Optamax-ng-ion-source-user
Optamax-ng-ion-source-user
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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
Glossary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .57
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
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
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Accessing Documentation
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requirements refer to the release notes on the software DVD.
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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.
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.
Contacting Us
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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
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.
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.
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:
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.
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
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.
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
hν
Photoionization
Agricultural
compounds
Drugs MeOH, AcCN
Chlorinated-solvents
Steroids
H2O, CO2, O2, N2
Threshold
10.0 eV
Methanol 10.85 eV
Acetonitrile 12.19 eV
Water 12.61 eV
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).
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.
Window
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.
• 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
H-ESI or APCI
drain insert
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.
Drain/waste port
(left side)
To external vent
Internal API source API source
drain tube
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
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.”
Sheath gas
Electrospray needle
Electrospray needle
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
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.
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.
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
Guide pin
2. Slowly place the spray insert into the heater assembly on the source.
3. With your hand, tighten the spray insert nut.
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.
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).
Figure 17. Mass spectrometer mount assembly with ion sweep cone
Spray cone
Figure 18. OptaMax NG ion source with unlocked levers (back view)
APCI components
–or–
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.”
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.
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
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
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.
Needle base
4. Rinse the needle with solvents compatible with your compounds, and then store the
needle in a safe place.
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.”
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.
Figure 21. API source showing the left-side H-ESI components (exploded view)
H-ESI/APCI drain
Pin insert
H-ESI cover
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).
Figure 22. API source showing the left-side APPI components (exploded view)
Pin
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.
Figure 23. Left side of the assembled APPI source with the APCI spray insert
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.
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.
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.
• 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.
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.
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)
Sample input
Grounding union installed in the
grounding union holder (bar)
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.
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.
For instructions on how to optimize the spray voltage, the API gas pressures, and the
discharge current (APCI only), refer to the Hardware Manual.
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
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
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
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
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.
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.
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.
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.
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.
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.
IMPORTANT For best results, wear clean gloves when you handle API spray insert
components.
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.”
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.
Figure 29. Needle insert removed from the H-ESI spray 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
4. Rotate the square ferrule clockwise until you can see the needle extend from the tool.
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.
IMPORTANT For best results, wear clean gloves when you handle the API spray insert
components.
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.
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
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.
Figure 33. Exit end of the fused-silica tubing protrudes 1 mm (0.04 in.)
Nozzle union
1 mm (0.04 in.)
Power switch
Lamp shield
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.
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.
If you were unable to remove all material from the lamp window, follow the procedure “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.
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.
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.
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.
Replaceable Parts
This chapter provides the part numbers for the OptaMax NG ion source’s replaceable parts.
• API Source Housing
• APCI Parts
• APPI Parts
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
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
C
chemical ionization (CI) plasma The collection of
ions, electrons, and neutral species formed in the ion
source during chemical ionization (CI).
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.
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.
Index
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