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The OptaMax NG Ion Source User Guide provides instructions for operating the ion source in H-ESI, APCI, and APPI modes. It includes information on compatible mass spectrometers, safety precautions, maintenance, and replaceable parts. The document is intended for research use only and is subject to copyright restrictions.

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0% found this document useful (0 votes)
51 views

Optamax-ng-ion-source-user

The OptaMax NG Ion Source User Guide provides instructions for operating the ion source in H-ESI, APCI, and APPI modes. It includes information on compatible mass spectrometers, safety precautions, maintenance, and replaceable parts. The document is intended for research use only and is subject to copyright restrictions.

Uploaded by

17861166770a
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
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OptaMax NG

Ion Source User Guide


For H-ESI, APCI, and APPI Modes

80111-97029 Revision A June 2018


© 2018 Thermo Fisher Scientific Inc. All rights reserved.

OptaMax NG, nanoViper, TSQ Fortis, and Viper are trademarks; and Orbitrap, Thermo Scientific, Tribid,
TSQ Altis, and TSQ Quantis are registered trademarks of Thermo Fisher Scientific Inc. in the United States.
Fisher Scientific is a registered trademark of Fisher Scientific Co. in the United States.

The following are registered trademarks in the United States and other countries: Liquinox is a registered
trademark of Alconox, Inc. Microsoft and Windows are registered trademarks of Microsoft Corporation.

The following are registered trademarks in the United States and possibly other countries: APPI, PhotoMate,
and Syagen are registered trademarks of Morpho Detection, Inc. Tygon is a registered trademark of Saint-
Gobain Performance Plastics Company. Viton is a registered trademark of DuPont Performance Elastomers
LLC.

Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use in the
product operation. This document is copyright protected and any reproduction of the whole or any part of this
document is strictly prohibited, except with the written authorization of Thermo Fisher Scientific Inc.

The contents of this document are subject to change without notice. All technical information in this
document is for reference purposes only. System configurations and specifications in this document supersede
all previous information received by the purchaser.
This document is not part of any sales contract between Thermo Fisher Scientific Inc. and a purchaser. This
document shall in no way govern or modify any Terms and Conditions of Sale, which Terms and Conditions of
Sale shall govern all conflicting information between the two documents.

Release history: Rev A, June 2018

For Research Use Only. Not for use in diagnostic procedures.


WEEE Directive
2012/19/EU

Thermo Fisher Scientific is registered with B2B Compliance (B2Bcompliance.org.uk) in the UK and with the
European Recycling Platform (ERP-recycling.org) in all other countries of the European Union and in Norway.

If this product is located in Europe and you want to participate in the Thermo Fisher Scientific Business-to-Business
(B2B) Recycling Program, send an email request to [email protected] with the following information:
• WEEE product class
• Name of the manufacturer or distributor (where you purchased the product)
• Number of product pieces, and the estimated total weight and volume
• Pick-up address and contact person (include contact information)
• Appropriate pick-up time
• Declaration of decontamination, stating that all hazardous fluids or material have been removed from the product

For additional information about the Restriction on Hazardous Substances (RoHS) Directive for the European Union,
search for RoHS on the Thermo Fisher Scientific European language websites.

IMPORTANT This recycling program is not for biological hazard products or for products that have been medically
contaminated. You must treat these types of products as biohazard waste and dispose of them in accordance with
your local regulations.
C

Contents
Preface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ix
Accessing Documentation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .ix
Compatible Mass Spectrometers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . x
Special Notices, Symbols, and Cautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . x
Safety Precautions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xii
Regulatory Compliance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xii
Contacting Us . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .xiii

Chapter 1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1
Preferred Ionization Modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
H-ESI Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
Guidelines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
APCI Mode. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
APPI Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
APPI Light Source. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
API Spray Insert Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

Chapter 2 API Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9


API Source Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
Solvent Waste System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
API Spray Inserts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
H-ESI Spray Insert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
APCI Spray Insert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Removing and Installing the API Spray Insert . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Removing and Installing the API Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Removing the API Source from the Mass Spectrometer. . . . . . . . . . . . . . . . . 18
Installing the API Source onto the Mass Spectrometer. . . . . . . . . . . . . . . . . . 19

Chapter 3 Changing the Ionization Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .23


Identifying the Ionization Configuration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Thermo Scientific OptaMax NG Ion Source User Guide v


Contents

Changing the Ionization Configuration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25


Changing the Position of the APCI Corona Discharge Needle . . . . . . . . . . . 27
Removing the APCI Corona Discharge Needle . . . . . . . . . . . . . . . . . . . . . . . 28
Configuring the API Source Housing for APPI Mode . . . . . . . . . . . . . . . . . . 29
Configuring the API Source Housing for H-ESI Mode . . . . . . . . . . . . . . . . . 33
Installing the H-ESI Grounding Union onto the API Source . . . . . . . . . . . . 34
Setting the Initial Ion Source Parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
Adjusting the Direction of the Spray Insert . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

Chapter 4 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .39


Maintenance Schedule. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
Tools and Supplies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
Flushing the Inlet Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
Maintaining the API Spray Insert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
Replacing the H-ESI Metal Needle Insert . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
Replacing the APCI Fused-Silica Sample Tube . . . . . . . . . . . . . . . . . . . . . . . 46
Maintaining the PhotoMate APPI Light Source . . . . . . . . . . . . . . . . . . . . . . . . 48
Maintenance for the APPI Lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
Maintenance for the APPI Fan Filter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
Maintaining the API Source Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

Chapter 5 Replaceable Parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .53


API Source Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
APCI Parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
APPI Parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53

Glossary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55

Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .57

vi OptaMax NG Ion Source User Guide Thermo Scientific


F

Figures
Figure 1. Polarity ranges for ESI, APCI, and APPI versus molecular weights . . . . . . . . . . . 2
Figure 2. APCI process in the positive ion polarity mode (cross-sectional components) . . . 5
Figure 3. Energetics of photoionization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
Figure 4. Selective photoionization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
Figure 5. Ionization potentials of typical compounds and solvents . . . . . . . . . . . . . . . . . . . 7
Figure 6. OptaMax NG ion source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
Figure 7. OptaMax NG ion source showing the H-ESI API spray insert, heater assembly,
and housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
Figure 8. OptaMax NG ion source (back and top view) . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Figure 9. Example solvent waste system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Figure 10. H-ESI (top) and APCI (bottom) API spray inserts . . . . . . . . . . . . . . . . . . . . . . . 13
Figure 11. H-ESI spray insert and its metal needle insert . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Figure 12. Sheath gas flow (blue lines) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Figure 13. Auxiliary gas flow (green lines) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Figure 14. APCI spray insert and its fused-silica needle insert . . . . . . . . . . . . . . . . . . . . . . . 16
Figure 15. Guide pin and guide pin slot locations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Figure 16. OptaMax NG ion source with unlocked levers (front view) . . . . . . . . . . . . . . . 19
Figure 17. Mass spectrometer mount assembly with ion sweep cone . . . . . . . . . . . . . . . . . 20
Figure 18. OptaMax NG ion source with unlocked levers (back view). . . . . . . . . . . . . . . . 21
Figure 19. Corona discharge needle adapter showing the On and knob positions . . . . . . . 28
Figure 20. Corona discharge needle (close-up view). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Figure 21. API source showing the left-side H-ESI components (exploded view) . . . . . . . 30
Figure 22. API source showing the left-side APPI components (exploded view). . . . . . . . . 31
Figure 23. Left side of the assembled APPI source with the APCI spray insert . . . . . . . . . . 32
Figure 24. Power connection to the APPI light source . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
Figure 25. Installed H-ESI grounding union and sample line (example) . . . . . . . . . . . . . . . 34
Figure 26. Front-to-back adjustment of the spray insert. . . . . . . . . . . . . . . . . . . . . . . . . . . 36
Figure 27. Side-to-side adjustment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
Figure 28. Depth adjustment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
Figure 29. Needle insert removed from the H-ESI spray insert . . . . . . . . . . . . . . . . . . . . . . 44
Figure 30. Installing the needle insert into the H-ESI spray insert . . . . . . . . . . . . . . . . . . . 44
Figure 31. Removing the fused-silica insert from the APCI spray insert . . . . . . . . . . . . . . . 46
Figure 32. APCI fused-silica insert assembly (exploded view). . . . . . . . . . . . . . . . . . . . . . . 47
Figure 33. Exit end of the fused-silica tubing protrudes 1 mm (0.04 in.) . . . . . . . . . . . . . . 48
Figure 34. PhotoMate APPI light source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

Thermo Scientific OptaMax NG Ion Source User Guide vii


Figures

viii OptaMax NG Ion Source User Guide Thermo Scientific


P

Preface
The OptaMax NG Ion Source User Guide describes how to install, remove, and maintain the
Thermo Scientific™ OptaMax NG™ source.

Note The Glossary defines some of the terms used in this guide.

• Accessing Documentation
• Compatible Mass Spectrometers
• Special Notices, Symbols, and Cautions
• Safety Precautions
• Regulatory Compliance
• Contacting Us

 To suggest changes to the documentation or to the Help

Complete a brief survey about this document by clicking the button below.
Thank you in advance for your help.

Accessing Documentation
Thermo Scientific mass spectrometers (MSs) include complete documentation. For system
requirements refer to the release notes on the software DVD.

 To view the product manuals

• (Windows 7) From the Microsoft™ Windows™ taskbar, choose Start > All Programs >
(Thermo Instruments > model x.x, and then open the applicable PDF file.
• (Windows 10) From the Windows taskbar, choose Start > All Apps> Thermo
Instruments > model x.x, and then open the applicable PDF file.

Thermo Scientific OptaMax NG Ion Source User Guide ix


Preface

 To view user documentation from the Thermo Fisher Scientific website

1. Go to thermofisher.com.
2. Point to Services & Support and click Manuals on the left.
3. In the Refine Your Search box, search by the product name.
4. From the results list, click the title to open the document in your web browser, save it, or
print it.
To return to the document list, click the browser Back button.

Compatible Mass Spectrometers


Install the OptaMax NG ion source on one of the Thermo Scientific TSQ Series II MSs, or
on an Orbitrap™ Tribrid™ Series MS.

If you have instrument compatibility questions, contact Thermo Fisher Scientific Customer
Service (see page xiii).

CAUTION The OptaMax NG ion source must connect to a certified Thermo Scientific
MS, which supplies high voltage capable of delivering a maximum of 8 kV and 100 μA.

Do not connect the ion source to another type of MS, as you might impair the protection
provided by the equipment.

Special Notices, Symbols, and Cautions


Make sure you understand the special notices, symbols, and caution labels in this guide. Most
of the special notices and cautions appear in boxes; those pertaining to safety also have
corresponding symbols. Some symbols are also marked on the API source itself and can
appear in color or in black and white. For complete definitions, see Table 1.
Table 1. Notices, symbols, labels, and their meanings (Sheet 1 of 2)
Notice, symbol, or label Meaning
IMPORTANT Highlights information necessary to prevent damage to
software, loss of data, or invalid test results; or might contain
information that is critical for optimal performance of the
product.
Note Highlights information of general interest.
Tip Highlights helpful information that can make a task easier.

x OptaMax NG Ion Source User Guide Thermo Scientific


Preface

Table 1. Notices, symbols, labels, and their meanings (Sheet 2 of 2)


Notice, symbol, or label Meaning
Caution: Read the cautionary information associated with this
task.

Chemical hazard: Observe safe laboratory practices and


procedures when handling chemicals. Only work with volatile
chemicals under a fume or exhaust hood. Wear gloves and other
protective equipment, as appropriate, when handling toxic,
carcinogenic, mutagenic, corrosive, or irritant chemicals. Use
approved containers and proper procedures to dispose of waste
oil and when handling wet parts of the instrument.
Hot surface: Before touching the API source assembly, allow
heated components to cool.

Risk of electric shock: When the mass spectrometer is


scanning. do not touch the grounding union, the solvent line or
the fittings that connect the grounding union to the probe’s
sample inlet. Doing so may result in an electrical shock that is
strong enough to cause an involuntary “startle” reaction leading
to injury.
Risk of electric shock: This instrument uses voltages that can
cause electric shock and personal injury. Before servicing the
instrument, shut it down and disconnect it from line power.
While operating the instrument, keep covers on.
Risk of eye injury: Eye injury can occur from splattered
chemicals, airborne particles, or sharp objects. Wear safety
glasses when handling chemicals or servicing the instrument.

Sharp object: Avoid handling the tip of the syringe needle.

Trip obstacle: Be aware of cords, hoses, or other objects located


on the floor.

Ultraviolet light hazard: For the APPI-configured ion source


(APPI source), do not look directly at the ultraviolet (UV) light
or into the UV source, or risk eye damage. Wear UV eye
protection.

Thermo Scientific OptaMax NG Ion Source User Guide xi


Preface

Safety Precautions
Observe the following safety precautions when you operate or perform service on the API
source.

CAUTION Do not perform any servicing other than that contained in this manual. To
avoid personal injury or damage to the instrument, do not perform any servicing other
than that contained in this manual or related manuals unless you are qualified to do so.

CAUTION Do not touch heated zones. Allow heated components to cool to room
temperature before you service them. The API source housing, its components, and the
MS’s ion transfer tube can be very hot and can cause severe burns if touched.

CAUTION Risk of eye damage. Do not look in the API source window at the ultraviolet
(UV) light during APPI mode operation. If you must do so, wear UV eye protection.

CAUTION Handle the APCI corona discharge needle with care. The corona discharge
needle is very sharp and can puncture your skin.

Regulatory Compliance
Thermo Fisher Scientific performs complete testing and evaluation of its products to ensure
full compliance with applicable North American and European regulations. The
OptaMax NG ion source was tested as part of the Thermo Scientific MS system, which meets
the applicable requirements in the electromagnetic compatibility (EMC) and product safety
standards. For additional regulatory information, refer to the MS manuals.

Unauthorized changes that you make to your system will void regulatory compliance and may
defeat the built-in protections for your instrument. Some examples of unauthorized changes
include using replacement parts or adding components, options, or peripherals that Thermo
Fisher Scientific has not qualified and authorized. Unauthorized changes can also result in
bodily injury and/or damage to your system and laboratory.

Ensure continued compliance with regulatory standards:


• Follow all installation instructions provided in the documentation that comes with your
system.
• Order replacement parts (as specified in the instrument manual) and additional
components, options, and peripherals directly from Thermo Fisher Scientific or an
authorized representative.

xii OptaMax NG Ion Source User Guide Thermo Scientific


Preface

Contacting Us
Contact Email Telephone QR Codea

U.S. Technical Support [email protected] (U.S.) 1 (800) 532-4752

U.S. Customer Service [email protected] (U.S.) 1 (800) 532-4752


and Sales

Global Support  To find global contact information or customize your request

1. Go to thermofisher.com.
2. Click Contact Us, select the country, and then select the type of support
you need.
3. At the prompt, type the product name.
4. Use the phone number or complete the online form.

 To find product support, knowledge bases, and resources

Go to thermofisher.com/us/en/home/technical-resources.

 To find product information

Go to thermofisher.com/us/en/home/brands/thermo-scientific.
Note To provide feedback for this document, go to surveymonkey.com/s/PQM6P62 or send an email message to
Technical Publications ([email protected]).
a
You can use your smartphone to scan a QR Code, which opens your email application or browser.

Thermo Scientific OptaMax NG Ion Source User Guide xiii


Preface

xiv OptaMax NG Ion Source User Guide Thermo Scientific


1

Introduction
This chapter provides general information about the API techniques (modes) for use with the
OptaMax NG ion source. The ionization mode is the specific process used to ionize the
sample.

The MS keeps the pressure in the API source housing at atmospheric levels, which reduces the
chemical noise that nebulized gases can cause when they are not properly evacuated from the
API source. The MS’s ion guides transmit the ions produced in the API source into the mass
analyzer, where the instrument analyzes them according to their mass-to-charge ratio (m/z).
For information about ion analysis, refer to the MS manuals.
• Preferred Ionization Modes
• H-ESI Mode
• APCI Mode
• APPI Mode

Preferred Ionization Modes


The preferred ionization modes are H-ESI for polar compounds (H-ESI is a type of ESI and
the ionization properties are the same for both), APCI for medium polarity compounds, and
APPI for certain polar and nonpolar compounds.

Thermo Scientific OptaMax NG Ion Source User Guide 1


1 Introduction
H-ESI Mode

Figure 1. Polarity ranges for ESI, APCI, and APPI versus molecular weights
\

100 000
E
S
10 000 I
MW
(Da)
A
1000
P
P A
I P
C
100 I

Nonpolar Polar
Polarity

H-ESI Mode
H-ESI transforms ions in solution into ions in the gas phase by using electrospray ionization
with heated auxiliary gas. An MS with H-ESI can analyze a range of molecular weights greater
than 100 000 Da, due to multiple charging. H-ESI is especially useful for the mass analysis of
polar compounds that make a preformed ion in solution. These compounds include
biological polymers (for example, proteins, peptides, glycoproteins, and nucleotides),
pharmaceuticals and their metabolites, and industrial polymers (for example, polyethylene
glycols).

Droplet size, surface charge, liquid surface tension, solvent volatility, and ion solvation
strength are factors that affect the electrospray process. Large droplets with high surface
tension, low volatility, strong ion solvation, low surface charge, and high conductivity prevent
good electrospray. The electrospray source produces charged aerosol droplets that contain
sample ions. The electrospray source accommodates liquid flow rates of 1 μL/min to
1 mL/min without splitting.

Organic solvents, such as methanol, acetonitrile, and isopropyl alcohol, are superior to water
for H-ESI. Volatile acids and bases are good, but salts above 10 mM concentration and strong
acids and bases are extremely detrimental.

2 OptaMax NG Ion Source User Guide Thermo Scientific


1 Introduction
APCI Mode

Guidelines
These guidelines will help you achieve a strong electrospray.
• Avoid using nonvolatile salts and buffers in the solvent system. For example, avoid the use
of phosphates and salts that contain sodium or potassium. If necessary, use ammonium
salts instead.
• Use organic-aqueous solvent systems.
• Use volatile acids and bases.
• If possible, optimize the pH of the solvent system for the analyte of interest. For example,
if the analyte of interest contains a primary or secondary amine, use an acidic mobile
phase (pH 2–5). The acidic pH tends to keep positive ions in solution.

For LC applications that require nonvolatile buffers, use these guidelines:


• Install the ion sweep cone on the MS.
• Optimize the spray insert position.
• Reduce the concentration of buffers to an absolute minimum.

APCI Mode
Atmospheric pressure chemical ionization (APCI) is a soft ionization technique, but it is not
as soft as H-ESI. APCI is used to analyze compounds of medium polarity that have some
volatility.

Figure 2 shows the APCI process for positive adduct ion formation. In APCI, the MS
produces and analyzes ions as follows:
1. The nozzle sprays the sample solution into a fine mist of droplets.
2. The APCI vaporizer (high temperature tube) vaporizes the droplets.
3. The MS applies a high voltage to a needle located near the exit end of the tube. The high
voltage creates a corona discharge that forms reagent ions through a series of chemical
reactions with solvent molecules and nitrogen sheath gas.
4. The reagent ions react with sample molecules to form sample ions.
5. The sample ions enter the MS and are analyzed.

APCI is a gas phase ionization technique. Therefore, the gas phase acidities and basicities of
the analyte and solvent vapor play an important role in the APCI process.

In the positive-ion mode, sample ionization occurs in a series of reactions that start with the
electron-initiated cation formation. The following are typical examples of primary, secondary,
and adduct ion formation:

Thermo Scientific OptaMax NG Ion Source User Guide 3


1 Introduction
APCI Mode

Primary ion formation e– + N2 → N2+• + 2e–


Secondary ion formation N2+• + H2O → N2 + H2O+•

H2O+• + H2O → H3O+ + HO•


Proton transfer H3O+ + M → (M + H)+ + H2O

In negative ion mode, (M – H)– is typically formed by the abstraction of a proton by OH–.

APCI is typically used to analyze small molecules with molecular weights up to about
1500 Da. A very robust ionization technique, APCI is not affected by minor changes in most
variables, such as changes in buffers or buffer strength.

You can use APCI in positive or negative ion polarity mode. For most molecules, the positive
ion mode produces a stronger ion current. This is especially true for molecules with one or
more basic nitrogen (or other basic) atoms. An exception to the general rule is that molecules
with acidic sites, such as carboxylic acids and acid alcohols, produce more negative ions than
positive ions.

Although, in general, APCI produces fewer negative ions than positive ions, negative ion
polarity is sometimes the mode of choice. Because the negative ion polarity mode sometimes
generates less chemical noise than in the positive mode, selectivity might be better in the
negative ion mode.

4 OptaMax NG Ion Source User Guide Thermo Scientific


1 Introduction
APCI Mode

Figure 2. APCI process in the positive ion polarity mode (cross-sectional components)
(Not to scale)
APCI spray insert inside the
heater assembly

Atmospheric
pressure region

APCI nozzle
Ion transfer tube

Chemical
ionization
M (M+H) +
S SM
SM M S
SMSMSM
SS H O+ HO
3 2

Corona discharge
needle (+3–5 kV)

H 20 H 20+ Corona
discharge
H 20+ region
Corona
H 20+ H 20+ (plasma)
discharge
needle
- N 2+ N 2+
(+3–5 kV) e -
e
+
++ +
++ -
N2+ e- N 2+e

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1 Introduction
APPI Mode

APPI Mode
Atmospheric pressure photoionization is also a soft ionization technique. In APPI an ion is
generated from a molecule when it interacts with a photon from a light source, such as the
Syagen™ PhotoMate™ APPI™ light source. APPI generates molecular ions for molecules that
have an ionization potential below the photon energy of the light being emitted by the light
source.

In APPI, the MS produces and analyzes ions as follows:


1. The H-ESI or APCI nozzle sprays the sample solution into a fine mist of droplets.
2. The vaporizer (high temperature tube) vaporizes the droplets.
3. The analyte molecule interacts with the light from the PhotoMate light source. The
analyte molecule M is ionized to a molecular ion M+ if the ionization potential of the
analyte is less than the photon energy hν:
M + hν → M+ + e–
4. In the presence of protic solvents, the analyte ion may extract a hydrogen to form an
(M + H)+ ion:
M+ + S → (M + H)+ + (S – H)
5. The analyte ions pass through the API ion transfer tube, enter the MS, and are analyzed.

Molecules including steroids, basic-drug entities, and pesticides have ionization potentials
below the threshold, and protonated molecules are generated in the LC/MS experiment. APPI
reduces fragmentation because only a small amount of energy is deposited in the molecule.
Molecules, such as the nitrogen sheath gas, the auxiliary gas, and the simple solvents used for
LC/MS, are not ionized because their ionization potentials are greater than the photon energy.
The result is selective ionization of an analyte versus the background. See Figure 3 and
Figure 4.
Figure 3. Energetics of photoionization

Gases in air,
solvent molecules Fragment ion
thresholds

Molecular ion
thresholds
Energy

Drugs and other


compounds

Photoionization

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1 Introduction
APPI Mode

Figure 4. Selective photoionization

Agricultural
compounds
Drugs MeOH, AcCN
Chlorinated-solvents

Steroids
H2O, CO2, O2, N2

Ionized Not Ionized

Threshold

APPI Light Source


The PhotoMate APPI light source uses a krypton, vacuum ultraviolet (VUV) lamp that emits
photons with energies of 10.0 and 10.6 eV. Molecules with ionization potentials less than
10 eV ionize to form M+ or (M + H)+, while those with greater ionization potentials do not.
Figure 5 shows ionization potentials of typical compounds and solvents.
Figure 5. Ionization potentials of typical compounds and solvents
Krypton 10.0 eV, 10.6 eV

Ionization Potentials (IP) Solvent Ionization Potentials (IP)

Anthracene 7.4 eV Toluene 8.82 eV


Fluoranthene 7.8 eV Acetone 9.70 eV
Caffeine 8.0 eV
4-Nitrotoluene 9.5 eV

10.0 eV
Methanol 10.85 eV
Acetonitrile 12.19 eV
Water 12.61 eV

API Spray Insert Selection


In APPI mode, you can use either the APCI Spray Insert or the H-ESI Spray Insert. You can
do APCI only, APPI only, or APCI/APPI. When you install the H-ESI spray insert, you can
switch between three ionization modes: H-ESI only, APPI only, and H-ESI/APPI.

Select the spray inset that is best suited for your compounds of interest. If the main analysis
mode is APPI, use the APCI spray insert. For additional information, contact Thermo Fisher
Scientific Technical Support (see Contacting Us).

Thermo Scientific OptaMax NG Ion Source User Guide 7


1 Introduction
APPI Mode

8 OptaMax NG Ion Source User Guide Thermo Scientific


2

API Source
This chapter provides general information about the OptaMax NG ion source (Figure 6) and
describes how to remove and install it.
• API Source Features
• Solvent Waste System
• API Spray Inserts
• Removing and Installing the API Spray Insert
• Removing and Installing the API Source

CAUTION To prevent electric shock, verify that the grounding union is made of stainless
steel. A grounding union made of a nonconductive material, such as PEEK, creates an
electric shock hazard.

Figure 6. OptaMax NG ion source

API spray insert depth adjustment

Retainer knobs for API spray insert


and heater assembly
Locking levers (locked position)

Grounding union holder

Side-to-side adjustment knob

Window

Thermo Scientific OptaMax NG Ion Source User Guide 9


2 API Source
API Source Features

API Source Features


The API source includes these features:
• Heater assembly—Mounts on top of the API source housing, and used for H-ESI, APCI,
and APPI modes. In H-ESI mode, the heater heats the auxiliary gas, which aids in
desolvation. In APCI and APPI modes, the heater vaporizes the sample before it reaches
the APCI corona discharge needle (APCI mode) or the PhotoMate light source (APPI
mode). For information about the ionization modes, see Chapter 1, “Introduction.”
• Adjustable API spray insert mount—Moves the API spray insert and heater assembly
front-to-back, or rotates them slightly to increase sensitivity or robustness. You can also
adjust the spray insert depth. See “Adjusting the Direction of the Spray Insert.”
• Mounting angle of the API spray insert—Fixed at the optimum angle for signal intensity
and API source robustness. You can view the spray insert through the API source window
while positioning it.
• Interchangeable ionization modes—You can change the ionization mode by installing a
different spray insert and reconfiguring the housing. See Chapter 3, “Changing the
Ionization Mode.”
• Safety interlock system—Prevents contact with high voltages. The API source housing
• has high-voltage, safety interlock switches that turn off the following voltages:
– Electrospray needle voltage or APCI corona discharge voltage
– All API source and lens voltages, including the ion transfer tube offset voltage
– Voltages on the MS ion guides
The following actions turn off these voltages:
• Removing the API spray insert from the API source
• Removing the API source from the MS
• Internal wiring and gas plumbing—You do not have to remove the LC or gas plumbing
to remove the API source or change the ionization mode.
• Internal drain inserts —There are two internal drain inserts: a taller one for H-ESI and
APCI and a shorter one for APPI. You have no external drain tube to remove when
removing the API source.
• Cooling vents—During operation, the external surface of the API source can become hot.
The ventilation holes in the housing aid cooling. Before you touch the housing or its
components, allow the system to cool for a minimum of 20 minutes.

CAUTION Avoid burns. Avoid touching the API source housing when the mass
spectrometer is in operation. The external surface of the housing can become hot
enough to burn your skin.

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2 API Source
API Source Features

• To prevent corrosion caused by liquid leaks or poor drainage, the API source includes
these features:
– Zero dead volume (ZDV) grounding union—(Required for H-ESI mode only)
Connects the solvent flow from the LC instrument or the syringe pump to the API
spray insert’s sample inlet. The grounding union’s position is offset to prevent liquid
leaks from dripping into the API source housing (Figure 7).
– Drain—Allows eluants to flow directly from the API spray insert into the drain.
(Figure 8).
Figure 7. OptaMax NG ion source showing the H-ESI API spray insert, heater assembly,
and housing
Sample inlet
(H-ESI) spray insert

Heater assembly
Grounding union
holder
Heater/vaporizer
tube not shown

Window

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2 API Source
Solvent Waste System

Figure 8. OptaMax NG ion source (back and top view)


Sample inlet (H-ESI)

Lever for the API High voltage connection (for the


spray insert depth H-ESI spray insert or the APCI
adjustment corona discharge needle)

Connector for heater power and


signal connections (readbacks
and safety interlock)

Sheath gas inlet

Auxiliary gas inlet

H-ESI or APCI
drain insert

Solvent Waste System


Solvent waste from the drain insert in the API source travels through a fully enclosed drain
tube inside the MS and exits the instrument at the left side. Figure 9 shows the solvent waste
system.

IMPORTANT Equip your laboratory with at least two fume exhaust systems. The analyzer
optics can become contaminated if the API source drain tube and the exhaust tubing from
the forepumps connect to the same fume exhaust system. Route the exhaust tubing from
the forepumps to a dedicated fume exhaust system.

For additional information, refer to the MS’s Preinstallation Requirements Guide.

12 OptaMax NG Ion Source User Guide Thermo Scientific


2 API Source
API Spray Inserts

Figure 9. Example solvent waste system

Drain/waste port
(left side)

To external vent
Internal API source API source
drain tube

Tygon™ tubing, 1 in. ID


(at least 1 m [3 ft])
Solvent waste
cap removed

Solvent waste container

API Spray Inserts


This section describes the API spray inserts (Figure 10) that you insert into the heater
assembly through the top of the API source (Figure 7).
Figure 10. H-ESI (top) and APCI (bottom) API spray inserts

H-ESI spray insert

APCI spray insert

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2 API Source
API Spray Inserts

H-ESI Spray Insert


The H-ESI spray insert includes a metal electrospray needle insert, a H-ESI nozzle, and the
sheath gas and auxiliary gas plumbing. Sample and solvent enter the nozzle through one of
two H-ESI needle inserts: one is for low flow (less than 10 μL/min) and the other, for high
flow (greater than 10 μL/min). To change the needle insert, see “Replacing the H-ESI Metal
Needle Insert.”

The H-ESI needle insert includes a stainless steel needle that extends from the sample inlet to
approximately 1.2 mm (0.05 in.) past the end of the spray insert nozzle. Figure 11 shows the
H-ESI needle insert removed from the H-ESI spray insert.
Figure 11. H-ESI spray insert and its metal needle insert

H-ESI needle insert


assembly
H-ESI spray insert
(without the needle insert)

Nozzle

The MS applies a large negative or positive voltage (typically ±3 to ±5 kV) to the metal
electrospray needle, which sprays the sample solution into a fine mist of charged droplets. The
H-ESI spray insert delivers the sheath gas and auxiliary gas to the nozzle. The sheath gas is the
inner coaxial nitrogen gas that sprays (nebulizes) the sample solution into a fine mist as it exits
the electrospray needle (see the light blue lines in Figure 12). The heated auxiliary gas is the
outer coaxial nitrogen gas that assists the sheath gas in the desolvation of sample solutions (see
the green lines in Figure 13).

The auxiliary gas heats as it passes through the heater/vaporizer tube. The heater/vaporizer
tube (Figure 7) is thermally insulated from the metal electrospray needle to prevent direct
heating of the sample solution. You can control the heater/vaporizer temperature from the
Thermo Scientific Tune or Method Editor application. The temperature range is from
ambient room temperature to 550 °C. For the recommended initial operating settings, see
“Setting the Initial Ion Source Parameters.”

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2 API Source
API Spray Inserts

Figure 12. Sheath gas flow (blue lines)

Sheath gas

Electrospray needle

Figure 13. Auxiliary gas flow (green lines)

Heated auxiliary gas

Electrospray needle

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2 API Source
API Spray Inserts

APCI Spray Insert


The APCI spray insert, which is shorter than the H-ESI spray insert, includes a fused-silica
capillary (APCI sample tube) insert, an APCI nozzle, and the sheath gas and auxiliary gas
plumbing. Sample and solvent enter the nozzle through the fused-silica capillary insert. To
change the fused-silica sample tube, see “Replacing the APCI Fused-Silica Sample Tube.”

The APCI fused-silica insert is a short section of 0.15 mm (0.59 in.) ID fused-silica tubing
that extends from the sample inlet to 1 mm (0.04 in.) past the end of the spray insert nozzle.
Figure 14 shows the APCI needle insert removed from the APCI spray insert.
Figure 14. APCI spray insert and its fused-silica needle insert

APCI needle insert


assembly
APCI spray insert (without
the needle insert)

Nozzle

The APCI spray insert sprays the sample solution into a fine mist that enters the APCI
vaporizer tube, which is ceramic and heated by the heater assembly. The vaporizer tube
vaporizes the mist droplets at temperatures up to 550 °C (typically 350–450 °C for flow rates
of 0.1–2 mL/min). The APCI spray insert delivers the sheath gas and auxiliary gas to the
nozzle. The flow of the nitrogen sheath and auxiliary gases pushes the sample vapor toward
the corona discharge needle.

During APCI operation, the tip of the corona discharge needle, which is mounted inside the
API source housing, is positioned near the vaporizer. The mass spectrometer applies a high
APCI corona discharge voltage (typically ±3 to ±5 kV) to the corona discharge needle to
produce a steady APCI corona discharge current of up to 100 μA (typically 5 μA). The corona
discharge from the needle produces chemical ionization (CI) plasma primarily from the
solvent vapor. Ion molecule reactions with the reagent ions in the plasma ionize the sample
vapor.

The APCI source can accommodate liquid flows of 100 μL/min to 2 mL/min without
splitting the flow from the LC.

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2 API Source
Removing and Installing the API Spray Insert

Removing and Installing the API Spray Insert


Use the following procedures when you want to change the ionization configuration (mode)
of the API source or perform the maintenance tasks in Chapter 4, “Maintenance.”

 To remove the API spray insert

1. Complete all data acquisition, if any.


2. Place the MS in Off mode as follows:
a. From the Windows taskbar, open the Tune application:
• (Windows 7) From the Microsoft™ Windows™ taskbar, choose Start > All Programs
> Thermo Instruments > model x.x > model Tune, where model is your specific MS.
• (Windows 10) From the Windows taskbar, choose Start > All Apps> Thermo
Instruments > model x.x, model Tune, where model is your specific MS.
b. Click the Off icon,
The center of the selected icon changes from white to green. You can leave the power
on for the MS, the LC components, and the data system.

CAUTION Hot surface. Accidental contact with the part of the API spray insert
located inside the housing can severely burn you, as this area of the insert can reach
350 °C (662 °F). In addition, although the housing’s exterior surface and the exposed
part of the spray insert fall below the limit of 70 °C (158 °F) for accessible metal
surfaces, they too pose a burn hazard. Before removing the API spray insert or
housing, allow the part to cool to room temperature (approximately 20 minutes)
before you touch it.

If the MS connects to an LC system, leave the solvent flow from the LC pump on
while the API spray insert cools to room temperature. Then turn off the solvent flow
to the API source.

3. Disconnect the sample line from the spray insert’s sample inlet (Figure 7).
4. After the spray insert cools to room temperature, loosen the spray insert nut (Figure 15).
5. Lift up and remove the spray insert from the heater assembly.

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2 API Source
Removing and Installing the API Source

 To install the API spray insert

1. Align the guide pin on the API spray insert with the guide pin slot in the heater assembly
(Figure 15).
Figure 15. Guide pin and guide pin slot locations

API spray insert nut

Guide pin

Guide pin slot

Heater assembly on the API source housing

2. Slowly place the spray insert into the heater assembly on the source.
3. With your hand, tighten the spray insert nut.

Removing and Installing the API Source


This section describes how to remove and install the OptaMax NG ion source. If any other
source is installed, refer to its documentation for how to remove it from the MS after it has
cooled to room temperature.
• Removing the API Source from the Mass Spectrometer
• Installing the API Source onto the Mass Spectrometer

Removing the API Source from the Mass Spectrometer


You must remove the API source to access the mass spectrometer’s ion sweep cone, ion
transfer tube, and ion source interface, and to access the APCI corona discharge needle and
the optional APPI lamp inside the API source housing. Always place the MS in off mode
before you remove any components. When the instrument is in standby mode, the API gases,
the high voltage, and the syringe pump are off.

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2 API Source
Removing and Installing the API Source

 To remove the API source

1. Place the MS in Off mode (see page 17).


2. Disconnect the sample line from the grounding union (H-ESI mode) or the spray insert’s
sample inlet (APCI or APPI mode). See Figure 25.
3. Rotate the locking levers to the unlocked position (Figure 16).
Figure 16. OptaMax NG ion source with unlocked levers (front view)

Locking lever (unlocked)

4. Grasp the source housing with both hands and slowly pull it away from the MS.

Note If you plan to store the API source, rotate the locking levers to the locked position.

Installing the API Source onto the Mass Spectrometer


Before installing the API source, you must prepare the MS.

 To prepare the mass spectrometer

1. If a different API source is installed, remove it from the MS after it has cooled to room
temperature.
2. While wearing a new pair of lint- and powder-free gloves, make sure that the ion sweep
cone is installed over the spray cone (Figure 17).

Thermo Scientific OptaMax NG Ion Source User Guide 19


2 API Source
Removing and Installing the API Source

Figure 17. Mass spectrometer mount assembly with ion sweep cone

Spray cone

Ion sweep cone

Guide pins on the MS

 To install the API source

1. Follow the procedure “To prepare the mass spectrometer.”


2. Make sure that the locking levers are in the unlocked position (Figure 16).
3. Align the two guide pin holes on the back of the source (Figure 18) with the guide pins
on the front of the MS (Figure 17).

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2 API Source
Removing and Installing the API Source

Figure 18. OptaMax NG ion source with unlocked levers (back view)

Locking lever (unlocked)

Guide holes on the back


of the housing

4. Carefully press the source onto the MS.


5. Lock the locking levers.
6. Reconnect the sample line to the grounding union (H-ESI mode) or the spray insert’s
sample inlet (APCI and APPI modes).

Thermo Scientific OptaMax NG Ion Source User Guide 21


2 API Source
Removing and Installing the API Source

22 OptaMax NG Ion Source User Guide Thermo Scientific


3

Changing the Ionization Mode


This chapter describes how to identify the current ionization configuration (mode) for the
API source and how to reconfigure it between H-ESI, APCI, and APPI combination modes.
• Identifying the Ionization Configuration
• Changing the Ionization Configuration
• Setting the Initial Ion Source Parameters
• Adjusting the Direction of the Spray Insert

Thermo Scientific OptaMax NG Ion Source User Guide 23


3 Changing the Ionization Mode
Identifying the Ionization Configuration

Identifying the Ionization Configuration


To identify the current ionization configuration, compare your API source housing to the
images shown in Table 2. These images show the API source housing configured for H-ESI
and APCI modes; and H-ESI, APCI, and APPI combination modes.
Table 2. Images showing the possible API source housing configurations
API source housing image Possible ionization modes

H-ESI or APCI modes

Shows the APCI corona needle assembly on the right


side of the API source housing with the APCI spray
insert.

You can replace the APCI spray insert with the


H-ESI spray insert.

APCI components

APPI/H-ESI combination mode

–or–

APPI/APCI combination mode

Shows the API source housing configured for APPI


(left side).

Depending on the intended combination mode,


install either spray insert (H-ESI or APCI) into the
housing.
APPI components

24 OptaMax NG Ion Source User Guide Thermo Scientific


3 Changing the Ionization Mode
Changing the Ionization Configuration

Changing the Ionization Configuration


The procedures in Table 3 show you how to configure the API source housing between
H-ESI, APCI, and APPI combination modes. Before you continue, make sure you know the
current ionization configuration (mode) for the API source housing (see Table 2).

CAUTION Handle the APCI corona discharge needle with care. The corona discharge
needle is very sharp and can puncture your skin.

CAUTION Hot surface. Avoid touching the API source housing or the API spray insert
when the MS is in operation. These components can become hot enough to burn your
skin. Allow the components to cool (minimum 20 minutes) before you touch them.

Table 3. Summary procedures for configuring the API source housing (Sheet 1 of 3)
Current mode New mode Procedure
H-ESI APCI 1. Remove the H-ESI spray insert (see page 17), and place it in a safe place.
2. Install the APCI spray insert (see page 18) and the LC plumbing.
3. Follow the procedure “Setting the Initial Ion Source Parameters.”
APPI 1. Remove the H-ESI spray insert (see page 17), and place it in a safe place.
2. If the API source is not already configured for APPI, do the following:
a. Remove the API source from the MS (see page 19).
b. Configure the API source for APPI mode (see page 29).
c. Install the API source onto the MS (see page 20).
3. Install the H-ESI spray insert (see page 18) and the LC plumbing. For
guidelines, see “API Spray Insert Selection.”
4. Turn on the left-side power switch for the APPI (VUV) lamp.
5. Follow the procedure “Setting the Initial Ion Source Parameters.”

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3 Changing the Ionization Mode
Changing the Ionization Configuration

Table 3. Summary procedures for configuring the API source housing (Sheet 2 of 3)
Current mode New mode Procedure
APCI H-ESI 1. Remove the APCI spray insert (see page 17), and place it in a safe place.
2. Do one of the following:
• Place the corona discharge needle in the (0) position away from the
spray insert (see page 28).
• Remove the corona discharge needle (see page 28), and then install the
API source onto the MS (see page 20).
3. If it is not already installed, install the grounding union and its holder onto
the API source (Figure 25).
4. Install the H-ESI spray insert (see page 18) and the LC plumbing.
5. Follow the procedure “Setting the Initial Ion Source Parameters.”
APPI 1. Remove the APCI spray insert (see page 17), and place it in a safe place.
2. If the API source is not already configured for APPI, do the following:
a. Remove the API source from the MS (see page 19).
b. Configure the API source for APPI mode (see page 29).
3. Do one of the following:
• Place the corona discharge needle in the (0) position away from the
spray insert (see page 28).
• Remove the corona discharge needle (see page 28).
4. If you removed the API source, install it onto the MS (see page 20).
5. Install the APCI spray insert (see page 18) and the LC plumbing.
For guidelines, see “API Spray Insert Selection.”
6. Turn on the left-side power switch for the APPI (VUV) lamp.
7. Follow the procedure “Setting the Initial Ion Source Parameters.”
Note The APCI needle can remain in the housing when the system operates in H-ESI or APPI mode.

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3 Changing the Ionization Mode
Changing the Ionization Configuration

Table 3. Summary procedures for configuring the API source housing (Sheet 3 of 3)
Current mode New mode Procedure
APPI H-ESI 1. If the APCI spray insert is installed, remove it (see page 17) and place it in a
safe place.
2. If it is not already done, install the grounding union and its holder onto the
ion source (Figure 25).
3. (Optional) Reinstall the APPI lamp cover.
4. Install the H-ESI spray insert (see page 18) and the LC plumbing.
5. Follow the procedure “Setting the Initial Ion Source Parameters.”
APCI 1. If the H-ESI spray insert is installed, remove it (see page 17) and place it in a
safe place.
2. (Optional) Reinstall the APPI lamp cover.
3. Install the APCI spray insert (see page 18) and the LC plumbing.
4. Follow the procedure “Setting the Initial Ion Source Parameters.”
Note The APPI components can remain in the housing when the system operates in H-ESI or APCI mode.

If you configure the API source housing for all three ionization modes (see the second image
in Table 2), set the APCI corona discharge needle and the PhotoMate APPI light source as
listed in Table 4.
Table 4. Light source and corona discharge needle settings for the ionization modes
Ionization mode Corona discharge needle PhotoMate light source
H-ESI
APCI On
APPI On
Combined H-ESI/APPI On
Combined APCI/APPI On On

Changing the Position of the APCI Corona Discharge Needle


Use the following procedure when you want to use the corona discharge needle (On position)
or move it out of the way of the API spray insert (Off position).

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3 Changing the Ionization Mode
Changing the Ionization Configuration

 To change the position of the corona discharge needle

Do the following to adjust the corona discharge needle position (Figure 19):
• To use the needle (APCI mode), turn the right-side knob to the On position.
• To not use the needle and move it away from the API spray insert (H-ESI and APPI
modes), turn the right-side knob to the position.
Figure 19. Corona discharge needle adapter showing the On and knob positions

Needle On position Needle position

Removing the APCI Corona Discharge Needle


If you do not plan to use APCI mode for a while, you can remove the corona discharge
needle.

 To remove the corona discharge needle

1. Remove the API source from the MS (see page 19).


2. Put on a new pair of lint- and powder-free gloves.
3. Using the pliers, grasp the base of the corona discharge needle and slowly pull it straight
out of the socket (Figure 20).

CAUTION To prevent damage to the corona needle tip, avoid touching it with the
pliers.

CAUTION Sharp object. The corona discharge needle can puncture your skin.
Handle it with care.

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3 Changing the Ionization Mode
Changing the Ionization Configuration

Figure 20. Corona discharge needle (close-up view)

Needle base

4. Rinse the needle with solvents compatible with your compounds, and then store the
needle in a safe place.

Configuring the API Source Housing for APPI Mode


Use the following procedures to install the left-side APPI components (see APPI Parts).
1. To remove the left-side H-ESI components from the API source
2. To install the APPI installation kit

Note If you already installed the left-side APPI components, you only need to install the
APPI drain insert and one of the spray inserts. For guidelines, see “API Spray Insert
Selection.”

 To remove the left-side H-ESI components from the API source

1. Put on a new pair of lint- and powder-free gloves.


2. After the API source cools to room temperature, remove it from the MS (see page 19).
3. Remove the H-ESI spray insert (see page 17). If you installed the APCI components,
place the corona discharge needle in the (0) position.
4. Using the 2 mm hex key and the Phillips #2 screwdriver, remove from the source the
left-side H-ESI cover and the APPI lamp cover (Figure 21).
You might need to use one of your gloved hands to push the APPI lamp cover out of the
housing.

CAUTION Sharp object. An installed APCI corona discharge needle can puncture
your skin. Be careful when you place your fingers inside the API source housing.

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3 Changing the Ionization Mode
Changing the Ionization Configuration

Figure 21. API source showing the left-side H-ESI components (exploded view)

H-ESI/APCI drain
Pin insert

H-ESI cover

APPI lamp port

APPI lamp cover

 To install the APPI installation kit

1. Follow the procedure “To remove the left-side H-ESI components from the API source.”
2. Remove the H-ESI/APCI drain insert, rinse it with methanol, and store it in a safe place.
3. Align the APPI drain insert alignment pin with the slot for the alignment pin on the
housing, and then carefully insert the drain insert into the housing.
4. Using the screwdriver, secure the APPI source cover onto the left side (Figure 22).

30 OptaMax NG Ion Source User Guide Thermo Scientific


3 Changing the Ionization Mode
Changing the Ionization Configuration

Figure 22. API source showing the left-side APPI components (exploded view)

APPI drain insert APPI source cover

Pin

PhotoMate APPI light source APPI lamp port

5. Using the 2 mm hex key, secure the APPI light source into the left-side APPI lamp port.

CAUTION To prevent damage to the APPI lamp, make sure that it does not touch the
APCI corona discharge needle (if installed).

6. Install either the H-ESI or APCI spray insert (see page 18).
For guidelines, see “API Spray Insert Selection.” Figure 23 shows the completed API
source housing for APPI mode.

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3 Changing the Ionization Mode
Changing the Ionization Configuration

Figure 23. Left side of the assembled APPI source with the APCI spray insert

APCI spray insert

Power switch for the APPI lamp

Thumbscrew for adjusting the APPI lamp depth

Fan and fan filter

7. Connect the APPI power supply unit as follows:


a. If it is not already connected, connect the detachable power supply cord to the power
supply unit, and then plug the power cord into a wall outlet.
b. Connect the DB15 plug to the top of the APPI light source. Figure 24 shows the
correct power connection on an older model ion source.
The DB15 plug is connected to a Y-cable. One side of the Y-cable connects to the
power supply unit and the other side connects to a USB port on the MS.
Figure 24. Power connection to the APPI light source

The DB15 plug provides


power to the APPI light
source assembly.

APPI lamp and shield

Remote LED

c. Connect the USB cable to an open USB port on the mass spectrometer, not to the
data acquisition computer. If both ports are occupied, install the provided USB
splitter into either USB port.

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3 Changing the Ionization Mode
Changing the Ionization Configuration

The USB ports are on the right side of the mass spectrometer. The Remote LED on
the APPI light source indicates that the USB connection is on.

Note For troubleshooting purposes, you might want to record which devices
connect to which USB ports on the mass spectrometer.

CAUTION After completing the power supply connections, route the cords so
that they are not a trip hazard.

8. Using your fingers, turn the thumbscrew (Figure 23) on the APPI light source clockwise
until it is fingertight (the default lamp depth position).
The thumbscrew controls the APPI lamp’s depth position inside the API source housing.
9. Place the power switch for the APPI lamp in the On (|) position.

You can now install the API source onto the mass spectrometer and connect the LC
plumbing.

Configuring the API Source Housing for H-ESI Mode


Use the following procedure to configure the API source for H-ESI mode.

Note If you did not install the APPI installation kit (see Identifying the Ionization
Configuration), you do not need to make any changes to the API source housing. If you
installed the APPI installation kit, you do not need to remove the housing components
from the API source.

 To configure the API source for H-ESI mode

• If you did not install the APPI installation kit, do the following:
– Make sure that the H-ESI spray insert is installed (Figure 10).
– Place the APCI corona needle in the (0) position (see page 27).
• If you installed the APPI installation kit, do the following:
a. Place the power switch for the APPI light source in the (0) position.
b. Disconnect the APPI power supply unit’s input and output cords.
c. Make sure that the H-ESI spray insert is installed (Figure 10).
d. After the API source cools to room temperature (allow 20 minutes), remove it from
the mass spectrometer (see page 19).
e. Remove the APPI drain insert, and then install the H-ESI/APCI drain insert
(Figure 22).
f. Install the APPI lamp cover.

Thermo Scientific OptaMax NG Ion Source User Guide 33


3 Changing the Ionization Mode
Changing the Ionization Configuration

g. Store the APPI power supply unit and APPI drain insert in a safe place.
h. If it is not already installed, install the H-ESI grounding union (Figure 25).

You can now install the API source onto the mass spectrometer and connect the LC
plumbing.

Installing the H-ESI Grounding Union onto the API Source


CAUTION Avoid operating the API source in H-ESI mode at elevated temperatures
without solvent flow. Running the source dry at elevated temperatures can cause blockage
of the replaceable metal needle.

Install the stainless steel grounding union (P/N 00101-1812) in the LC liquid flow path when
you want to use the API source for H-ESI mode. You can optionally leave this plumbing
installed when you use APCI mode; the plumbing path is not used for APCI mode. Refer to
the mass spectrometer manual for how to install the grounding union, its holder, and the
sample line (Figure 25).

CAUTION To prevent electric shock, verify that the grounding union is made of stainless
steel. A grounding union made of a nonconductive material, such as PEEK, creates an
electric shock hazard.

Figure 25. Installed H-ESI grounding union and sample line (example)

High flow needle: Viper™ capillary 0.13 mm


ID, 15 cm long
Low flow needle: nanoViper™ capillary 50 μm
ID, 15 cm long
H-ESI spray insert
sample inlet

Sample input
Grounding union installed in the
grounding union holder (bar)

34 OptaMax NG Ion Source User Guide Thermo Scientific


3 Changing the Ionization Mode
Setting the Initial Ion Source Parameters

Setting the Initial Ion Source Parameters


After you install the configured source, use the Tune application to set the initial ion source
parameters for the experiment’s LC flow rate. For example, the ion source parameters for
H-ESI mode include the spray voltage, the three API gas pressures, the ion transfer tube
temperature, and the vaporizer temperature. For the auxiliary gas flow with vaporizer
temperatures up to 100 °C, the allowable range is 0–25 units. For vaporizer temperatures
above 100 °C, the minimum is 5 units (recommended).

The initial settings provide a starting point for optimizing system performance. The optimal
settings for your experiment depend on the compound of interest, the solvent matrix, and the
chromatographic conditions. For information on how to optimize the ion source settings,
refer to the Hardware Manual.

CAUTION For best results in H-ESI mode, avoid operating the API source at elevated
temperatures without solvent flow from the LC system or the syringe pump. Allowing the
API spray insert to run dry at elevated temperatures can cause blockage of the replaceable
metal needle, which you would then need to replace.

 To set the initial ion source parameters

1. Open the Tune application, and then open the Ion Source pane.
2. In the Current LC Flow (μL/min) box, enter a value for the experiment.
3. Click Get Defaults, and then click Apply.
The Tune application sets the default parameters for the H-ESI, APCI, or APPI source.

 To optimize the API source parameters

For instructions on how to optimize the spray voltage, the API gas pressures, and the
discharge current (APCI only), refer to the Hardware Manual.

Adjusting the Direction of the Spray Insert


To maximize sensitivity or robustness, you can adjust the direction of the spray inlet by a few
millimeters. Typically, you adjust the direction of the spray insert while optimizing the API
source parameters for the analytes.
Note The angle of the API spray insert and heater assembly is not adjustable.

Thermo Scientific OptaMax NG Ion Source User Guide 35


3 Changing the Ionization Mode
Adjusting the Direction of the Spray Insert

 To adjust the front-to-back position of the spray insert

CAUTION Hot surface. Avoid touching the API source housing when the mass
spectrometer is in operation. The external surface of the housing can become hot
enough to burn your skin. Allow the housing to cool for 20 minutes before you touch
it.

1. Loosen the top two retainer knobs that secure the spray insert. Figure 26 shows one of the
knobs.
2. Slide the spray insert forward or backward to the appropriate position: 1, 2, or 3.
Figure 26. Front-to-back adjustment of the spray insert

Retainer knob for


the API spray insert
Front-to-back
position indicator

36 OptaMax NG Ion Source User Guide Thermo Scientific


3 Changing the Ionization Mode
Adjusting the Direction of the Spray Insert

 To adjust the side-to-side position of the spray insert

Turn the side-to-side adjustment knob to the appropriate position indicator Figure 27.
Figure 27. Side-to-side adjustment

Side-to-side position
indicator

Side-to-side adjustment knob

 To adjust the depth position of the spray insert

1. Loosen the thumb screw on the depth adjustment lever (Figure 28).
2. Move the lever to the appropriate depth position: low, low-medium, or medium.
3. Tighten the thumbscrew.
Figure 28. Depth adjustment

Medium depth
Low-medium depth
Low depth

Thumbscrew for depth


adjustment lever

4. Tighten the top two retainer knobs by hand (Figure 6).

Thermo Scientific OptaMax NG Ion Source User Guide 37


3 Changing the Ionization Mode
Adjusting the Direction of the Spray Insert

38 OptaMax NG Ion Source User Guide Thermo Scientific


4

Maintenance
This chapter provides routine maintenance procedures that you must perform to ensure
optimum performance of the OptaMax NG ion source. For a list of replaceable parts, see
Chapter 5, “Replaceable Parts.”
• Maintenance Schedule
• Tools and Supplies
• Preparation
• Flushing the Inlet Components
• Maintaining the API Spray Insert
• Maintaining the PhotoMate APPI Light Source
• Maintaining the API Source Housing

Maintenance Schedule
Table 5 list the recommended frequency for maintenance procedures.
Table 5. API source maintenance procedures and frequency
Recommended frequency Procedure Location
Daily (end of the work day) Flush (clean) the sample transfer line, sample page 41
tube, and API spray insert.
Clean the APPI lamp window. page 48
As needed Replace the H-ESI metal needle insert. page 43
Replace the APCI fused-silica sample tube. page 44
Replace the APPI lamp. page 50
Clean the APPI fan filter. page 50
Clean the API source housing. page 51

Thermo Scientific OptaMax NG Ion Source User Guide 39


4 Maintenance
Tools and Supplies

Tools and Supplies


The API source requires few tools to perform routine maintenance procedures. Table 6 lists
the tools and supplies for maintaining the ion source.

CAUTION Avoid exposure to potentially harmful materials.

By law, producers and suppliers of chemical compounds are required to provide their
customers with the most current health and safety information in the form of Material
Safety Data Sheets (MSDSs) or Safety Data Sheets (SDSs). The MSDSs and SDSs must
be freely available to lab personnel to examine at any time. These data sheets describe the
chemicals and summarize information on the hazard and toxicity of specific chemical
compounds. They also provide information on the proper handling of compounds, first
aid for accidental exposure, and procedures to remedy spills or leaks.

Read the MSDS or SDS for each chemical you use. Store and handle all chemicals in
accordance with standard safety procedures. Always wear protective gloves and safety
glasses when you use solvents or corrosives. Also, contain waste streams, use proper
ventilation, and dispose of all laboratory reagents according to the directions in the MSDS
or SDS.

Table 6. Chemicals, equipment, and tools (Sheet 1 of 2)


Item Part number
Chemicals
Detergent (for example, Liquinox™) (Liquinox) Fisher Scientific:
• 16-000-125 (1 quart)
• 16-000-128 (1 gallon)
Isopropyl alcohol Fisher Scientific A459-1
Methanol, LC/MS-grade Fisher Scientific A456-1
Nitrogen gas, clean and dry –
Water, LC/MS-grade Fisher Scientific W6-1
Equipment and tools
Cotton-tipped swabs, lint-free Fisher Scientific NC9954124
Kimwipes S47299
Fused-silica cutting toola Fisher Scientific NC9003245
Gloves, lint-free and powder-free –
b
Needle Adjustment Tool Thermo Fisher Scientific:
80000-20957
Magnification device –

40 OptaMax NG Ion Source User Guide Thermo Scientific


4 Maintenance
Preparation

Table 6. Chemicals, equipment, and tools (Sheet 2 of 2)


Item Part number
Screwdriver, Phillips #2 –
Wrench, 3/8 and 3/16 in. –
a Provided in the installation kit
b Provided in the installation kit

Preparation
Before you perform the procedures in this chapter, do the following:
• Place the necessary tools, supplies, and replacement parts (when applicable) nearby.
• Place the components on a clean, lint-free work surface.
• Wear a new pair of lint- and powder-free gloves when handling internal components.
Never reuse gloves after you remove them because the surface contaminants on them
recontaminate clean parts.

Flushing the Inlet Components


At the end of each work day (or more often if you suspect contamination) flush the inlet
components (sample transfer line, sample tube, and API spray insert) with a 50:50
methanol/water solution from the LC system through the API source to remove
contamination.

Tip You do not need to flush the inlet components daily. However, if a mass spectrum
shows unwanted contamination peaks, flush the inlet components.

CAUTION When the ion transfer tube is installed, do not flush it with cleaning solution,
which flushes the residue into the MS.

 To flush the inlet components

1. Complete all data acquisition, if any.


2. Open the Tune application, and then place the mass spectrometer in the On mode.
The center of the selected icon changes from white to green, .
3. Open the Ion Source page in the Ion Source pane, and set the parameters listed in Table 7
based on the API source housing’s configured mode (see the images in Table 2 on
page 24).

Thermo Scientific OptaMax NG Ion Source User Guide 41


4 Maintenance
Maintaining the API Spray Insert

4. Set up and start a flow of 50:50 methanol/water solution at 200 μL/min from the LC to
the API source.

Note For the flushing solution, use a solvent bottle without buffers.

Table 7. Ion source parameters for flushing the inlet components


Parameter H-ESI mode APCI or APPI mode
Spray Voltage (V) 0 0
Sheath Gas (Arbitrary) 30 30
Auxiliary Gas (Arbitrary) 5 5
Capillary Heater (°C) 350 350
Vaporizer Temperature (°C) 400 450

5. Click Apply.
6. Flush the solution through the inlet components for 15 minutes. Then, turn the liquid
flow from the LC.
7. Place the mass spectrometer in Standby mode, .
The API source turns.

Maintaining the API Spray Insert


The H-ESI and APCI spray inserts require minimum maintenance.
• Replacing the H-ESI Metal Needle Insert
• Replacing the APCI Fused-Silica Sample Tube

CAUTION Hot surface. Accidental contact with the part of the API spray insert located
inside the housing can severely burn you, as this area of the insert can reach 350 °C
(662 °F). In addition, although the housing’s exterior surface and the exposed part of the
spray insert fall below the limit of 70 °C (158 °F) for accessible metal surfaces, they too
pose a burn hazard. Therefore, handle ALL heated components with extreme caution.

42 OptaMax NG Ion Source User Guide Thermo Scientific


4 Maintenance
Maintaining the API Spray Insert

Replacing the H-ESI Metal Needle Insert


If the H-ESI metal needle (sample tube) in the H-ESI spray insert becomes plugged, you must
replace it. Replacing the metal needle requires that you partially disassemble the spray insert.
.

IMPORTANT For best results, wear clean gloves when you handle API spray insert
components.

 To review the animation “H-ESI Needle Replacement” for your MS

1. Go to thermofisher.com.
2. In the search field enter either TSQ Altis, TSQ Quantis, or TSQ Fortis.
3. In the Catalog tab click on the instrument name.
4. Scroll down until you see the Product overview, Videos, and Documents tab.
5. Click Videos and select “H-ESI Needle Replacement.”

Follow these procedures:


1. To remove the needle insert from the H-ESI spray insert
2. To install the new needle insert into the H-ESI spray insert

 To remove the needle insert from the H-ESI spray insert

CAUTION Before you begin, place the mass spectrometer in Standby mode (see
page 17).

1. If your LC/MS system includes an LC pump, turn the liquid flow to the API source.
2. After the API source cools to room temperature, remove the spray insert (see page 17).
3. Remove the needle insert from the spray insert as follows:
a. With one hand, twist the locking nut (Figure 29).
b. Pull the collar with the pins straight out of the spray insert.

Thermo Scientific OptaMax NG Ion Source User Guide 43


4 Maintenance
Maintaining the API Spray Insert

Figure 29. Needle insert removed from the H-ESI spray insert

Locking nut Collar with pins Needle insert

c. Using the 3/8 in. wrench or your other hand, loosen the square nut of the needle
insert.
d. Slowly pull the needle insert out of the spray insert.

 To install the new needle insert into the H-ESI spray insert

1. Place the needle into the H-ESI spray probe.


2. Rotate the square PEEK ferrule about four turns to secure the needle insert in the spray
insert.
3. Insert the spray insert into the needle adjustment tool (Figure 30) and make sure the
spray insert is seated firmly.
Figure 30. Installing the needle insert into the H-ESI spray insert

Square PEEK H-ESI spray Needle


ferrule probe

4. Rotate the square ferrule clockwise until you can see the needle extend from the tool.

44 OptaMax NG Ion Source User Guide Thermo Scientific


4 Maintenance
Maintaining the API Spray Insert

5. Slowly rotate the square ferrule counterclockwise until the spray needle is flush with the
tool.
6. Continue to rotate the square ferrule counterclockwise until the square nut is aligned with
the square housing. The needle protrudes within the 1.2 to 1.5 mm specification.
7. Place the collar with pins over the spray insert.
8. Screw the locking nut over the spray insert.
9. Place the spray insert into the source housing and connect it.

Thermo Scientific OptaMax NG Ion Source User Guide 45


4 Maintenance
Maintaining the API Spray Insert

Replacing the APCI Fused-Silica Sample Tube


If the fused-silica sample tube (capillary) in the APCI spray insert becomes plugged, you must
replace it. Replacing the sample tube requires that you partially disassemble the spray insert
and then the fused-silica insert.

IMPORTANT For best results, wear clean gloves when you handle the API spray insert
components.

Follow these procedures:


1. To remove the fused-silica insert from the APCI spray insert
2. To remove the fused-silica tubing from the fused-silica insert assembly
3. To install the new fused-silica tubing into the insert assembly
4. To install the fused-silica insert into the APCI spray insert

 To remove the fused-silica insert from the APCI spray insert

1. Place the mass spectrometer in Off mode (see page 17).


2. If your LC/MS system includes an LC pump, turn the liquid flow to the API source.
3. After the API source cools to room temperature, remove the spray insert (see page 17).
4. Remove the fused-silica insert from the spray insert as follows:
a. With one hand, grasp the spray insert nut (Figure 31).
Figure 31. Removing the fused-silica insert from the APCI spray insert
Spray insert nut

Guide nut

Nozzle union
3/8-in.

b. Using the 3/8 in. wrench or your other hand, loosen the nozzle union.
c. Slowly pull the fused-silica insert out of the spray insert.

46 OptaMax NG Ion Source User Guide Thermo Scientific


4 Maintenance
Maintaining the API Spray Insert

 To remove the fused-silica tubing from the fused-silica insert assembly

1. Using the 3/8 in. and 3/16 in. wrenches, loosen and remove the nozzle union from the
PEEK guide nut (Figure 32).
Figure 32. APCI fused-silica insert assembly (exploded view)

Nozzle union

Fused-silica tubing PEEK guide nut PEEK ferrule Viton™ O-ring

2. Remove the PEEK ferrule from inside the nozzle union.


3. Slide the ferrule and guide nut of the fused-silica tubing, and then discard the tubing.

 To install the new fused-silica tubing into the insert assembly

1. If necessary, replace the nozzle union’s Viton O-ring (Figure 32).


2. Using the fused-silica cutting tool, cut an approximate 13 cm (5 in.) length of fused-silica
tubing, and then under magnification check that the end is squarely cut.
3. Connect the fused-silica tubing to the nozzle union as follows:
a. Slide the guide nut and the ferrule onto the tubing (Figure 32).
b. While you press the tubing into the externally threaded end of the APCI nozzle
union, tighten the guide nut until the tubing is secure.

 To install the fused-silica insert into the APCI spray insert

1. Carefully insert the free end of the fused-silica tubing into the top of the spray insert and
out of the nozzle tip. Then, fingertighten the APCI nozzle union.
2. Using the 3/8 in. wrench, tighten the nozzle union an additional quarter turn.
3. Using the fused-silica cutting tool, cut the tubing so that approximately 1 mm (0.04 in.)
protrudes past the nozzle tip (Figure 33).
4. Reinstall the APCI spray insert into the API source.

Thermo Scientific OptaMax NG Ion Source User Guide 47


4 Maintenance
Maintaining the PhotoMate APPI Light Source

Figure 33. Exit end of the fused-silica tubing protrudes 1 mm (0.04 in.)
Nozzle union

1 mm (0.04 in.)

APCI nozzle tip

Maintaining the PhotoMate APPI Light Source


When you flush the mass spectrometer’s inlet components at the end of the day, you also clean
the APPI lamp window. Any time you notice a weak ion signal in APPI mode, you might
want to clean or polish the APPI lamp window (Figure 34).
Figure 34. PhotoMate APPI light source

Power switch

USB status LED VUV lamp and window

Lamp shield

Fan and filter

Maintenance for the APPI Lamp


This section describes how to clean and polish the APPI lamp window (the glass piece secured
to the end of the lamp), and how to replace a damaged lamp.
• To prepare the API source
• To clean the APPI lamp window
• To remove the APPI lamp and polish the window
• To replace the APPI lamp

48 OptaMax NG Ion Source User Guide Thermo Scientific


4 Maintenance
Maintaining the PhotoMate APPI Light Source

CAUTION Minimize the chance of breaking the APPI lamp by doing the following:
• Always wear clean gloves when you handle the lamp. Fingerprints on the lamp can
cause it to fail when in use.
• Do not spray solvent on the lamp while it is hot, as the lamp can crack.
• Never turn the power to the PhotoMate light source while the vaporizer is hot.
Without power, the fan stops running and the vaporizer heat can damage the light
source’s internal printed circuit board (PCB).
• Do not leave the LC or other liquid delivery device on while the mass spectrometer is
in standby mode or off. The absence of sheath and auxiliary gas can cause the hot
lamp to break upon contact with liquids.

 To prepare the API source

1. If your LC/MS system includes an LC pump, turn the liquid flow to the source.
2. Place the mass spectrometer in Off mode (see page 17).
3. Make sure that the APPI lamp and shield are at room temperature.

CAUTION Hot surface. The vaporizer heater can reach temperatures of 500 °C
(923 °F). Allow the vaporizer and APPI lamp/shield to cool to room temperature
(approximately 30 minutes) before you touch them.

4. Configure the API source as follows:


a. Place the APPI power switch (Figure 34) in the position, and then disconnect the
DB15 plug (Figure 24) from the APPI light source.
b. If you installed the APCI components, place the corona discharge needle in the (0)
position.
5. Remove the API source from the mass spectrometer (see page 19).

 To clean the APPI lamp window

1. Follow the procedure “To prepare the API source.”


2. Put on a clean pair of lint- and powder-free gloves.
3. Soak a lint-free swab in the LC solvent, and then carefully wash the lamp window.

If you were unable to remove all material from the lamp window, follow the procedure “To
remove the APPI lamp and polish the window.”

Thermo Scientific OptaMax NG Ion Source User Guide 49


4 Maintenance
Maintaining the PhotoMate APPI Light Source

 To remove the APPI lamp and polish the window

1. While wearing clean gloves, carefully pull the lamp out of the lamp shield.
2. Soak a lint-free swab in isopropyl alcohol, and then dip the swab in aluminum oxide
polishing compound (5 micron powder).
3. Carefully polish the lamp window with the swab until you remove the remaining
material.
4. Soak another lint-free swab in isopropyl alcohol and remove the polishing compound
from the window.
5. While wearing a new pair of clean gloves, carefully push the lamp into the lamp shield.

 To replace the APPI lamp

1. Follow the procedure “To prepare the API source.”


2. While wearing clean gloves, carefully pull the lamp out.
3. Push the new lamp into the light source.

You can now install the API source onto the mass spectrometer, reconnect the DB15 plug to
the APPI light source, and turn on the APPI power switch.

Maintenance for the APPI Fan Filter


This procedure describes how to clean the air filter for the APPI light source’s fan.

 To clean the APPI fan filter

1. Follow steps 1–3 in the procedure “To prepare the API source.”
2. Place the APPI power switch in the position.
3. Using the screwdriver, remove the fan guard.
4. Remove the air filter.
5. Wash the filter in a solution of soap and tap water.
6. Rinse the filter with tap water, and then allow it to air dry.
7. Reinstall the filter and then the fan guard.

50 OptaMax NG Ion Source User Guide Thermo Scientific


4 Maintenance
Maintaining the API Source Housing

Maintaining the API Source Housing


Only Thermo Fisher Scientific field service engineers can service the API source housing,
while user maintenance is limited to cleaning the housing as necessary. For any additional
service, contact your local Thermo Fisher Scientific service engineer.

 To clean the API source housing

1. After the API source cools to room temperature, remove it from the mass spectrometer
(see page 19).
2. Put on appropriate eyewear and gloves.
3. Under an appropriate fume hood, use a spray bottle to put UHPLC/MS-grade methanol
on Kimwipes
4. Wipe the interior of the housing with the moistened Kimwipes.
5. Use MS grade Nitrogen gas to blow dry the API source housing.

Thermo Scientific OptaMax NG Ion Source User Guide 51


4 Maintenance
Maintaining the API Source Housing

52 OptaMax NG Ion Source User Guide Thermo Scientific


5

Replaceable Parts
This chapter provides the part numbers for the OptaMax NG ion source’s replaceable parts.
• API Source Housing
• APCI Parts
• APPI Parts

API Source Housing


OptaMax NG Source Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . OPTON-32100
H-ESI/APCI combination nozzle (spray insert) and source housing . . . . . . . . 80111-60470
H-ESI spray insert (high flow). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . OPTON-32103
Viper capillary, high flow, 0.13 mm ID, 15 cm long . . . . . . . . . . . . . . . . . . OPTON-30137
Viper Capillary Kit, 0.13 mm ID 15 cm long (5 each) . . . . . . . . . . . . . . . .00109-99-00068
Needle insert, electrospray, low flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . OPTON-30139
nanoViper™capillary, low flow, 50 μm ID, 15 cm long . . . . . . . . . . . . . . . . OPTON-30695

APCI Parts
APCI kit w/APCI Sprayer, OptaMax. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . OPTON-32101
APCI nozzle assembly, complete . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80111-60060
APCI corona needle, stainless steel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80111-20683
APCI fused-silica capillary insert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80000-60164
APCI fused-silica insert assembly
Fused-silica sample tube (capillary), 150 μm ID, 390 μm OD,
8.8 cm long . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00106-10498
O-ring, Viton, 0.219 in. ID, 1/16 in. thick . . . . . . . . . . . . . . . . . . . . . . . 00107-04000

APPI Parts
APPI VUV lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00950-10002
APPI Interface Kit (see page 31) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . OPTON-30185
APPI drain insert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80000-60396
Cover, APPI source (left side) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80000-10327
PhotoMate APPI light source and accessories . . . . . . . . . . . . . . . . . . . 00950-01-00235

Thermo Scientific OptaMax NG Ion Source User Guide 53


5 Replaceable Parts
APPI Parts

54 OptaMax NG Ion Source User Guide Thermo Scientific


G

Glossary

A B C D E F G H I J K L M N O P Q R S T U V W X Y Z

A API source The sample interface between the liquid


chromatograph (LC) and the mass spectrometer
APCI corona discharge current The ion current (MS).
carried by the charged particles in the APCI source.
The voltage on the APCI corona discharge needle APPI nozzle The nozzle in the APPI spray insert that
supplies the potential required to ionize the particles. sprays the sample solution into a fine mist.
The APCI corona discharge current is set; the APCI
atmospheric pressure chemical ionization (APCI) A
corona discharge voltage varies, as required, to
soft ionization technique done in an ion source
maintain the set discharge current.
operating at atmospheric pressure. Electrons from a
APCI corona discharge voltage The high voltage that corona discharge initiate the process by ionizing the
is applied to the corona discharge needle in the APCI mobile phase vapor molecules, forming a reagent gas.
source to produce the APCI corona discharge. The
atmospheric pressure ionization (API) Ionization
corona discharge voltage varies, as required, to
performed at atmospheric pressure by using
maintain the set APCI spray current.
electrospray ionization (ESI), heated-electrospray
APCI corona discharge needle A needle to which a ionization (H-ESI), atmospheric pressure chemical
sufficiently high voltage (typically ±3 to ±5 kV) is ionization (APCI), or atmospheric pressure
applied to produce a chemical ionization (CI) plasma photoionization (APPI).
by the corona discharge mechanism.
atmospheric pressure photoionization (APPI) A
APCI sample tube A fused silica tube that delivers soft ionization technique that shows an ion generated
sample solution to the APCI nozzle. The APCI from a molecule when it interacts with a photon
sample tube extends from the sample inlet to the from a light source.
APCI nozzle.
auxiliary gas The outer-coaxial gas (nitrogen) that
APCI vaporizer A heated tube that vaporizes the assists the sheath (inner-coaxial) gas in dispersing
sample solution as the solution exits the APCI and/or evaporating sample solution as the sample
sample tube and enters the atmospheric pressure solution exits the ESI, APCI (optional), or APPI
region of the APCI-configured source. (optional) spray insert.

API ion transfer tube A tube assembly that assists in


desolvating ions that are produced by the ESI, APCI,
or APPI nozzle.

Thermo Scientific OptaMax NG Ion Source User Guide 55


Glossary: chemical ionization (CI) plasma

C
chemical ionization (CI) plasma The collection of
ions, electrons, and neutral species formed in the ion
source during chemical ionization (CI).

corona discharge In the APCI source, an electrical


discharge in the region around the corona discharge
needle that ionizes gas molecules to form a chemical
ionization (CI) plasma, which contains CI reagent
ions.

E
electrospray ionization (ESI) A type of atmospheric
pressure ionization that is currently the softest
ionization technique available to transform ions in
solution into ions in the gas phase.

H
heated-electrospray ionization (H-ESI) A type of
atmospheric pressure ionization that converts ions in
solution into ions in the gas phase by using
electrospray (ESI) in combination with heated
auxiliary gas.

I
ion source See API source.

ion sweep cone A removable cone shaped metal cover


that fits on top of the API ion transfer tube and acts
as a physical barrier to protect the entrance of the
tube.

N
nozzle The nozzle in the spray insert that sprays the
sample solution into a fine mist.

S
sheath gas The inner coaxial gas (nitrogen), which is
used in the API ion transfer tube to help nebulize the
sample solution into a fine mist as the sample
solution exits the H-ESI or APCI nozzle.

56 OptaMax NG Ion Source User Guide Thermo Scientific


I

Index

A See APCI corona discharge needle settings


corrosion prevention 11
APCI corona discharge needle, settings 27
APCI mode
description 2–3 D
spray insert, description 16 directives
API source WEEE iii
features 10 documentation, accessing ix
heater assembly (figure) 11
heater/vaporizer tube (figure) 11
H-ESI spray insert (figure) 11 F
housing figures, list of vii
cleaning 51 fume exhaust requirements 12
installing 20
mode configurations
identifying (images) 24
G
summary procedures 25 gas plumbing, H-ESI spray insert 15
removing 19 grounding union, installing for H-ESI mode 34
safety interlocks 10
API spray inserts H
description 13–16
gas plumbing, H-ESI 15 heater assembly
description 10
APPI installation kit, installing 30
location (figure) 11
APPI lamp depth position 33
H-ESI mode
APPI mode
components (figure) 30
configuring the housing 29
configuring the housing 33
DB15 plug, function 32
grounding union, installing 34
description 6
spray insert, description 14
light source, description 7
power supply unit, connecting 32
spray insert, selecting 7 I
auxiliary gas flow (figure) 15 ion analysis 1
ion source
C See API source
ionization modes
chemical noise 4
APCI, description 2–3
compliance
APPI, description 6
regulatory xii
changing, summary procedures 25
contacting us xiii combined modes
corona discharge needle

Thermo Scientific OptaMax NG Ion Source User Guide 57


Index: K

setting the light source and corona discharge installing 44


needle 27 removing 43
compound polarity vs. molecular weight (figure) 2 housing
changing the mode configuration 25
cleaning 51
K H-ESI components, removing 29
kits, APPI installation 30 inlet components, flushing 41

L R
lamp, APPI regulatory compliance xii
See APPI mode, light source Remote LED (APPI) 33
light source
See PhotoMate APPI light source settings
liquid flow rates 2 S
safety interlocks 10
safety precautions xii–xiii
M
sample inlet, location 12
maintenance sample line, installing 34
See procedures
sheath gas flow (figure) 15
maintenance schedule 39
solvent waste system 12
mass spectrometer
source
compatible models per API source model x
See API source
standby mode 17
spray insert
model difference, ion sources 10
See API spray inserts
standby mode, mass spectrometer 17
O symbols, meaning x
optimizing
API source parameters 35 T
spray direction 35
Thermo Fisher Scientific website, user documents x
organic solvents 2
tools and supplies for maintenance procedures 40
trip hazard xi
P
PhotoMate APPI light source settings 27
U
polarity ranges, ionization modes 2
USB cable, APPI 32
procedures
APCI corona discharge needle
changing the position 28 V
removing 28 viewing documents x
APCI fused-silica insert
VUV lamp
installing 47
See APPI mode, light source
removing 46
APCI fused-silica sample tube, replacing 47
API spray insert W
installing 18 WEEE directive iii
removing 17
APPI (VUV) lamp
cleaning the window 49
replacing the lamp 50
APPI fan filter, cleaning 50
APPI installation kit, installing 30
H-ESI metal needle insert

58 OptaMax NG Ion Source User Guide Thermo Scientific

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