup

Unscrewing pillars, fitting cone gas nozzle, connecting gas outlet.

Final Assembly and Cover Installation

Fitting O rings, perspex cover, and nanoflow end flange.

Nanoflow Interface Setup: Lighting and Connections

Microscope/Camera Bracket and Light Source

Attaching brackets, inserting light guide, and setting light source brightness.

Blocking Gas Outlets and Connecting Cables

Blocking gas outlets and connecting Capillary/Corona and ESI/APcI cables.

Nanoflow Camera and Microscope Operation

Camera System Magnification Control

Controlling magnification with zoom lens and fine focus with objective lens.

Microscope Focusing Adjustment

Adjusting microscope focus by rotating its top.

Nanoflow Glass Capillary Option

Glass Capillary Handling and Installation

Handling fragile capillaries, removing unions, passing nut/elastomer/union.

Capillary Setup and Nitrogen Flow

Tightening nut for capillary protrusion, loading sample, setting Capillary voltage, turning on nitrogen.

Nanoflow Spray Restart Procedure

Restarting Spray with Manipulator Adjustment

Restarting spray by adjusting manipulator to touch sample cone and shear glass hair.

Applying Back Pressure for Spray Restart

Using back pressure to force liquid from capillary if spray stops.

Nanoflow Nano-LC Option Installation

Preparing Tubing and Fittings

Cutting tubing, setting ferrule position, threading fused silica through fitting.

Assembling Nano-LC Chamber

Ensuring silica flush, tightening nut, placing O ring, threading silica through chamber.

Nanoflow Nano-LC Option Operation

Checking Capillary Flow

Connecting capillary to syringe pump for flow check, cutting fused silica, attaching tubing.

Nano-LC Setup and Operation

Setting liquid flow, gas pressure, viewing spray, adjusting stage and capillary voltage.

Nanoflow Option Switching

Switching Between Capillary and Nano-LC

Rotating stage outwards, removing/replacing protective cover and holder.

HPLC System Plumbing

Connecting sprayer to HPLC system, detailing injection valve plumbing (P, C, S, W).

Atmospheric Pressure Chemical Ionisation (APCI) Introduction

APCI Principle and Applications

APCI for singly-charged molecules, suitability for LC-MS with high organic/aqueous phases.

APCI Interface Components

Description of Z-spray source with corona discharge pin and heated nebuliser probe.

APCI Operation: Desolvation Gas and Preparation

Desolvation Gas and Background Spectrum

Importance of desolvation gas, background spectrum dependence on Cone setting.

APCI Preparation Steps

Source assembly, nitrogen supply connection, and baffle fitting for APcI.

Checking the APcI Probe

Probe Heater and Gas Flow Checks

Ensuring probe heater is off, connecting PTFE tube to Nebuliser, checking gas flow.

Liquid Jet and Aerosol Formation

Checking liquid jet flow, LC pump back pressure, nitrogen pressure, and aerosol formation.

APCI Operation: Obtaining an Ion Beam

Ion Beam Acquisition Steps

Setting Source/Probe Temps, Corona, Cone, Desolvation Gas, Nebuliser Gas.

Tuning and Probe Position for Beam

Adjusting Mass/Span, Gain, Probe position (in/out, sideways) for optimal ion beam.

APCI Ion Beam Stability and Tuning

Stable Solvent Ion Beam Check

Checking for a stable beam of solvent ions and referring to Sample Analysis hints.

APCI Operation Warnings

Warnings about source enclosure temperature and switching off liquid flow before probe removal.

APCI Sample Analysis Hints

Tuning for Qualitative Analysis

Typical parameters for qualitative analysis of mixtures.

Tuning for Maximum Sensitivity

Optimizing APcI conditions for quantitative MRM analysis using standard solutions.

APCI Source Parameter Optimization

Corona Current Optimization

Adjusting Corona current for optimal sensitivity based on compound polarity.

Probe Position and Temperature Optimization

Adjusting probe position and APcI Probe Temp for maximum sensitivity.

Desolvation Gas Effect on Noise

Desolvation gas effect on chemical background noise levels, checked using MRM mode.

Removing the APcI Probe

APcI Probe Removal Steps

Turning off LC flow, setting probe temp, deselecting Operate, turning off nitrogen.

Probe Removal Warnings

Warnings about burns risk and shortening probe heater life if removed when hot.

Maintenance and Fault Finding Introduction

General Maintenance Precautions

Importance of cleanliness, preparing workspace, handling components carefully.

Cooling Fans and Air Filters

Ensuring fans are unobstructed and checking/replacing fan filters.

Vacuum System Performance and Issues

Impact of Poor Vacuum on Performance

How analyser pressure affects performance (resolution, noise) and LED indications.

Vacuum System Fault Diagnosis Points

Points to note before suspecting a leak: turbopump operation, rotary pump maintenance, over-temperature.

Vacuum System Troubleshooting

Locating Vacuum Leaks

Basic points for locating leaks: suspect disturbed components, check flanges and O rings.

Pirani and Magnetron Gauge Maintenance

Pirani gauge requires no routine maintenance; Magnetron gauge cleaning refers to Edwards literature.

Rotary Pump Gas Ballasting and Oil Recirculation

Gas Ballasting Purposes

Purging oil of contaminants and returning oil mist from filter via gas ballasting.

E1M18 and E2M28 Pump Operation

Recommended continuous gas ballast for E1M18, manual operation for E2M28.

Rotary Pump Maintenance: Ballasting and Filters

Ballasting Cautions

Cautions regarding frequent ballasting and venting with E2M28 manual gas valve open.

Oil Mist Filter Maintenance

Maintenance of oil mist filter elements: odour and mist elements.

Foreline Trap Maintenance

Replacing sorbent in foreline trap based on discoloration or schedule.

Rotary Pump Oil Maintenance

Maintaining Rotary Pump Oil Level and Condition

Checking oil level weekly, replacing oil based on color or intervals.

Procedure for Changing Rotary Pump Oil

Steps for changing oil: gas ballasting, venting, draining, flushing, refilling.

The Source Assembly Overview

Source Basic Components

Three basic parts: probe adjustment flange, glass tube, source flange assembly.

Accessing Source Components

Removing probe flange and glass tube for access to cone, nozzle, pin, baffle, nanoflow interface.

Cleaning Source Components

Cleaning cone, nozzle, ion block, and hexapole lens, with warnings on solvents.

Cleaning the Cone Gas Nozzle and Sample Cone

Cone Gas Nozzle and Sample Cone Cleaning Procedure

Steps for cleaning: launching tune page, switching off pumps/flow, setting temps, disconnecting gas.

Cleaning Warnings and Tips

Warnings about hot components, probe heater life, and using ultrasonic bath.

Source Component Cleaning and Isolation

Disconnecting Electrical and Probe Connections

Disconnecting electrical connections and removing probe/flange/tube.

Isolation Valve Operation

Rotating isolation valve to its fully anticlockwise position.

Sample Cone and Nozzle Cleaning Details

Cone Gas Inlet Line Disconnection

Disconnecting cone gas inlet line and using extraction tool.

Sample Cone Handling and Cleaning

Removing sample cone, gasket, and nozzle, wiping with swabs or ultrasonic bath.

Reassembling Source Components

Drying and Cleaning Baffle/Liner

Drying cone/nozzle with nitrogen, removing/cleaning/replacing baffle and liner.

Refitting Cone/Nozzle and Isolation Valve

Refitting sample cone/nozzle, noting isolation valve position.

Removing and Cleaning the Ion Block

Vent Instrument and Remove Components

Venting instrument, removing source enclosure, cone, nozzle as described previously.

Ion Block Cover Plate Removal

Cover Plate Removal Steps

Removing screws and washers to remove the cover plate from the ion block.

Heater Supply Warning

Warning that heater supply remains live until system is fully vented.

Ion Block Removal and Component Handling

Disconnecting Heater and Thermocouple

Removing screws from heater connections, straightening leads, unhooking thermocouple.

Ion Block Support and O Ring Checks

Removing screws securing ion block, withdrawing block, checking O rings.

Cleaning the Ion Block Assembly

Restrictor Bush Removal and Cleaning

Unscrewing restrictor bush, collecting washer, wiping restrictor end.

Ultrasonic Cleaning of Ion Block

Immersing ion block in ultrasonic bath with solvents and drying components.

Removing and Cleaning the Ion Tunnel Assembly

Ion Tunnel Assembly Removal Steps

Removing ion block, screws for support, withdrawing ion tunnel carefully.

O Ring and Pumping Block Caution

Ensuring O ring location and caution about scratching pumping block internal bore.

Cleaning the Ion Tunnel Assembly

Sonication and Drying of Ion Tunnel

Immersing assembly in solvent for sonication and drying with nitrogen.

Severe Case Cleaning Procedures

Removing differential aperture plate, cleaning with glass fibre pencil and ultrasonic bath.

Reassembling and Checking the Source

O Ring Checks and Spring Loading

Checking O rings, feeding hexapole transfer lens with springs.

Replacing Ion Block Support and Restrictor

Replacing ion block support, screws, restrictor, bush, washer, and ion block.

Final Source Reassembly Steps

Connecting Thermocouple and Cover Plate

Inserting thermocouple, reconnecting heater leads, replacing cover plate.

Isolation Valve and Pump Down Check

Checking isolation valve closure and clicking Pump after instrument pumps down.

The Discharge Pin: Cleaning and Replacement

Procedure for cleaning or replacing the APcI corona discharge pin.

Electrospray Probe Maintenance

Indications for Probe Maintenance

Unstable ion beam, peak broadening/tailing, high LC pump back pressure.

Troubleshooting Probe Blockages

Clearing blockages in sample capillary or tubing, using formic acid.

Electrospray Probe Blockage and Gas Flow Issues

Clearing Sample Capillary Blockages

Flushing capillary with solvent or reverse flushing to clear blockages.

Gas Flow Problem Checks

Checking all gas connections for leaks using soap solution or leak searching agent.

Replacing the Stainless Steel Sample Capillary

Probe Removal and Disconnection

Removing probe, LC line, nut, grub screw, cover, and probe tip.

Capillary Replacement Procedure

Removing old capillary, remaking LC connection, sleeving new capillary.

Connecting the New Sample Capillary

Connecting Capillary to LC Union

Using GVF/16 ferrule and adapter nut to connect capillary to LC union.

Final Probe Assembly and Tightening

Feeding capillary through probe, adjusting tip protrusion, replacing cover and tightening grub screw.

The APcI Probe: Maintenance and Cleaning

Indications for APcI Probe Maintenance

Probe tip contamination, peak broadening/tailing, low/high LC pump back pressure.

Cleaning the APcI Probe Tip

Removing deposits from probe heater with a brush soaked in methanol:water.

Replacing the APcI Probe Tip Heater

Probe Tip Assembly Removal

Loosening grub screws to remove probe tip assembly, disconnecting heater.

Fitting and Reconnecting Heater Assembly

Fitting a new heater assembly and reconnecting the probe tip assembly.

Replacing the Fused Silica Capillary (APCI)

Probe Removal and Filter Disconnection

Removing probe tip assembly, heater, end cover, retaining screws, and loosening filter.

Cutting and Connecting New Capillary

Cutting new fused silica capillary and connecting it to the filter using ferrule and adapter nut.

Finalizing Fused Silica Capillary Replacement

Feeding and Adjusting New Capillary

Feeding capillary through probe, cutting at nebuliser, adjusting protrusion.

Polyamide Coating Removal and Reassembly

Removing polyamide coating, re-feeding capillary, tightening adapter nut, replacing cover.

Analyser and Detector System

Analyser Contamination and Cleaning

Analyser quadrupoles should not require cleaning; pre-filter assembly cleaning infrequent.

Detector System Maintenance

Detector designed for trouble-free operation; seek assistance for issues.

Instrument Electronics and Fuses

High Voltage Warnings

Warning about high voltages present throughout the spectrometer.

Fuse List by PCB

Table listing fuse numbers, types, and reference numbers for various PCBs.

Fault Finding: No Beam and Low Intensity

Troubleshooting 'No Beam' Condition

Checks for no beam: tuning, cables, Operate mode, source assembly, isolation valve, errors.

Diagnosing Unsteady or Low Intensity Beam

Checks for unsteady beam: gas/liquid flows, analyser pressure.

Identifying Ripple Issues

Causes of ripple: unstable power supplies, photomultiplier supply, vibration.

High Noise Levels in MRM Analyses

Distinguishing Chemical vs. Electronic Noise

Method to distinguish noise types by setting ion energies negative.

Addressing Chemical Noise

Troubleshooting carry-over, LC contaminants, MRM transitions, solvent purity.

Noise Troubleshooting and Back Pressure

Addressing Electronic Noise

Adjusting ion counting threshold, comparing measurements, engineer investigation.

Resolving High Back Pressure in Electrospray

Causes of high back pressure (blockage) and methods to clear it.

Troubleshooting General Performance Loss

Checking Source/Probe Voltages

Checking voltage readbacks and reassembly of source/hexapole transfer lens.

Service Engineer Investigation

Further investigation requiring qualified service engineer personnel.

Cleaning Materials and Procedures

Recommended Abrasives for Cleaning

Using 600/1200 grade emery paper or lapping paper for metal components.

Recommended Solvents for Cleaning

Solvents like IPA, Methanol, Acetone for cleaning, followed by blotting dry.

Preventive Maintenance Checklist

Weekly Maintenance Tasks

Gas ballast, checking oil level/colour, checking water chiller.

Monthly and Quarterly Tasks

Changing oil mist filter elements, sorbent in foreline trap.

Four-Monthly Maintenance Tasks

Changing oil mist filter mist element and changing rotary pump oil.

Reference Information Overview

Calibration Reference File Format

Format of calibration files (two columns: mass, intensity).

Purchasing Samples from Sigma

Contact information for Sigma chemical company for ordering samples.

Editing Calibration Reference Files

Reading Reference Files into Notepad

Steps to read currently selected reference file into Notepad text editor.

Saving Edited Reference Files

Procedures for saving edited files, including new and overwrite options.

Positive Ion Calibration Reference Files

Reference Files for Protein and Hb Analysis

UBQ, HBA, SOD, HBB, MYO reference files for various analyses.

Reference Files for ES and APcI Calibration

PEGH1000, PEGH2000, NAICS, NAIRB files for ES and APcI calibration.

Positive Ion Reference Data: Myoglobin and PEG

Horse Heart Myoglobin Reference Data

Calculated m/z values for Horse Heart Myoglobin (myo.ref).

Polyethylene Glycol Reference Data

Calculated m/z values for Polyethylene Glycol (PEGH1000, PEGH2000).

Positive Ion Reference Data: Inorganic Salts

Sodium Iodide/Caesium Iodide Mixture Data

Calculated m/z values for NAICS reference file.

Sodium Iodide/Rubidium Iodide Mixture Data

Calculated m/z values for NAIRB reference file.

Negative Ion Calibration Reference Files

Negative Ion Sample Types

MYONEG, SUGNEG, NAINEG reference files for general, low mass, and ES calibration.

Horse Heart Myoglobin Negative Ion Data

Calculated m/z values for MYONEG reference file.

Mixture of Sugars Negative Ion Data

Calculated m/z values for SUGNEG reference file.

Negative Ion Reference Data: Inorganic Salts

Sodium Iodide/Iodide Mixture Data

Calculated m/z values for NAINEG reference file.

Preparation of Calibration Solutions

PEG + Ammonium Acetate for ES and APcI

Preparation of PEG solutions with ammonium acetate for positive ion ES and APcI calibration.

PEG + Ammonium Acetate (Extended Mass Range)

Preparation of PEG solutions for extended mass range positive ion ES calibration.

Preparation of Sodium Iodide Calibration Solutions

Method 1: Sodium Iodide/Caesium Iodide

Preparation of NaI/CsI solution for positive ion ES calibration, use of NAICS.REF.

Method 2: Sodium Iodide/Rubidium Iodide

Preparation of NaI/RbI solution for positive ion ES calibration, use of NAIRB.REF.

Solution for Negative Ion Electrospray

Suitability of solutions for negative ion calibration, use of NAINEG.REF.