DESI System
Operator’s Guide
715004701/Revision A
Copyright © Waters Corporation 2015
All rights reserved
January 14, 2015, 715004701 Rev. A
Page ii
General Information
Copyright notice
© 2015 WATERS CORPORATION. PRINTED IN THE UNITED STATES OF AMERICA AND
IN IRELAND. ALL RIGHTS RESERVED. THIS DOCUMENT OR PARTS THEREOF MAY NOT
BE REPRODUCED IN ANY FORM WITHOUT THE WRITTEN PERMISSION OF THE
PUBLISHER.
The information in this document is subject to change without notice and should not
be construed as a commitment by Waters Corporation. Waters Corporation assumes
no responsibility for any errors that may appear in this document. This document is
believed to be complete and accurate at the time of publication. In no event shall
Waters Corporation be liable for incidental or consequential damages in connection
with, or arising from, its use. For the most recent revision of this document, consult
the Waters Web site (waters.com).
Trademarks
Waters, “THE SCIENCE OF WHAT’S POSSIBLE.”, ESCi, UPLC, Xevo, and MassLynx are
registered trademarks of Waters Corporation and IntelliStart, LockSpray, NanoFlow,
NanoLockSpray, StepWave andT-Wave, are trademarks of Waters Corporation.
Microsoft, Windows, Word, Excel, and PowerPoint are registered trademarks of
Microsoft Corporation in the United States and/or other countries.
PEEK is a trademark of Victrex plc.
TaperTip is a trademark of New Objective, Inc.
Other registered trademarks or trademarks are the sole property of their owners.
Customer comments
Waters’ Technical Communications organization invites you to report any errors that
you encounter in this document or to suggest ideas for otherwise improving it. Help
us better understand what you expect from our documentation so that we can
continuously improve its accuracy and usability.
We seriously consider every customer comment we receive. You can reach us at
[email protected].
January 14, 2015, 715004701 Rev. A
Page iii
Contacting Waters
Contact Waters with enhancement requests or technical questions regarding the use,
transportation, removal, or disposal of any Waters product. You can reach us via the
Internet, telephone, or conventional mail.
Waters contact information:
Contacting medium
Information
Internet
The Waters Web site includes contact
information for Waters locations worldwide.
Visit www.waters.com.
Telephone and fax
From the USA or Canada, phone
800 252-4752, or fax 508 872 1990.
For other locations worldwide, phone and fax
numbers appear in the Waters Web site.
Conventional mail
Waters Corporation
34 Maple Street
Milford, MA 01757
USA
Safety considerations
Some reagents and samples used with Waters instruments and devices can pose
chemical, biological, or radiological hazards (or any combination thereof). You must
know the potentially hazardous effects of all substances you work with. Always follow
Good Laboratory Practice, and consult your organization’s standard operating
procedures.
Safety hazard symbol notice
Documentation needs to be consulted in all cases where the
symbol is used to
find out the nature of the potential hazard and any actions which have to be taken.
January 14, 2015, 715004701 Rev. A
Page iv
Considerations specific to the DESI
Power cord replacement hazard
Warning: To avoid electric shock, use the SVT-type power cord in the
United States and HAR-type (or better) in Europe. The main power cord
must only be replaced with one of adequate rating. For information
regarding what cord to use in other countries, contact your local Waters
distributor.
High temperature hazard
Warning: To avoid burn injuries, before performing maintenance
operations that involve handling components inside the mass
spectrometer's ion source, allow the source interior to cool.
High voltage hazard
Warning:
• To avoid electric shock, do not remove the mass spectrometer’s
protective panels. The components they cover are not
user-serviceable.
• To avoid nonlethal electric shock when the instrument is in Operate
mode, avoid touching the areas marked with the high voltage warning
symbol. To touch those areas, first put the instrument in Standby
mode.
Crush hazards
Warning: To avoid crush injury, be careful when working near the
moving parts of the DESI.
Hazards associated contamination
Warning: To avoid personal contamination with biohazards,
toxic materials, and corrosive materials, wear
chemical-resistant gloves during all phases of instrument
decontamination.
Warning: To avoid puncture injuries, handle syringes, fused silica lines,
and borosilicate tips with extreme care.
January 14, 2015, 715004701 Rev. A
Page v
When you remove the instrument from use to repair or dispose of it, you must
decontaminate all of its vacuum areas. These are the areas in which you can expect to
encounter the highest levels of contamination:
•
Source interior
•
Waste tubing
•
Exhaust system
The need to decontaminate other vacuum areas of the instrument depends on the
kinds of samples the instrument analyzed and their levels of concentration. Do not
dispose of the instrument or return it to Waters for repair until the authority
responsible for approving its removal from the premises specifies the extent of
decontamination required and the level of residual contamination permissible. That
authority must also prescribe the method of decontamination to be used and the
appropriate protection for personnel undertaking the decontamination process.
You must handle items such as syringes, fused silica lines, and borosilicate tips used
to carry sample into the source area in accordance with laboratory procedures for
contaminated vessels and sharps. To avoid contamination by carcinogens, toxic
substances, or biohazards, you must wear chemical-resistant gloves when handling or
disposing of used oil.
Bottle placement prohibition
Prohibited: To avoid equipment damage caused by spilled solvent, do
not place reservoir bottles directly atop an instrument or device or on its
front ledge. Instead, place the bottles in the bottle tray, which serves as
a secondary containment in the event of spills.
FCC radiation emissions notice
Changes or modifications not expressly approved by the party responsible for
compliance, could void the users authority to operate the equipment. This device
complies with Part 15 of the FCC Rules. Operation is subject to the following two
conditions: (1) this device may not cause harmful interference, and (2) this device
must accept any interference received, including interference that may cause
undesired operation.
Electrical power safety notice
Do not position the instrument so that it is difficult to operate the disconnecting
device.
Equipment misuse notice
If the equipment is used in a manner not specified by the manufacturer, the
protection provided by the equipment may be impaired.
Safety advisories
Consult Appendix A for a comprehensive list of warning advisories and notices.
January 14, 2015, 715004701 Rev. A
Page vi
Operating this DESI ion source
When operating this DESI ion source, follow standard quality-control (QC) procedures
and the guidelines presented in this section.
Applicable symbols
Symbol
Definition
Manufacturer
Date of manufacture
Authorized representative of the European
Community
Confirms that a manufactured product complies
with all applicable European Community directives
Australia EMC compliant
or
Confirms that a manufactured product complies
with all applicable United States and Canadian
safety requirements
Consult instructions for use
Supply ratings
Electrical and electronic equipment with this
symbol may contain hazardous substances and
should not be disposed of as general waste.
For compliance with the Waste Electrical and
Electronic Equipment Directive (WEEE)
2012/19/EU, contact Waters Corporation for the
correct disposal and recycling instructions.
Serial number
Part number catalog number
5()
January 14, 2015, 715004701 Rev. A
Page vii
Audience and purpose
This guide is for operators with high levels of experience. The DESI ion source should
not be used by anyone who has not been trained adequately. This manual gives an
overview of the DESI ion source, and explains how to prepare it, change its modes of
operation, and maintain it.
Intended use of the DESI ion source
The DESI ion source is designed for use with XEVO G2-XS and SYNAPT G2-Si mass
spectrometers. The source offers automated sample positioning and the full
advantage of desorption electrospray ionization technology. When used with a mass
spectrometer, the DESI source eliminates the need for complex and time-consuming
sample preperation.
DESI ion source instrumentation is not intended for use as a medical device. It is
intended for use only in a laboratory environment in non-medical applications.
The DESI ion source must not be used in human experimentation or be applied to
living humans in any way.
The efficacy of DESI has been demonstrated in many applications, from explosives to
proteomics.
See Appendix B for information about operating the source.
EMC considerations
Canada spectrum management emissions notice
This class A digital product apparatus complies with Canadian ICES-001.
Cet appareil numérique de la classe A est conforme à la norme NMB-001.
ISM Classification: ISM Group 1 Class A
This classification has been assigned in accordance with IEC CISPR 11 Industrial
Scientific and Medical (ISM) instruments requirements. Group 1 products apply to
intentionally generated and/or used conductively coupled radio-frequency energy that
is necessary for the internal functioning of the equipment. Equipment defined as Class
A is suitable for use in all establishments other than domestic establishments. Class A
equipment can be directly connected to a low-voltage power-supply network that
supplies buildings used for domestic purposes.
January 14, 2015, 715004701 Rev. A
Page viii
EC authorized representative
Waters Corporation
Stamford Avenue
Altrincham Road
Wilmslow SK9 4AX UK
Telephone:
+44-161-946-2400
Fax:
+44-161-946-2480
Contact:
Quality manager
January 14, 2015, 715004701 Rev. A
Page ix
January 14, 2015, 715004701 Rev. A
Page x
Table of Contents
General Information .................................................................. iii
Copyright notice ......................................................................................... iii
Trademarks ................................................................................................ iii
Customer comments ................................................................................... iii
Contacting Waters ...................................................................................... iv
Safety considerations .................................................................................. iv
Safety hazard symbol notice.............................................................. iv
Considerations specific to the DESI.....................................................
v
FCC radiation emissions notice........................................................... vi
Electrical power safety notice............................................................. vi
Equipment misuse notice .................................................................. vi
Safety advisories ............................................................................. vi
Operating this DESI ion source .................................................................... vii
Applicable symbols.......................................................................... vii
Audience and purpose .................................................................... viii
Intended use of the DESI ion source................................................. viii
EMC considerations ................................................................................... viii
Canada spectrum management emissions notice ................................ viii
ISM Classification: ISM Group 1 Class A ............................................ viii
EC authorized representative ........................................................................ ix
..................................................................................................... ix
1 Desorption Electrospray Ionisation (DESI) ion source .............
13
1.1
Description .............................................................................................. 14
1.2
Handling .................................................................................................. 15
2 The Waters spray head ............................................................
2.1
2.2
19
Waters spray head assembly ..................................................................... 19
2.1.1
Installing the Waters spray head........................................................ 20
2.1.2
Removing the Waters spray head....................................................... 20
Maintenance ............................................................................................ 20
2.2.1
Replacing the fused silica emitter tip .................................................. 21
2.2.2
Cleaning the Waters spray head ........................................................ 25
January 14, 2015, 715004701 Rev. A
Page xi
3 Maintenance Procedures ..........................................................
27
3.1
Maintenance schedule ............................................................................... 27
3.2
Spare parts .............................................................................................. 28
3.2.1
Parts catalogue ............................................................................... 28
3.3
Replacing fuses ........................................................................................ 28
3.4
Spray-head nozzle/emitter replacement ....................................................... 28
3.5
Spray head cleaning .................................................................................. 29
3.5.1
Prosolia spray head.......................................................................... 29
3.5.2
Waters spreay head ......................................................................... 29
A Safety Advisories .....................................................................
A.1
31
Warning symbols ...................................................................................... 31
A.1.1
Specific warnings ............................................................................ 32
A.2
Notices ................................................................................................... 34
A.3
Bottles Prohibited symbol .......................................................................... 34
A.4
Required protection .................................................................................. 35
A.5
Warnings that apply to all Waters instruments and devices ............................. 35
A.6
Warnings that address the replacing of fuses ................................................ 38
A.7
Electrical and handling symbols .................................................................. 40
A.7.1
Electrical symbols............................................................................ 40
A.7.2
Handling symbols ............................................................................ 41
B Prosolia DESI Source 2D, Installation and Operation Manual ...
B.1
43
The Prosolia DESI manual .......................................................................... 43
January 14, 2015, 715004701 Rev. A
Page xii
1
Desorption Electrospray
Ionisation (DESI) ion source
This chapter describes the DESI ion source. For a description of the control and
operation of the DESI ion source, see Appendix B.
Warning: To avoid the escape of vaporised materials, from the DESI
source, which is not gas tight, to the laboratory atmosphere, observe the
appropriate safety guidelines for the material being sampled.
January 14, 2015, 715004701 Rev. A
Page 13
1.1 Description
Desorption Electrospray ionisation (DESI), is a pneumatically assisted electrospray
technique, in which a solvent is directed towards the sample of intrest. The resultant
ions are sampled directly, under ambient conditions, in the Mass Spectrometer.
High voltage
source
Solvent
N2
Spray
nozzle
Inlet to mass
spectrometer
Freely
moving
sample
stage
Desorbed ions
Spray
Sample
These variables can help achieve optimal spectral results;
•
Solvent
•
Gas flow rate
•
Amount of applied voltage
•
Spray angle
•
Ion uptake angle
•
Distances involved in aligning the spray
•
Sample type
An expanded publications list related to DESI is available on the Prosolia website,
www.prosolia.com.
January 14, 2015, 715004701 Rev. A
Page 14
1.2 Handling
Warning: To avoid burn injuries, do not touch the ion block when the
instrument is in use or when it has been in recent use.
Warning: To avoid puncture wounds, do not touch the sharp tips of the
spray capillaries or emitter.
Warning: To avoid electric shock, ensure that the high voltage is
switched off before touching the source‘s spray head. The ion block and
the spray head must be installed before the high voltage is switched on.
Warning: To avoid injury, from the sudden release of highly
pressurised Nitrogen, depressurize before working on the source head or
spray capillaries.
Warning: To avoid crush injury, be careful when working near the
moving parts of the DESI.
Notice: To avoid damaging the DESI source, do not lift it by its handles.
The handles are intended only for lifting the source‘s lid.
Solvent input
Emitter
Gas input
High voltage
input
Prosolia spray head
January 14, 2015, 715004701 Rev. A
Page 15
Gas fitting
H.V. connection
PEEK body
Solvent fitting
Gas cone
Mounting
bracket
Waters spray head
The Waters spray head is designed to operate with lower gas and solvent flow rates
than previous models. This will allow for greater accuracy of analysis.
When installing, removing or handling the DESI unit, care must be taken to prevent
damage.
Particular care should be taken to make sure damage does not occur to:
•
The emitter/spray head
•
Fused silica
•
Solvent tubing
•
Gas connections and tubing
•
Ion transfer capillary (Bazooka).
January 14, 2015, 715004701 Rev. A
Page 16
Ion block
Ion capilliary
Spray-head arm, folded
for access
Spray head
When moving the spray-head arm, ensure that the tubing and cabling does not
become stretched and the routing is not altered.
When moving the tray, ensure that the ion transfer capilliary clears the tray‘s surface.
Notice: To avoid damaging the DESI source, do not lift it by its handles.
The handles are intended only for lifting the source‘s lid.
When necessary, lift the DESI source from the instrument by supporting it from its
underside.
When preparing tubing, ensure that all cuts are perpindicular or square to the tubing.
January 14, 2015, 715004701 Rev. A
Page 17
January 14, 2015, 715004701 Rev. A
Page 18
2
The Waters spray head
This chapter describes the installation, removal and maintenance of the Waters
spray head.
2.1 Waters spray head assembly
Gas fitting
H.V. connection
PEEK body
Solvent fitting
Gas cone
Mounting
bracket
Notice: There are differences between the way the Waters spray head
and the Prosolia spray head are set up and operated. The Waters spray
head is initially installed by a Waters technician. If the Prosolia spray
head is to be installed after the initial installation, you must refer to the
Prosolia documentation (at Appendix B) for set up and gas pressure
information.
The Waters spray head is shipped preloaded with a fused silica emitter. Before using
the source, you must adjust the length of the emitter that protrudes from the nozzle
by turning the nozzle clockwise using the 4-mm wrench provided with the source. The
emitter must protrude approximately 1-mm beyond the tip of the spray nozzle.
You must also connect tubing for the spray solvent and nitrogen nebulizing gas to the
spray head. The tubing and fittings necessary to make these connections are provided
with the source.
The spray head uses TaperTip® emitters, which are precut to 40-mm and provide an
identical configuration when replaced. Thus they are designed to provide
reproducability, robustness, and high performance.
January 14, 2015, 715004701 Rev. A
Page 19
2.1.1
Installing the Waters spray head
1.
Turn the source out of operate and power off the DESI control unit.
2.
Open the cover, and remove it, if necessary.
Warning: To avoid crush injury, be careful when working near the
moving parts of the DESI.
3.
Lower the DESI stage, and move the arm to the maintenance position.
Warning: To avoid puncture wounds, do not touch the sharp tips of the
spray capillaries or emitter.
4.
On the new spray head, use a 4-mm wrench to turn the gas cone clockwise until
the emitter tip protrudes by approx 0.5-mm to 1-mm.
5.
Install the new mounting bracket and spray head assembly.
6.
Install the solvent fitting to the spray head.
Note: The supplied 360 µm o.d. fitting for the solvent capillary does not require a
sleeve. Capilliaries whose outer dimensions are larger or smaller than 360 µm
require the use of alternative fittings. Refer to the Waters website for
information about spare parts.
7.
Install the high voltage connection onto the spray head.
8.
Fit the gas fitting to the spray head.
9.
Install the cover, if necessary.
2.1.2
Removing the Waters spray head.
1.
Turn the source out of operate and power off the DESI control unit.
2.
Disconnect the voltage connection.
Warning: To avoid burn injuries, do not touch the ion block when the
instrument is in use or when it has been in recent use.
3.
Turn off the gas supply.
4.
Disconnect the gas fitting.
5.
Disconnect the solvent fitting.
Warning: To avoid puncture wounds, do not touch the sharp tips of the
spray capillaries or emitter.
6.
Remove the spray head assembly, including the mounting bracket.
2.2 Maintenance
The Waters spray head requires no routine maintenance procedures. Nevertheless,
depending on usage, you should perform the following procedures periodically:
January 14, 2015, 715004701 Rev. A
Page 20
•
Replace the fused silica emitter tip
•
Clean the Waters spray head
2.2.1
Replacing the fused silica emitter tip
Replace the fused silica emitter tip when any of the following conditions apply:
•
The Waters spray head is dismantled.
•
When you suspect the use of contaminated solvent.
•
You suspect a regularly used instrument is giving erroneous results.
To remove the emitter tip:
Warning: To avoid puncture wounds, do not touch the sharp tips of the
spray capillaries or emitter.
1.
Turn the source out of operate and power off the DESI control unit.
2.
Disconnect the voltage, gas and solvent inputs.
3.
Lower the stage.
4.
Swing the arm to access the spray head.
5.
Remove the spray head.
6.
Remove the metal rear section from the body of the spray head.
January 14, 2015, 715004701 Rev. A
Page 21
7.
Use wrenches to loosen the front section of the metal assembly.
8.
Remove the emitter tip.
To install a new fused silica emitter-tip:
Warning: To avoid puncture wounds, do not touch the sharp tips of the
spray capillaries or emitter.
1.
Remove the metal assembly from the PEEK body.
2.
Use a wrench to seperate the two parts of the metal assembly.
Front metal part
3.
Ferrule
Remove and keep the ferrule.
January 14, 2015, 715004701 Rev. A
Page 22
Rear metal part
4.
Screw the positioning nut onto the rear metal part.
Positioning
nut
5.
Insert a new emitter, cut-end first, through the front, metal part and through
the ferrule.
6.
Install the front, metal part on the rear metal part.
7.
Ensure that the emitter found its correct place against the positioning nut.
8.
Use wrenches to tighten together the front, metal part and the rear, metal part.
Apply wrenches here
January 14, 2015, 715004701 Rev. A
Page 23
9.
Install the metal assembly in the PEEK body.
10. Hold the PEEK body so that it is horizontal, and install the gas cone on the front,
metal part.
Gas cone
11. Use a wrench to wind the gas cone into the body until the emitter tip protrudes
by approx 1.0-mm.
12. Remove the positioning nut.
13. Ensure that the DESI control unit is off and the source is out of operate.
14. Install the spray head.
January 14, 2015, 715004701 Rev. A
Page 24
2.2.2
Cleaning the Waters spray head
Clean the Waters spray head when any of the following conditions apply:
•
The fused silica emitter tip is removed or replaced.
•
The solvent is changed.
•
When you suspect the use of contaminated solvent.
You clean the system by pumping solvent through it without using a lockmass.
January 14, 2015, 715004701 Rev. A
Page 25
January 14, 2015, 715004701 Rev. A
Page 26
3
Maintenance Procedures
Keep to a maintenance schedule, and perform maintenance as required and
described in this chapter.
3.1 Maintenance schedule
The following table lists maintenance operations that ensure optimum instrument
performance.
Perform replacement tasks as necessary. Those appearing below apply to instruments
that normally receive moderate use.
See Appendix A for safety advisory information.
Warning: To avoid personal contamination from contact with
biohazards or toxic materials, always wear clean,
chemical-resistant, powder-free gloves when performing
maintenance operations.
Warning: To prevent injury, always observe Good Laboratory Practice
when handling solvents, changing tubing, or operating the instrument.
Know the physical and chemical properties of the solvents used (see the
Material Safety Data Sheets for the solvents in use).
Warning: To avoid electric shock:
• do not remove the instrument’s panels. There are no user-serviceable
items inside the instrument.
• ensure that the instrument is in Standby mode before begining any
maintenance operation.
Maintenance schedule:
Procedure
Clean the instrument case.
Frequency
Information...
As required.
Do not clean with
abrasive or
solvents.
Clean the source components. When sensitivity
decreases to
unacceptable levels.
January 14, 2015, 715004701 Rev. A
Page 27
See Appendix B
Maintenance schedule: (continued)
Procedure
Frequency
Information...
Spray head cleaning.
When sensitivity
decreases to
unacceptable levels.
See Appendix B
(Prosolia) or
Chapter 2.2.2
(Waters)
Spray head nozzle/Emitter
replace.
As required on
condition.
See Appendix B
(Prosolia) or
Chapter 2.1,
(Waters).
Fuse replacement.
As required.
See Appendix B
3.2 Spare parts
To ensure that the system operates as designed, use only Waters Quality Parts. Visit
www.waters.com/wqp for information about Waters Quality Parts, including how to
order them.
3.2.1
Parts catalogue
See Appendix B for a list of Waters-approved Prosolia parts.
For Waters consumable parts refer to Waters.com.
3.3 Replacing fuses
Under normal operation, the fuses protecting the DESI control electronics do not need
replacing. Should a fuse for the control electronics open, replace it according to the
procedure at Appendix B.
3.4 Spray-head nozzle/emitter replacement
A qualified technician must replace the spray nozzle/emitter. Improper installation can
adversley affect the quality of results.
For details about replacing the spray-head nozzle/emitter, see Appendix B (Prosolia)
or Chapter 2.1.2 (Waters).
January 14, 2015, 715004701 Rev. A
Page 28
3.5 Spray head cleaning
You can clean the spray head of the DESI source if you suspect chemical
contamination of the spray head. When doing so, avoid damaging the spray head‘s
o-ring seals. Simple cleaning of the outer surfaces involves wiping the spray head
using a wipe saturated in methanol. Note that you must not submerge the spray head
in solvents.
3.5.1
Prosolia spray head
Thoroughly cleaning the Prosolia spray head requires disassembly and removal of the
o-ring seals. Except for the electrode assembly, you can clean all parts of the spray
head by sonication in methanol. After removing the spray head from the source,
follow the procedure in Appendix B to disassemble and clean the spray head.
3.5.2
Waters spreay head
For details about cleaning the Waters spray head, follow the procedure in
Chapter 2.2.2
January 14, 2015, 715004701 Rev. A
Page 29
January 14, 2015, 715004701 Rev. A
Page 30
A
Safety Advisories
Waters instruments and devices display hazard symbols that alert you to the hidden
dangers associated with a product’s operation and maintenance. The symbols also
appear in product manuals where they accompany statements describing the hazards
and advising how to avoid them. This appendix presents the safety symbols and
statements that apply to all of Waters’ product offerings.
A.1 Warning symbols
Warning symbols alert you to the risk of death, injury, or seriously adverse
physiological reactions associated with the misuse of an instrument of device. Heed all
warnings when you install, repair, or operate any Waters instrument or device. Waters
accepts no liability in cases of injury or property damage resulting from the failure of
individuals to comply with any safety precaution when installing, repairing, or
operating any of its instruments or devices.
The following symbols warn of risks that can arise when you operate or maintain a
Waters instrument or device or component of an instrument or device. When one of
these symbols appear in a manual’s narrative sections or procedures, an
accompanying statement identifies the applicable risk and explains how to avoid it.
Warning: (General risk of danger. When this symbol appears on an
instrument, consult the instrument’s user documentation for important
safety-related information before you use the instrument.)
Warning: (Risk of burn injury from contacting hot surfaces.)
Warning: (Risk of electric shock.)
Warning: (Risk of fire.)
Warning: (Risk of sharp-point puncture injury.)
Warning: (Risk of hand crush injury.)
Warning: (Risk of injury caused by moving machinery.)
Warning: (Risk of exposure to ultraviolet radiation.)
Warning: (Risk of contacting corrosive substances.)
January 14, 2015, 715004701 Rev. A
Page 31
Warning: (Risk of exposure to a toxic substance.)
Warning: (Risk of personal exposure to laser radiation.)
Warning: (Risk of exposure to biological agents that can pose a serious health
threat.)
Warning: (Risk of tipping.)
Warning: (Risk of explosion.)
Warning: (Risk of high-pressure gas release.)
A.1.1 Specific warnings
The following warnings (both symbols and text) can appear in the user manuals of
particular instruments and devices and on labels affixed to them or their component
parts.
A.1.1.1
Burst warning
This warning applies to Waters instruments and devices fitted with nonmetallic tubing.
Warning: To avoid injury from bursting, nonmetallic tubing, heed these
precautions when working in the vicinity of such tubing when it is pressurized:
• Wear eye protection.
• Extinguish all nearby flames.
• Do not use tubing that is, or has been, stressed or kinked.
• Do not expose nonmetallic tubing to compounds with which it is chemically
incompatible: tetrahydrofuran, nitric acid, and sulfuric acid, for example.
• Be aware that some compounds, like methylene chloride and dimethyl
sulfoxide, can cause nonmetallic tubing to swell, significantly reducing the
pressure at which the tubing can rupture.
A.1.1.2
Mass spectrometer shock hazard
The following warning applies to all Waters mass spectrometers.
Warning: To avoid electric shock, do not remove the mass spectrometer’s
protective panels. The components that they cover are not user-serviceable.
The following warning applies to certain mass spectrometers when they are in
Operate mode.
Warning: To avoid harmless, static-like electric shock, ensure the mass
spectrometer is in Standby mode before you touch any of its external surfaces
that are marked with this high voltage warning symbol.
January 14, 2015, 715004701 Rev. A
Page 32
A.1.1.3
Mass spectrometer flammable solvents warning
This warning applies to mass spectrometers performing an analysis that requires the
use of flammable solvents.
Warning: To prevent ignition of flammable solvent vapors in the enclosed
space of a mass spectrometer’s ion source, ensure that nitrogen flows
continuously through the source. The nitrogen supply pressure must not fall
below 690 kPa (6.9 bar, 100 psi) during an analysis requiring the use of
flammable solvents. Also a gas-fail device must be installed, to interrupt the
flow of LC solvent should the nitrogen supply fail.
A.1.1.4
Biohazard warning
The following warning applies to Waters instruments and devices that can process
material containing biohazards, which are substances that contain biological agents
capable of producing harmful effects in humans.
Warning: To avoid infection with potentially infectious, human-sourced
products, inactivated microorganisms, and other biological materials, assume
that all biological fluids that you handle are infectious.
Specific precautions appear in the latest edition of the US National Institutes of
Health (NIH) publication, Biosafety in Microbiological and Biomedical
Laboratories (BMBL).
Observe Good Laboratory Practice (GLP) at all times, particularly when working
with hazardous materials, and consult the biohazard safety representative for
your organization regarding the proper use and handling of infectious
substances.
January 14, 2015, 715004701 Rev. A
Page 33
A.1.1.5
Biohazard and chemical hazard warning
These warnings apply to Waters instruments and devices that can process biohazards,
corrosive materials, or toxic materials.
Warning: To avoid personal contamination with biohazards, toxic materials, or
corrosive materials, you must understand the hazards associated with their handling.
Guidelines prescribing the proper use and handling of such materials appear in the
latest edition of the National Research Council's publication, Prudent Practices in the
Laboratory: Handling and Management of Chemical Hazards.
Observe Good Laboratory Practice (GLP) at all times, particularly when working with
hazardous materials, and consult the safety representative for your organization
regarding its protocols for handling such materials.
A.2 Notices
Notice advisories appear where an instrument or device can be subject to use or
misuse that can damage it or compromise a non-clinical sample’s integrity (risks to
clinical sample integrity are accompanied by warning symbols). The exclamation point
symbol and its associated statement alert you to such risk.
Notice: To avoid damaging the instrument’s case, do not clean it with
abrasives or solvents.
A.3 Bottles Prohibited symbol
The Bottles Prohibited symbol alerts you to the risk of equipment damage caused by
solvent spills.
Prohibited: To avoid equipment damage caused by spilled solvent, do not
place reservoir bottles directly atop an instrument or device or on its front
ledge. Instead, place the bottles in the bottle tray, which serves as secondary
containment in the event of spills.
January 14, 2015, 715004701 Rev. A
Page 34
A.4 Required protection
The Use Eye Protection and Wear Protective Gloves symbols alert you to the
requirement for personal protective equipment. Select appropriate protective
equipment according to your organization’s standard operating procedures.
Requirement: Use eye protection when refilling or replacing solvent bottles.
Requirement: Wear clean, chemical-resistant, powder-free gloves when
handling samples.
A.5 Warnings that apply to all Waters instruments
and devices
When operating this device, follow standard quality-control procedures and the
equipment guidelines in this section.
Attention: Changes or modifications to this unit not expressly approved by the
party responsible for compliance could void the user’s authority to operate the
equipment.
Important: Toute modification sur cette unité n’ayant pas été expressément
approuvée par l’autorité responsable de la conformité à la réglementation peut
annuler le droit de l’utilisateur à exploiter l’équipement.
Achtung: Jedwede Änderungen oder Modifikationen an dem Gerät ohne die
ausdrückliche Genehmigung der für die ordnungsgemäße Funktionstüchtigkeit
verantwortlichen Personen kann zum Entzug der Bedienungsbefugnis des
Systems führen.
Avvertenza: qualsiasi modifica o alterazione apportata a questa unità e non
espressamente autorizzata dai responsabili per la conformità fa decadere il
diritto all'utilizzo dell'apparecchiatura da parte dell'utente.
Atencion: cualquier cambio o modificación efectuado en esta unidad que no
haya sido expresamente aprobado por la parte responsable del cumplimiento
puede anular la autorización del usuario para utilizar el equipo.
注意：未經有關法規認證部門允許對本設備進行的改變或修改,可能會使使用者喪失操作該設
備的權利。
注意：未经有关法规认证部门明确允许对本设备进行的改变或改装，可能会使使用者丧失操
作该设备的合法性。
주의: 규정 준수를 책임지는 당사자의 명백한 승인 없이 이 장치를 개조 또는 변경할 경우,
이 장치를 운용할 수 있는 사용자 권한의 효력을 상실할 수 있습니다.
January 14, 2015, 715004701 Rev. A
Page 35
注意：規制機関か ら 明確な承認 を 受け ず に 本装置の変更や改造 を ⾏ う と 、 本装置の ユ ー
ザ ー と し て の承認が無効 に な る 可能性が あ り ま す。
Warning: Use caution when working with any polymer tubing under pressure:
•
•
•
•
Always wear eye protection when near pressurized polymer tubing.
Extinguish all nearby flames.
Do not use tubing that has been severely stressed or kinked.
Do not use nonmetallic tubing with tetrahydrofuran (THF) or concentrated
nitric or sulfuric acids.
• Be aware that methylene chloride and dimethyl sulfoxide cause nonmetallic
tubing to swell, which greatly reduces the rupture pressure of the tubing.
Attention: Manipulez les tubes en polymère sous pression avec precaution:
• Portez systématiquement des lunettes de protection lorsque vous vous
trouvez à proximité de tubes en polymère pressurisés.
• Eteignez toute flamme se trouvant à proximité de l’instrument.
• Evitez d'utiliser des tubes sévèrement déformés ou endommagés.
• Evitez d'utiliser des tubes non métalliques avec du tétrahydrofurane (THF) ou
de l'acide sulfurique ou nitrique concentré.
• Sachez que le chlorure de méthylène et le diméthylesulfoxyde entraînent le
gonflement des tuyaux non métalliques, ce qui réduit considérablement leur
pression de rupture.
Vorsicht: Bei der Arbeit mit Polymerschläuchen unter Druck ist besondere
Vorsicht angebracht:
• In der Nähe von unter Druck stehenden Polymerschläuchen stets Schutzbrille
tragen.
• Alle offenen Flammen in der Nähe löschen.
• Keine Schläuche verwenden, die stark geknickt oder überbeansprucht sind.
• Nichtmetallische Schläuche nicht für Tetrahydrofuran (THF) oder
konzentrierte Salpeter- oder Schwefelsäure verwenden.
Durch Methylenchlorid und Dimethylsulfoxid können nichtmetallische Schläuche
quellen; dadurch wird der Berstdruck des Schlauches erheblich reduziert.
Attenzione: fare attenzione quando si utilizzano tubi in materiale polimerico
sotto pressione:
• Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero
pressurizzati.
• Spegnere tutte le fiamme vive nell'ambiente circostante.
• Non utilizzare tubi eccessivamente logorati o piegati.
• Non utilizzare tubi non metallici con tetraidrofurano (THF) o acido solforico o
nitrico concentrati.
• Tenere presente che il cloruro di metilene e il dimetilsolfossido provocano
rigonfiamenti nei tubi non metallici, riducendo notevolmente la pressione di
rottura dei tubi stessi.
January 14, 2015, 715004701 Rev. A
Page 36
Advertencia: se recomienda precaución cuando se trabaje con tubos de
polímero sometidos a presión:
• El usuario deberá protegerse siempre los ojos cuando trabaje cerca de tubos
de polímero sometidos a presión.
• Si hubiera alguna llama las proximidades.
• No se debe trabajar con tubos que se hayan doblado o sometido a altas
presiones.
• Es necesario utilizar tubos de metal cuando se trabaje con tetrahidrofurano
(THF) o ácidos nítrico o sulfúrico concentrados.
Hay que tener en cuenta que el cloruro de metileno y el sulfóxido de dimetilo
dilatan los tubos no metálicos, lo que reduce la presión de ruptura de los tubos.
警告：當在有壓力的情況下使用聚合物管線時，小心注意以下幾點。
• 當接近有壓力的聚合物管線時一定要戴防護眼鏡。
• 熄滅附近所有的火焰。
• 不要使用已經被壓癟或嚴重彎曲管線。
• 不要在非金屬管線中使用四氫呋喃或濃硝酸或濃硫酸。
要了解使用二氯甲烷及二甲基亞楓會導致非金屬管線膨脹，大大降低管線的耐壓能力。
警告：当有压力的情况下使用管线时，小心注意以下几点：
• 当接近有压力的聚合物管线时一定要戴防护眼镜。
• 熄灭附近所有的火焰。
• 不要使用已经被压瘪或严重弯曲的管线。
• 不要在非金属管线中使用四氢呋喃或浓硝酸或浓硫酸。
要了解使用二氯甲烷及二甲基亚枫会导致非金属管线膨胀，大大降低管线的耐压能力。
경고: 가압 폴리머 튜브로 작업할 경우에는 주의하십시오.
• 가압 폴리머 튜브 근처에서는 항상 보호 안경을 착용하십시오.
• 근처의 화기를 모두 끄십시오.
• 심하게 변형되거나 꼬인 튜브는 사용하지 마십시오.
• 비금속(Nonmetallic) 튜브를 테트라히드로푸란(Tetrahydrofuran: THF) 또는
농축 질산 또는 황산과 함께 사용하지 마십시오.
염화 메틸렌 (Methylene chloride) 및 디메틸술폭시드 (Dimethyl sulfoxide) 는
비금속 튜브를 부풀려 튜브의 파열 압력을 크게 감소시킬 수 있으므로 유의하십시오 .
警告：圧⼒の か か っ た ポ リ マ ー チ ュ ー ブ を 扱 う と き は、 注意 し て く だ さ い。
• 加圧 さ れ た ポ リ マ ー チ ュ ー ブ の付近で は、 必ず保護 メ ガ ネ を 着用 し て く だ さ い。
• 近 く に あ る 火 を 消 し て く だ さ い。
• 著 し く 変形 し た 、 ま た は折れ曲が っ た チ ュ ー ブ は使用 し な い で く だ さ い。
• 非⾦属 チ ュ ー ブ に は、 テ ト ラ ヒ ド ロ フ ラ ン (THF)や⾼濃度の硝酸 ま た は硫酸な ど を 流 さ
な い で く だ さ い。
塩化 メ チ レ ン や ジ メ チ ル ス ル ホ キ シ ド は、 非⾦属 チ ュ ー ブ の膨張 を 引 き 起 こ す場合が あ
り 、 そ の場合、 チ ュ ー ブ は極め て 低い圧⼒で破裂 し ま す。
Warning: The user shall be made aware that if the equipment is used in a
manner not specified by the manufacturer, the protection provided by the
equipment may be impaired.
Attention: L’utilisateur doit être informé que si le matériel est utilisé d’une
façon non spécifiée par le fabricant, la protection assurée par le matériel risque
d’être défectueuses.
January 14, 2015, 715004701 Rev. A
Page 37
Vorsicht: Der Benutzer wird darauf aufmerksam gemacht, dass bei
unsachgemäßer Verwendung des Gerätes die eingebauten
Sicherheitseinrichtungen unter Umständen nicht ordnungsgemäß funktionieren.
Attenzione: si rende noto all'utente che l'eventuale utilizzo
dell'apparecchiatura secondo modalità non previste dal produttore può
compromettere la protezione offerta dall'apparecchiatura.
Advertencia: el usuario deberá saber que si el equipo se utiliza de forma
distinta a la especificada por el fabricante, las medidas de protección del equipo
podrían ser insuficientes.
警告：使用者必須非常清楚如果設備不是按照製造廠商指定的方式使用，那麼該設備所提供
的保護將被消弱。
警告：使用者必须非常清楚如果设备不是按照制造厂商指定的方式使用，那么该设备所提供
的保护将被削弱。
경고 : 제조업체가 명시하지 않은 방식으로 장비를 사용할 경우 장비가 제공하는 보호 수단
이 제대로 작동하지 않을 수 있다는 점을 사용자에게 반드시 인식시켜야 합니다 .
警告： ユ ー ザ ー は、 製造元 に よ り 指定 さ れ て い な い方法で機器 を 使用す る と 、 機器が提供
し て い る 保証が無効 に な る 可能性が あ る こ と に 注意 し て 下 さ い。
A.6 Warnings that address the replacing of fuses
The following warnings pertain to instruments and devices equipped with
user-replaceable fuses. Information describing fuse types and ratings sometimes, but
not always, appears on the instrument or device.
Finding fuse types and ratings when that information appears on the
instrument or device
Warning: To protect against fire, replace fuses with those of the type and
rating printed on panels adjacent to instrument fuse covers.
Attention: pour éviter tout risque d'incendie, remplacez toujours les fusibles
par d'autres du type et de la puissance indiqués sur le panneau à proximité du
couvercle de la boite à fusible de l'instrument.
Vorsicht: Zum Schutz gegen Feuer die Sicherungen nur mit Sicherungen
ersetzen, deren Typ und Nennwert auf den Tafeln neben den
Sicherungsabdeckungen des Geräts gedruckt sind.
Attenzione: per garantire protezione contro gli incendi, so8stituire i fusibili
con altri dello stesso tipo aventi le caratteristiche indicate sui pannelli adiacenti
alla copertura fusibili dello strumento.
January 14, 2015, 715004701 Rev. A
Page 38
Advertencia: Para evitar incendios, sustituir los fusibles por aquellos del tipo
y características impresos en los paneles adyacentes a las cubiertas de los
fusibles del instrumento.
警告 ：為了避免火災，更換保險絲時，請使用與儀器保險絲蓋旁面板上所印刷之相同類型與
規格的保險絲。
警告：为了避免火灾，应更换与仪器保险丝盖旁边面板上印刷的类型和规格相同的保险丝。
경고 : 화재의 위험을 막으려면 기기 퓨즈 커버에 가까운 패널에 인쇄된 것과 동일한 타입
및 정격의 제품으로 퓨즈를 교체하십시오 .
警告：火災予防の た め に 、 ヒ ュ ー ズ交換で は機器 ヒ ュ ー ズ カ バ ー脇の パ ネ ル に 記載 さ れ て
い る タ イ プ お よ び定格の ヒ ュ ー ズ を ご 使用 く だ さ い。
Finding fuse types and ratings when that information does not appear on the
instrument or device
Warning: To protect against fire, replace fuses with those of the type and
rating indicated in the “Replacing fuses” section of the Maintenance Procedures
chapter.
Attention: pour éviter tout risque d'incendie, remplacez toujours les fusibles
par d'autres du type et de la puissance indiqués dans la rubrique
"Remplacement des fusibles" du chapitre traitant des procédures de
maintenance.
Vorsicht: Zum Schutz gegen Feuer die Sicherungen nur mit Sicherungen
ersetzen, deren Typ und Nennwert im Abschnitt "Sicherungen ersetzen" des
Kapitels "Wartungsverfahren" angegeben sind.
Attenzione: per garantire protezione contro gli incendi, sostituire i fusibili con
altri dello stesso tipo aventi le caratteristiche indicate nel paragrafo
"Sostituzione dei fusibili" del capitolo "Procedure di manutenzione".
Advertencia: Para evitar incendios, sustituir los fusibles por aquellos del tipo
y características indicados en la sección "Sustituir fusibles".
警告 ：為了避免火災，更換保險絲時，應使用 「維護步驟」章節中 「更換保險絲」所指定
之相同類型與規格的保險絲。
警告：为了避免火灾，应更换 “ 维护步骤 ” 一章的 “ 更换保险丝 ” 一节中介绍的相同类
型和规格的保险丝。
경고 : 화재의 위험을 막으려면 유지관리 절차 단원의 “ 퓨즈 교체 ” 절에 설명된 것과 동일
한 타입 및 정격의 제품으로 퓨즈를 교체하십시오 .
警告： 火災予防の た め に 、 ヒ ュ ー ズ交換で は メ ン テ ナ ン ス 項目の 「 ヒ ュ ー ズ の交換」 に 記
載 さ れ て い る タ イ プ お よ び定格の ヒ ュ ー ズ を ご 使用 く だ さ い。
January 14, 2015, 715004701 Rev. A
Page 39
A.7 Electrical and handling symbols
A.7.1 Electrical symbols
The following electrical symbols and their associated statements can appear in
instrument manuals and on an instrument’s front or rear panels.
Symbol
Description
Electrical power on
Electrical power off
Standby
Direct current
Alternating current
Alternating current (3 phase)
Safety ground
Frame, or chassis, terminal
Fuse
Functional ground
Input
Output
January 14, 2015, 715004701 Rev. A
Page 40
A.7.2 Handling symbols
The following handling symbols and their associated statements can appear on labels
affixed to the packaging in which instruments, devices, and component parts are
shipped.
Symbol
Description
Keep upright!
Keep dry!
Fragile!
Use no hooks!
Upper limit of temperature
Lower limit of temperature
Temperature limitation
January 14, 2015, 715004701 Rev. A
Page 41
January 14, 2015, 715004701 Rev. A
Page 42
B
Prosolia DESI Source 2D,
Installation and Operation
Manual
This Appendix contains the Prosolia DESI Source 2D, Installation and Operation
manual. This manual is not a Waters document.
B.1 The Prosolia DESI manual
The Prosolia DESI manual in this appendix is intended for reference purposes only and
is subject to change without notice.
The manual includes the following chapters:
1.
Introduction
2.
Source Assembly
3.
DESI ion source installation
4.
DESI motion control box connections
5.
Operation of DESI source
6.
DESI ion source testing
7.
Source maintenance
8.
Spare parts
9.
Troubleshooting
10. Where to get help
January 14, 2015, 715004701 Rev. A
Page 43
DESI 2D Ion Source Installation and Operation Manual Waters Xevo Mass Spectrometers Prosolia, Inc. 6500 Technology Center Drive Suite 200 Indianapolis, IN 46278 [email protected] PN:P900‐16205‐01 www.prosolia.com Phone: 866‐241‐0239 Phone: 317‐275‐5794 Fax: 317‐873‐3175 Revision A.1 © Prosolia, Inc. 2015 All Rights Reserved. The technical information contained in the DESI 2D Ion Source Installation and Operation Manual is intended for reference purposes only and is 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 user. Prosolia has endeavored to make every reasonable effort to supply complete and accurate information regarding the installation and operation of the DESI 2D system. Prosolia, Inc. makes no representations that this document is complete, accurate, or error‐free and assumes no responsibility for any errors, omissions, damage, or loss that might result from any use of any information contained within this document, even if the information in the document is followed properly. No license or other rights under any patents, copyrights or trademarks owned by Prosolia or under which Prosolia is licensed are granted or implied by the sale of the DESI 2D system. The customer shall not resell or reverse engineer this equipment. Ownership and use of the DESI Ion Source is subject to Prosolia's Standard Terms and Conditions, a copy of which has been provided or is available upon request to Prosolia. TRADEMARKS PEEK is a trademark of Victrex plc. Xevo™, Synapt™, and MassLynx™ are trademarks of Waters Corporation. Swagelok® is a registered trademark of Swagelok Company. Omni Slide™ is a trademark of Prosolia, Inc. i Limited Warranty Prosolia warrants to the Customer and any other end user of the Products manufactured by Prosolia that such Products will be substantially free from defects in material and workmanship when properly installed, maintained and used in conformity with the guidelines provided in the Product’s accompanying documentation. This limited warranty will be in effect for each Product for a period of one (1) year from the date of invoice to the original Customer. This limited warranty excludes the following: (a) parts that are not defective at time of delivery but which become defective by virtue of usage, including but not limited to normal wear, tear and replacement; (b) any damages or problems caused by the failure to properly install, maintain or use the Products; (c) products or parts that have been repaired or altered by anyone other than Prosolia or its authorized agents or affiliates; (d) expendable items including but not limited to capillaries, tubing, fittings, substrates, fuses, o‐rings, belts, gaskets, cartridges, probe tips and chemical standards; (e) products not manufactured by Prosolia; or (f) software products from third parties that are included with the Products or as optional add‐on modules or features ("Third Party Software"). THE FOREGOING WARRANTY IS INTENDED SOLELY FOR THE BENEFIT OF THE FIRST CUSTOMER OF THE PRODUCTS AND IS NON‐ASSIGNABLE. PROSOLIA SPECIFICALLY DISCLAIMS ALL OTHER WARRANTIES, EXPRESS OR IMPLIED INCLUDING, BUT NOT LIMITED TO, ANY IMPLIED WARRANTY OF MERCHANTABILITY, ANY IMPLIED WARRANTY OF FITNESS FOR A PARTICULAR PURPOSE, AND ANY WARRANTY OF TITLE AND AGAINST INFRINGEMENT. PROSOLIA AND ITS LICENSORS AND THEIR SUPPLIERS DO NOT WARRANT THAT THE PRODUCTS ARE OR WILL BE ERROR OR BUG FREE, OR THAT CUSTOMER'S USE OF THE PRODUCTS WILL BE UNINTERRUPTED. PROSOLIA AND ITS LICENSORS AND THEIR SUPPLIERS ASSUME NO RESPONSIBILITY FOR THE PROPER INSTALLATION AND USE OF THE PRODUCTS OR ANY THIRD PARTY PRODUCT OR SYSTEM. PROSOLIA AND ITS LICENSORS AND THEIR SUPPLIERS MAKE NO REPRESENTATIONS ABOUT ANY DATA, RESULTS OR INFORMATION PRODUCED OR MADE ACCESSIBLE BY THE PRODUCTS. SOME JURISDICTIONS DO NOT ALLOW THE EXCLUSION OF IMPLIED WARRANTIES, SO THE ABOVE EXCLUSION MAY NOT APPLY TO CUSTOMER. IN THAT EVENT, TO THE EXTENT PERMISSIBLE, ANY IMPLIED WARRANTIES ARE LIMITED IN DURATION TO THIRTY (30) DAYS FROM THE DATE OF FIRST SALE OF THE PRODUCTS. The foregoing limited warranty shall be qualified by and subject to the standard terms and conditions applicable to the purchase of the Product. In the event of a claim under the foregoing limited warranty, Prosolia's exclusive liability shall be the repair or replacement, at Prosolia's option, of any defective systems or parts which Prosolia can confirm are defective and are covered by the warranty. Customer shall be responsible for any shipping expenses relating to repairs and replacements. All repairs and replacements that are not covered by the limited warranty in Section 3 above are subject to Prosolia’s standard labor and materials charges. Customer must notify Prosolia in writing of any claim regarding shortages, defective or nonconforming products or parts within 30 days after such defect or nonconformity is or should have been discovered by Customer. If Customer fails to notify Prosolia timely of a claim, the Products shall be deemed accepted by Customer without objection and any such claim by Customer shall be waived. Customer is responsible for decontamination of the part(s) or product(s) and providing factual evidence that the part(s) or product(s) are free from contamination prior to replacement or repair of the defective part(s) or product(s). Customer is responsible for all such expenses related to decontamination of the part(s) or product(s). If the part(s) or product(s) cannot be made free from contamination, then the limited warranty is void. Prosolia will not accept under any circumstances, any item that has been exposed to radioactivity or is microbiologically contaminated. THE REMEDIES PROVIDED TO CUSTOMER HEREIN SHALL BE THE SOLE AND EXCLUSIVE REMEDIES OF CUSTOMER AND CUSTOMER HEREBY WAIVES ALL OTHER REMEDIES PROVIDED BY APPLICABLE LAW OR EQUITY, INCLUDING WITHOUT LIMITATION, INDIRECT, INCIDENTAL, CONSEQUENTIAL, LIQUIDATED, PUNITIVE OR ANY OTHER DAMAGES. PROSOLIA SHALL NOT BE LIABLE TO CUSTOMER FOR ANY LOST PROFITS, ANY INDIRECT, INCIDENTAL, CONSEQUENTIAL, SPECIAL OR SIMILAR DAMAGES (INCLUDING LOSS OF CARGO), OR ANY CLAIMS OR DEMANDS BROUGHT BY OR AGAINST CUSTOMER, HOWEVER CAUSED AND UNDER ANY THEORY OF LIABILITY. IN NO EVENT SHALL PROSOLIA'S AGGREGATE LIABILITY TO CUSTOMER ARISING OUT OF, RELATED TO OR IN CONNECTION WITH THE SALE OF ANY PRODUCTS UNDER THIS AGREEMENT EXCEED THE PURCHASE PRICE PAID TO PROSOLIA BY CUSTOMER FOR SUCH PRODUCTS. Customer acknowledges that the use of any Third Party Software may be subject to additional end user license agreements (each a "EULA") and agrees to execute and comply with the terms of any such EULA. EULAs may be contained as a click‐through agreement during the installation of Third Party Software or in executable form. The use of any Third Party Software shall evidence Customer's acceptance of the terms of the related EULA. Customer can receive the specific terms of any EULA upon request from Prosolia. Notwithstanding the provisions of Section 4 to the contrary, Prosolia disclaims any warranty for Third Party Software, and the only warranties that shall apply to Third Party Software shall be those, if any, which are set forth in the applicable EULA.
ii Notice of Intended Use The DESI 2D system should be used for research purposes only and only in an indoor laboratory environment. The DESI 2D system must not be used in human experimentation or applied to living humans in any way. The DESI 2D system is not a medical device. Notice of Proper Use of Prosolia Instruments If this instrument is used in a manner not specified by Prosolia, the protections provided by the instrument could be impaired. Any changes or modifications made to the instrument may void compliance with one or more safety and/or electromagnetic compatibility standards. All replacement parts should be purchased directly from Prosolia or its authorized representatives. Any necessary repairs should be performed only by authorized Prosolia personnel or their affiliates. Notice on Handling and Lifting of Prosolia Instruments The DESI 2D system is a precision scientific instrument and should be handled with care. While no special precautions are necessary while transporting the equipment, dropping or other rough handling should be avoided. If dropped or other rough handling is suspected, please contact Prosolia for further information. End users should retain all packaging materials for the DESI 2D system in the event the instrument must be returned to Prosolia for repair. The user is responsible for adequately packaging and the safe transport of the system to the repair depot. The DESI 2D system has been designed and is intended to be installed by a single person. For your safety, DO NOT attempt to lift the DESI 2D system by the cover handles. Only lift the system after removing the cover and by firmly grasping the sides of the 2D stage or instrument mounting flange. If you are unable to safely lift 20 lbs (9 kg), obtain the help of a second person before attempting to lift or install the DESI 2D system. Notice on the Use of Accessory Devices with Prosolia Instruments The DESI 2D system should only be used with accessories specified and provided by Prosolia and its authorized representatives. Do not use any other accessory device or consumable components with the DESI 2D system. Use with unauthorized accessories may void compliance with one or more safety and/or electromagnetic compatibility standards.
iii Explanation of Warning Symbols Electric Shock: This instrument uses high voltages that can cause personal injury. Before servicing, shut down the instrument and disconnect the instrument from line power. Do not use the instrument without its protective enclosure. Choc électrique: L’instrument utilise des tensions capables d’infliger des blessures corporelles. L’instrument doit être arrêté et débranché de la source de courant avant tout intervention. Ne pas utiliser l'instrument sans son boîtier de protection. Heat: Surfaces/components present at high temperatures. Allow heated components on the instrument to cool before servicing. Haute Temperature: Surfaces/composants présents à des températures élevées. Laissez les composants chauds sur l'instrument refroidir avant l'entretien. Chemical Hazard: This instrument may contain hazardous chemicals. Wear gloves when handling toxic, carcinogenic, mutagenic, or corrosive or irritant chemicals. Use approved containers and proper procedures for disposal of waste. Decontaminate the system before service. Danger Chimique: Cet instrument peut contenir des produits chimiques. Portez des gants pour manipuler produits chimiques toxiques, cancérigènes, mutagènes, ou corrosifs/irritants. Utiliser des récipients et des procédures appropriés pour l'élimination des déchets. Décontaminez le système avant l’utilisation. Biohazard: Use of this instrument with biological samples may present a biohazard to the user. Always wear appropriate personal protective equipment when using biohazardous substances and follow your institutions Biological Safety Manual. Biohazard: Utilisation de cet instrument avec des échantillons biologiques peut présenter un danger biologique à l'utilisateur. Porter toujours un équipement de protection individuelle approprié en utilisant des substances biologiques dangereuses et suivre le manuel de sécurité biologique de votre institution. iv Eye Hazard: Eye damage could occur from splattered chemicals or flying particles. Wear safety glasses when handling chemicals or servicing the instrument. Danger pour les yeux: Des projections d’agents chimiques, liquides, ou solides peuvent être dangereuses pour les yeux. Portez des lunettes de protection lors de l’utilisation. Pinch Hazard: This instrument contains automated, motor driven components. Avoid contact with moving parts. Pincez danger: Danger de pincement: Cet instrument contient des composants, motorisés automatisés. Eviter le contact avec les pièces mobiles. General Hazard: A hazard is present that is not included in the above categories. Also, this symbol appears on the instrument to refer the user to instructions in this manual. Danger général: Indique la présence d’un risque n’appartenant pas aux catégories citées plus haut. Ce symbole figure également sur l’instrument pour renvoyer l’utilisateur aux instructions du présent manuel. When the safety of a procedure is questionable or unclear, contact Prosolia. Contact information can be found at www.prosolia.com. v Precautions for Use The interface components of the mass spectrometer are heated to very high temperatures. Allow the interface region to cool before installing or removing the DESI 2D. Les composants d’interface avec l’appareil de spectrométrie de masse sont chauffés a très hautes températures. Laissez refroidir les composants d’interface avant d’installer ou retirer le DESI 2D. This equipment may be used with substances that present chemical and/or biological hazards. Wear appropriate personal protective equipment while operating and servicing the system. Cet appareil peut être utilise avec de dangereux agents chimiques ou biologiques. Utilisez des protections individuelles appropriées lors de l’utilisation ou services de l’appareil. Systems that are contaminated with biological, carcinogenic, mutagenic, corrosive, toxic, or irritant hazards must be decontaminated before servicing. Décontaminez avant utilisation tous les composants contaminés avec des produits chimiques toxiques, cancérigènes, mutagènes, ou corrosifs/irritants. To reduce the risk of exposure to hazards, ensure the mass spectrometer is connected to an exhaust system. Pour reduire le risque d’exposition, connectez l’appareil de spectrométrie de masse à un système de d’échappement. This instrument uses high voltages that can cause personal injury. Before servicing, shut down the instrument and disconnect the instrument from line power. Do not use the instrument without its protective enclosure. L’instrument utilise des tensions capables d’infliger des blessures corporelles. L’instrument doit être arrêté et débranché de la source de courant avant tout intervention. Ne pas utiliser l'instrument sans son boîtier de protection. vi To maintain compliance with international safety standards, the electrospray high voltage used with the DESI 2D system must only be supplied from a mass spectrometer with a power supply whose output does not exceed non‐hazardous limits established by IEC 61010‐1, clauses 6.3.1 and 6.3.2, as well as the rated input voltage. Use with higher output currents is unsafe and may lead to electrical shock or injury. Pour maintenir la conformité avec les normes internationales de surété, au sujet de l’électrospray haute tension utilisée avec le système DESI 2D, n’utiliser qu’une source de courant qui vient d’un spectromètre de masse duquel la sortie correspond aux limites non‐hasardeuses établies par IEC 61010‐1, clauses 6.3.1 et 6.3.2, aussi bien que la tension indiquée. Si on utilise une source de courant avec une sortie électrique plus haute, on risque le choc électrique et la blessure. Moving components are exposed during use and service. Avoid contact with all moving parts. Les pièces mobiles sont exposées lors de l’utilisation et du service. Évitez tout contact avec les pièces mobiles. Do not use this system in a manner inconsistent with its intended use. Ne pas utiliser l’appareil d’une manière incompatible avec son utilisation prévue. Read and understand all instructions before using the system. Instructions doivent être lues et comprises avant l‘utilisation de l’appareil. Maintenance and test procedures should only be performed by trained and qualified individuals. La maintenance et les tests de procédures doivent être effectués par un personnel de maintenance qualifié vii Safety Considerations The use of some solvents, reagents, and samples with the DESI 2D system can pose chemical and biological hazards to the user. Users must know and assess the potential hazards associated with all substances and samples used with the DESI system. Users must be trained to evaluate and identify these hazards and in the proper identification, use, and disposal of personal protective equipment (PPE) used to mitigate these hazards. Training for chemical and biological hazards and for proper selection and use of PPE is obtained from your Organization/Institution’s safety representative(s). This manual contains many safety and special notices. Make sure that you read, understand, and follow the precautionary statements contained within this manual. viii Table of Contents Limited Warranty .................................................................................................................... ii Notice of Intended Use ........................................................................................................... iii Notice of Proper Use of Prosolia Instruments ......................................................................... iii Notice on Handling and Lifting of Prosolia Instruments .......................................................... iii Notice on the Use of Accessory Devices with Prosolia Instruments ........................................ iii Explanation of Warning Symbols ............................................................................................ iv Precautions for Use ................................................................................................................ vi Safety Considerations ............................................................................................................ viii Table of Contents ....................................................................................................................ix Preface .................................................................................................................................... 1 Contacting Prosolia .................................................................................................................. 2 1. Introduction ........................................................................................................................ 3 1.1 Key References ................................................................................................................................... 4 2. System Components ........................................................................................................... 5 3 DESI 2D System Specifications and Overview ....................................................................... 6 3.1 Specifications ..................................................................................................................................... 6 3.2 DESI 2D System Overview .................................................................................................................. 7 General Operation .................................................................................................................................... 7 System Components ................................................................................................................................. 8 4 DESI 2D System Pre‐Installation Requirements .................................................................. 11 4.1 Line Power ........................................................................................................................................ 11 4.2 Solvents ............................................................................................................................................ 12 4.3 Gases ................................................................................................................................................ 12 4.4 Mass Spectrometer .......................................................................................................................... 13 4.5 Exhaust ............................................................................................................................................. 13 5 DESI 2D System Assembly .................................................................................................. 14 5.1 Camera Installation ........................................................................................................................... 14 5.2 Camera/Lamp Adjustment ................................................................................................................ 16 5.3 Spray Head Assembly ........................................................................................................................ 17 5.4 Gas Connections ................................................................................................................................ 24 5.5 Cable and Tubing Routing ................................................................................................................. 26 6 DESI 2D System Installation ................................................................................................ 27 6.1 Preparation of Waters Xevo Mass Spectrometers ............................................................................ 27 6.2 Mounting the DESI 2D System .......................................................................................................... 28 ix 6.3 Ion Transfer Capillary Installation ..................................................................................................... 32 6.4 Installation of the DESI 2D System Cover and Exhaust Line ............................................................. 34 6.5 Removal and Storage of the DESI 2D system .................................................................................... 38 7 Electrical Connections ......................................................................................................... 39 7.1 Electrical Mains Connection .............................................................................................................. 39 7.2 Rear Panel Connections .................................................................................................................... 40 7.3 Front Panel Connections ................................................................................................................... 42 7.4 I/O (Trigger) Cable Connection ......................................................................................................... 43 8 Operation of the DESI 2D System ....................................................................................... 44 8.1 Spray Head Manipulators .................................................................................................................. 44 8.2 Motion of the X and Y Stages ............................................................................................................ 45 8.3 Manual Positioning of the Sample Stage Z Axis ................................................................................ 47 8.4 Spray Head Arm ................................................................................................................................ 47 8.5 High Voltage Interlock ....................................................................................................................... 48 8.6 Slide Holder Operation ...................................................................................................................... 50 8.7 Automating Data Collection with MassLynx™ .................................................................................. 51 9 DESI 2D System Testing ....................................................................................................... 56 9.1 General Operating Parameters ......................................................................................................... 56 9.2 Standards Preparation ...................................................................................................................... 57 9.3 Preparing and Using the Omni Slide for Analysis .............................................................................. 58 9.4 Testing ............................................................................................................................................... 61 9.5 Additional Experimental Examples ................................................................................................... 65 10 Maintenance .................................................................................................................... 70 10.1 General Cleaning ............................................................................................................................. 70 10.2 Preventative Maintenance .............................................................................................................. 71 10.3 Spray Head Nozzle/Emitter Replacement ....................................................................................... 71 10.4 Spray Head Cleaning ....................................................................................................................... 75 10.5 Extended Transfer Capillary Cleaning ............................................................................................. 80 10.6 Fuse Replacement ........................................................................................................................... 81 10.7 Decommissioning and Disposal ....................................................................................................... 82 11 Replacement Parts ............................................................................................................ 83 12 Troubleshooting ............................................................................................................... 86 Hardware Errors ...................................................................................................................................... 86 Communications Errors ........................................................................................................................... 87 Experimental Errors ................................................................................................................................ 87 x Preface This manual describes the installation, operation, and maintenance of the DESI 2D system on Waters Corporation mass spectrometers featuring the Xevo ion source and interface. This manual contains many safety and special notices. Make sure that you read, understand, and follow the precautionary statements contained within this manual. Safety and special notices appearing throughout the manual use the following conventions: CAUTION Highlights hazards to humans, property, or the environment. Each CAUTION notice is accompanied by an appropriate CAUTION symbol. ATTENTION Le symbole CAUTION/ATTENTION indique une situation potentiellement dangereuse pour l’utilisateur, les biens ou environnent. Chaque CAUTION/ ATTENTION sont accompagnés d’un symbole d’alerte pour reconnaitre la nature du danger potentiel. IMPORTANT Highlights information necessary for proper operation of the system. NOTE Highlights general information of interest to the user. TIP Highlights helpful information that can make a task easier to perform. 1 Contacting Prosolia There are several ways to reach Prosolia. Our standard business hours are from 8 AM to 5 PM Eastern Standard Time, Monday through Friday. General Inquires/Ordering Information Phone 866‐241‐0239 or 317‐275‐5794 Fax 317‐873‐3175 E‐mail [email protected] Web www.prosolia.com Technical Support Phone 866‐241‐0239 or 317‐275‐5794 Fax 317‐873‐3175 E‐mail [email protected] Web www.prosolia.com
2 1. Introduction The DESI 2D system has been designed to give you the full advantage of the Desorption Electrospray Ionization (DESI) technology originally invented in the laboratory of Prof. R. Graham Cooks at Purdue University. This manual contains the installation and operating instructions for the DESI 2D System with automated sample positioning that is compatible with the Waters mass spectrometers with the Xevo atmospheric pressure interface. The DESI 2D system is simple to operate. It eliminates the need for complex and time consuming sample preparation allowing for faster results. Desorption Electrospray Ionization (DESI) technology* was first reported by Prof. Cooks’ group in Science (2004, 306, 471‐473). DESI is a pneumatically assisted electrospray technique that directs an appropriate solvent mixture towards the sample of interest and the resultant ions are sampled directly into the mass analyzer, as shown below, all under ambient conditions. The contents of the solvent spray, the gas flow rate, the amount of applied voltage, the spray angle and the ion uptake angle, as well as the various distances in aligning the spray, sample and mass spectrometer are all variables which can be studied to achieve an optimal mass spectrum for a particular type of sample. ILLUSTRATION OF DESORPTION ELECTROSPRAY IONIZATION solvent
N2
H
spray emitter
inlet of mass
spectrometer
spray
desorbed
ions
spray nozzle
sample
freely moving sample stage
DESI has been demonstrated in a wide range of applications from the detection of explosives to proteomics. References for reviews on this exciting technology are listed below. An expanded publications list related to DESI is available on our website, www.prosolia.com We hope you enjoy the DESI 2D experience. *US Patent 7,335,897 3 1.1 Key References Takats, Z.; Wiseman, J. M.; Gologan, B.; Cooks, R. G., Mass Spectrometry Sampling Under Ambient Conditions with Desorption Electrospray Ionization. Science 2004, 306, 471‐473. Takats, Z.; Wiseman, J. M.; Cooks, R. G., Ambient Mass Spectrometry using Desorption Electrospray Ionization (DESI): Instrumentation, Mechanisms and Applications in Forensics, Chemistry, and Biology. J. Mass Spectrom. 2005, 40, (10), 1261‐1275. Cooks, R. G.; Ouyang, Z.; Takats, Z.; Wiseman, J. M.; Ambient Mass Spectrometry. Science 2006, 311, 1566‐1570. Omni Spray Ion Source 2‐D Automation Software Installation and Reference Manual
4 2. System Components The DESI 2D system is shipped to the user packaged in several boxes, the contents of which will vary based on the compatible mass spectrometer. Each system is configured with the following components: 






DESI 2D system compatible with Waters mass spectrometers DESI 2D system installation and accessory kit DESI spray head kit DESI 2D electronics kit Region specific mains power cord Mass spectrometer I/O cable Instruction manua
5 3 DESI 2D System Specifications and Overview The DESI 2D system has been designed to be operated in a normal laboratory environment. Details of the specifications can be found in later sections of this manual. For software specifications, please refer to the Omni Spray Ion Source 2D Automation Software Installation and Reference Manual. 3.1 Specifications Physical DESI 2D System Size ‐ H 218mm (8.6”) x W 358.5mm (14.1”) x D 279.5mm (11.0”) Weight – Approximately 8 kg (17.6 lbs) Control Electronics Size ‐ H 181mm (7.2”) x W 184mm (7.25”) x D 58mm (2.3”) Weight – Approximately 1.5 kg (3.3 lbs) Environmental Temperature – 5‐40°C (41 ‐ 104 °F), Optimum Operating 15‐30°C (59 ‐ 86°F). Relative Humidity – 20‐80% with no condensation Altitude – Sea level to 3000m Environment – Indoor laboratory environment, no direct sunlight Electrical DESI 2D System – 24 VDC ±10%, 3A Max AC/DC Power Supply – Input: 100‐240 VAC ±10%, ~2A , 50/60 Hz, Output: 24VDC, 2.5A, 60W Spray HV input* – ±8kVDC , 100 µA Max 6 *CAUTION To maintain compliance with international safety standards, the electrospray high voltage used with the DESI 2D system must only be supplied from a mass spectrometer with a power supply whose output does not exceed non‐
hazardous limits established by IEC/EN/UL 61010‐1, clauses 6.3.1 and 6.3.2, as well as the rated input voltage. Use with higher output currents is unsafe and may lead to electrical shock or injury. ATTENTION Pour maintenir la conformité avec les normes internationales de surété, au sujet de l’électrospray haute tension utilisée avec le système DESI 2D, n’utiliser qu’une source de courant qui vient d’un spectromètre de masse duquel la sortie correspond aux limites non‐hasardeuses établies par IEC/EN/UL 61010‐1, clauses 6.3.1 et 6.3.2, aussi bien que la tension indiquée. Si on utilise une source de courant avec une sortie électrique plus haute, on risque le choc électrique et la blessure. 3.2 DESI 2D System Overview The following section provides an overview of the system to acquaint the user with the features of the DESI 2D system for Waters Xevo mass spectrometers. General Operation The DESI 2D system is an automated surface sampling and ionization source for mass spectrometry featuring desorption electrospray ionization technology. In DESI, ions are generated from a sample situated on a surface by way of bombardment with high velocity, charged micro‐droplets. The spray impact at the surface causes the formation of microscopic liquid layers on the sample surface into which analyte dissolve. Desorption of micron‐sized droplets containing dissolved analyte occurs via momentum transfer when additional droplets from the spray collide with the liquid layer forcing the desorbed droplets into the gas phase. These droplets are sampled by the sampling aperture of the mass spectrometer for analysis. The DESI 2D system is controlled using Prosolia’s Omni Spray 2D Motion Control Software, operating on the mass spectrometer’s data system computer. The software communicates to the DESI control electronics though USB and is responsible for the control of the 2D sample stage in manual and automated movement modes. Automated sample analysis experiments, such as surface imaging, are programmed into the motion control software along with the appropriate sample sequence in the mass spectrometer software. The DESI 2D system triggers data acquisition on the mass spectrometer in synchronization with the progress of the DESI experiment. 7 System Components The following figures describe the location of major components of the OS‐6205 DESI 2D system which are referenced throughout this manual. In these figures, wiring and tubing has been removed for clarity. Instrument Mounting Flange Each DESI 2D system is designed to closely couple to compatible mass spectrometers through as integrated mounting flange which supports the 2D stage, positioning manipulators for the DESI spray head, a camera for visualizing the sprayer/inlet region, and a safety enclosure to prevent access to hazards during operation. Figure 3.2.1 shows the instrument mounting flange and three (3) mounting fasteners. Instruction for mounting the DESI 2D system to the mass spectrometer are found in Section 6 of this manual. Figure 3.2.1 Instrument mounting flange showing the three (3) mounting fasteners 2D Sample Stage The 2D sample stage is automated for positioning sample plates relative to the inlet of the mass spectrometer for analysis. Mounted to the 2D stage is a sample plate holder, capable of carrying one (1) microtiter footprint slide or two (2) 76 x 26 mm glass microscope slides. The stage features and over all travel of 120 x 80 mm and performs several automated scan types through the Omni Spray 2D Motion Control Software. Details on the operation of the stage are found in the Motion Control software manual and in Section 8.2. 8 Figure3.2.2 2D Sample stage and sample plate holder Spray Head Manipulator The DESI spray head is mounted into the manipulator assembly allowing for the spray tip to be positioned in three axes and rotationally relative to the sample surface and mass spectrometer inlet. Figure 3.3.3 shows the rotational manipulator assembly and Section 8.1 describes its use. Figure 3.3.3 Illustration of the spray head rotational/linear manipulators for adjusting the spray emitter position. 9 System Enclosure The DESI 2D system for Waters Xevo mass spectrometers includes a system cover to prevent access to the system components will in operation and the help shield users from solvent vapors and sample aerosols when connected to a proper exhaust system. Details of the enclosure are given in Sections 6.4 and 8.5. Figure 3.2.4 OS‐6205 DESI 2D system with the system enclosure in place 10 4 DESI 2D System Pre‐Installation Requirements The DESI 2D system has minimal requirements for operation and use. This section details these requirements which must be met before installation can begin: 4.1 Line Power The DESI 2D system includes an AC/DC power supply with a wide ranging input that will operate worldwide. The DESI 2D system requires one (1) outlet near the mass spectrometer for operation. The line voltage should be free from fluctuations, surges, sags, and transients in voltage Mains Power: 100‐240 VAC, ~2A, 50/60 Hz When installing the equipment, position the unit such that the unit can easily be unplugged from the mains voltage (outlet) in an emergency. CAUTION For safety compliance, the outlet must be connected to Earth ground. ATTENTION Conformément aux mesures de sécurité générales, la prise électrique doit être connectée et mise a la terre. CAUTION Use only the original power supply provided with the system. ATTENTION L’appareil doit uniquement être utilisé a partir d’une source d’énergie qui remplitles spécifications mentionnées sur l’étiquette de puissance électrique du produit
CAUTION Do not replace the mains supply cord with one of inadequate rating. ATTENTION Ne remplacez pas les cordes électriques avec un matériel non agrée et de différentes caractéristiques. 11 Country Plug Type USA/Canada NEMA 5‐15P United Kingdom BS 1363 Diagram Europe CEE 7/7 Australia AS 3112 Switzerland SEV 1011 China GB 2099 Note: Authorized distributors may supply additional power cord types as required Table 4.1.1 List of mains power cords supplied with the DESI 2D System 4.2 Solvents The DESI 2D system requires the use of HPLC grade solvents and modifiers for best performance. Solvents and reagents used should be free from impurities. Solvents are delivered to the DESI 2D System at flow rates between 1 and 5 L/min. The solvent delivery system (typically a syringe pump) used with the DESI 2D system should be free from pulsation at the above flow rates. If you do not have a suitable solvent delivery pump, recommended syringe pumps can be purchased directly from Prosolia. Please contact for more information. 4.3 Gases A high pressure nitrogen gas source is required for the operation of the DESI 2D System. This nitrogen gas is used to aid in the formation of the DESI spray and direct the droplets produced towards the sample surface. A regulated, high pressure nitrogen source must be provided with a variable pressure between 80‐150 PSI (5.5‐10.3 bar), and preferably variably between 80‐200 PSI (5.5‐13.8 bar). The nitrogen gas should be free from contamination and at a recommended purity of 99.999%. The DESI 2D System features a ¼ inch, Swagelok® compression fitting for the nebulizing gas input. Due to the varying length of tubing necessary for each installation, the tubing has not been provided with the ion source. Recommended tubing for this connection is 12 th
¼ inch outer diameter PFA tubing (1/8 inch inner diameter), available from suppliers such as Swagelok, Upchurch Scientific, McMaster‐Carr, and others. Ensure that the ¼ inch tubing used to make the connection between your high pressure nitrogen source and the DESI 2D System is rated to a working pressure of at least 250 PSI. 4.4 Mass Spectrometer The DESI 2D system is designed and engineered to be compatible with certain models of mass spectrometer. The components of the DESI 2D system are provided for specific mass spectrometers based on customer requirements. The DESI 2D system shall only be used on systems which are deemed compatible by Prosolia. Use on non‐compatible mass spectrometers is not supported and may present the user with safety hazards not anticipated in the design and engineering of the system. Compatible mass spectrometers should be installed, tuned, and calibrated according to the manufacturer’s instructions for best performance. Any required ventilation for the mass spectrometer vacuum pumps and ionization source must be installed according to the mass spectrometer manufacturer’s requirements. The instruments shall be in good repair and free from defects or modifications. Use on mass spectrometers that have been modified is not supported and may present the user with safety hazards not anticipated in the design and engineering of the system. 4.5 Exhaust The DESI 2D system is an atmospheric pressure ionization source which creates an aerosol of spray solvents and samples during analysis Although the volumes of solvent and sample consumed during this process is small, there is the potential for aerosol/vapors to escape and thus the users must be aware of the potential chemical hazards. Each laboratory and user MUST assess the hazards and risks associated with the spray solvents and samples in use in their laboratory environment during use and employ appropriate PPE if hazards warrant its use. The DESI 2D system is designed to be connected to a local exhaust ventilation system during operation. The user must provide a proper, negative pressure exhaust system with a minimum vacuum of 5 mbar below atmospheric pressure. Connection to the exhaust system is detailed in Section 6.4 13 5 DESI 2D System Assembly Prior to the installation of your new DESI 2D system onto your mass spectrometer, some simple assembly is required. All of the tools necessary for the assembly of the DESI system have been included with the system kits. The directions in this section will acquaint users with the DESI 2D system and explain how to assemble the system for use. Items not included in the kit, which are necessary for the operation of the ion source, include a high pressure nitrogen source that can be regulated between 80‐200 psig and high purity solvents. The requirements for these items are discussed in following sections of this manual. Figure 5.1 DESI 2D system kit for the Waters mass spectrometers with the Xevo interface. (Note: all parts not shown) 5.1 Camera Installation The DESI 2D system is equipped with a single video camera and LED lamp to assist in the positioning and monitoring of the spray and surface. Both the camera and LED lamp are attached to the spray head arm. The camera assembly is located in the electronics accessory kit and will not be attached to the ion source when shipped. The LED light will be in place on the system when shipped from Prosolia. 14 Camera Clamp
LED Light
Figure 5.1.1 DESI 2D system camera clamp and LED light locations The camera is equipped with a mirror to capture images at a 90˚ angle to the body of the camera. Follow the steps below to install the camera and as shown in Figure 5.2.2 1. Open up the camera clamp by loosening the clamp screw. 2. Insert the camera from the back of the clamp loop with the mirror of the camera entering the clamp first. You may need to gently pull on the upper portion of the camera clamp to allow the camera body to slide freely. 3. Turn the camera housing until the mirror is pointing down towards the surface. 4. Tighten the clamp screw to secure the camera in place. NOTE To obtain a video picture with the proper orientation, it may be necessary to make small adjustments to the mirror rotation relative to the camera body. To make this adjustment, loosen or tighten the threaded lens assembly slightly. 15 Tighten Screw
Insert Camera
Figure 5.1.2 Installation of the camera to view the sample surface 5.2 Camera/Lamp Adjustment The camera and LED light will need to be adjusted once the system is mounted and running on the mass spectrometer. Changes in camera position is made by loosening the clamp screw, moving the camera horizontally within the clamp, and retightening the clamp screw. The camera should be adjusted to look straight down towards the sample surface so that the spray head tip, capillary inlet, and sample surface can be seen within the same image. Focus on the camera is achieved by adjusting the camera height relative to the surface. The camera height is changed my turning the adjustment knob as shown in Figure 5.2.1. The focal length of the cameras is approximately 7 cm. The LED lamp can also be adjusted by pivoting the lamp using the adjustment lever. 16 Camera Adjustment
Knob
Light Adjustment
Lever
Figure 5.2.1 Location of the camera adjustment knob on the spray head arm 5.3 Spray Head Assembly The spray head of the DESI 2D system comes preloaded with a fused silica emitter. Before using the system, the length of the emitter which protrudes from the nozzle must be adjusted by turning the nozzle clockwise using the 4 mm wrench provided with your component kit (see section 10.3 for further details). The emitter should protrude approximately 1mm beyond the tip of the spray nozzle. Figure 5.3.1 Adjustment of the emitter protrusion using a 4 mm wrench Connections for both the spray solvent and nitrogen nebulizing gas must be made to the spray head. The tubing and fittings necessary to make these connections have been provided with your DESI 2D system. 17 Solvent
connection
Neubulizer gas
connection
HV connection
Figure 5.3.2 Connections made to the DESI spray head Figure 5.3.3 Exploded view of DESI spray head Spray head solvent connection: 1. Remove Microtight nut and ferrule from the rear port of the spray head. 2. Insert yellow Microtight sleeve (P300‐00004‐01) through the ferrule so that it protrudes approximately 4 mm from the point of the ferrule 3. Slide nut over the provided fused silica tubing (part number P300‐00011‐99) followed by carefully inserting the fused silica through the sleeve 4. Using a capillary cleaving tool, cut ~1 cm of the fused silica tubing to ensure the end is cut square and free of debris 5. Pull the fused silica back through the sleeve such that the ends are flush 6. Insert the ferrule/sleeve/fused silica into the port of the spray head tee. They should bottom out in the tee and automatically set the depth within the tee 7. Tighten nut over threads to secure the connection The liquid path through the spray head includes a grounded union to prevent the high voltage applied to the spray head from reaching the syringe. The stainless steel union which makes the liquid junction for the ground point is attached to the system via a holder under the 2‐D platform. The union can be snapped in place by placing it at the opening of the holder and pushing into the slot. The union will be held in place when seated completely into the holder. To remove, simply push the union downwards from the holder. 18 CAUTION To avoid a possible static like shock, always place the grounding union into the holder. Do not handle the grounding union while the instrument is in Operate Mode. ATTENTION Pour éviter un choc statique semblable, placez toujours l'union de la terre dans le support. Ne manipulez pas l'union de la terre lorsque l'appareil est en Mode d'exploitation. Gas Manifold and
Shut-off Valve
Grounding Union
Holder
Figure 5.3.4 Location of grounding union under the system’s 2‐D platform The free end of the fused silica capillary is connected to the grounding union. To make this connection: 1. Insert a 1/16th inch PEEK ferrule (P300‐00017‐02) into a red fingertight nut (P300‐00016‐01) 2. Insert 1/16th inch yellow sleeve (P300‐00018‐01) through the nut/ferrule so that it protrudes approximately 4 mm from the point of the ferrule 3. Using a capillary cleaving tool, cut the fused silica tubing to length. Ensure the tubing will reach the grounding union holder and will have sufficient length to allow the spray head and manipulator to move through their entire range of motion 4. Carefully insert the end of the fused silica solvent tubing through the 1/16th inch yellow sleeve 5. Again, using a capillary cleaving tool, cut ~1 cm of the fused silica tubing to ensure the end is cut square and free of debris 6. Pull the fused silica back through the sleeve such that the ends are flush 7. Insert this assembly into an open end of the stainless steel union (P300‐00015‐01) and tighten firmly 19 The connection between the grounding union and the syringe is made using 1/32nd inch PEEK tubing for ruggedness. The first connection to make with the 1/32nd inch PEEK tubing is to the grounding union. 1. Insert a 1/32nd inch PEEK ferrule (P300‐00029‐01) into a red finger tight nut 2. Insert one end of the 1/32nd inch PEEK tubing (P300‐00047‐01) through the nut/ferrule so that it protrudes approximately 4 mm from the point of the ferrule 3. Insert this assembly into an open end of the stainless steel union and tighten firmly Fused Silica
SS union adapter
Ferrules
1/32” PEEK tubing
Figure 5.3.5 Syringe adapter connections for solvent delivery to the DESI spray head Finally, the opposite end of the 1/32nd inch PEEK tubing is connected to the syringe though the adapter union. To make this connection: 1. Insert the gauge plug provided with the adapter union (P300‐00030‐01) into the union and gently tighten into place 2. Cut the PEEK tubing to the appropriate length to reach the syringe pump 3. Carefully insert the end of the 1/32nd inch PEEK through the smaller threaded fitting so that it protrudes approximately 4 mm from the tip 4. Insert this assembly into the open end of the adapter union and tighten firmly 5. Remove the gauge plug from the larger end of the adapter union 6. Insert the short length of Teflon tubing supplied with the system (P300‐00013‐01) into the larger threaded fitting leaving approximately 4 mm protruding from the tip 7. Insert this assembly into the open end of the adapter union and tighten until snug 8. Insert the needle of the syringe into the Teflon tube. The fitting may need to be loosened and then retighten to permit the needle to pass through the sealing area 20 1/32” PEEK Tubing
Union adapter
Teflon sleeve
Gauge plug
Figure 5.3.6 Syringe adapter connections for solvent delivery to the DESI spray head For details on making the gas connection, please see section 5.4. With the gas and liquid connection made, the spray head can be placed in the rotational manipulator of the DESI 2D system. 1. Remove cap from rotational manipulator by removing the two hex head screws (see Figure 5.3.7) 2. Place the spray head into the retaining cap so that the high voltage connector points through the hole on the face of the cap as shown in Figure 5.3.8. Push the cap onto the spray head until the high voltage cap is protrudes through the hole and the spray head sits flat against the cap. The gas connection should be located on below the retaining cap and the solvent connection will fit in the grove of the cap 3. Place the spray head and cap into the open end of the rotational manipulator with the spray head pointing down 4. While holding the spray head and cap in position, evenly tighten the screws to secure the spray head in the manipulator (Figure 5.3.8) 21 Retaining Cap
Figure 5.3.7 Rotational manipulator before the spray head is installed HV Connector
Figure 5.3.8 Rotational manipulator with the spray head is installed At this time, the red high voltage cable can also be connected to the red liquid junction connector of the spray head. To connect, insert the 2 mm banana plug into the jack at the end of the high voltage wire. The emitter installed in the spray head will need to be replaced if it becomes clogged or damaged. Refer to the Section 10.3 for instructions for emitter replacement. Damage is 22 often caused by crashing the spray head into the inlet of the mass spectrometer or the sample surface. Use caution when positioning the spray head to avoid this damage. To change the angle at which the spray head is positioned, turn the rotational knob to the desired angle as shown in Figure 5.3.9. The manipulator is capable of providing a spray head angle anywhere between 40 – 80 degrees. The actual spray head angle is indicated by the mark that is just visible on the rotational arm as it exits the holder. Angle
Indicator
Adjustment
Knob
Figure 5.3.9 Spray head angle adjustment Y Axis, Z Axis, X Axis
Figure 5.3.10 Spray head X‐Y‐Z position adjustment Finally, the spray head arm has an X‐Y‐Z manual manipulator as shown in Figure 5.3.10. This three axis manipulator is used to position the spray head relative to the sample and capillary inlet. See Section 9 for a detailed discussion of the optimal angle and position settings of the spray head. 23 5.4 Gas Connections A high pressure nitrogen gas source is required for operation of the DESI 2D system. This nitrogen gas is used to aid in the formation of the DESI spray and direct the droplets produced towards the sample surface. Tefzel tubing (P300‐00010‐03) has been provided with the system kits to make the gas connecting lines between 1) the gas manifold and 2) the gas shutoff valve mounted under system’s the 2‐D stage (Figure 5.4.1). Another section of tubing is necessary to make the gas connection between 1) the gas shutoff valve and 2) the spray head gas connection (Figure 5.4.2) Using the supplied length of tubing, make the first tubing connections as follows: 1. Cut the end of the provided tubing square using an appropriate tubing cutter or razor blade 2. Slide the red Vacutight nut and ferrule onto the cut end of the tubing 3. Insert the Vacutight fitting and tubing into the threaded port on gas manifold mounted at the ends of the drawer guide rails and tighten appropriately 4. Connect the other end of the tubing to the shutoff valve, cutting the tubing to length. 5. Slide the nut and ferrule from the shutoff valve onto the tubing 6. Insert the fittings and tubing into the port of the valve and tighten appropriately Using the remaining tubing, make the second tubing connection between the shutoff valve and the spray head as follows: 1. Ensure the end of the tubing has been cut square. If not, cut the end of the tubing square using an appropriate tubing cutter or razor blade 2. Slide the nut and ferrule from the shutoff valve onto the cut end of the tubing 3. Insert the fittings and tubing into the port of the valve and tighten appropriately 4. Connect the other end of the tubing to the spray head, cutting the tubing to length. 5. Slide the red Vacutight nut and ferrule onto the cut end of the tubing 6. Insert the Vacutight fitting and tubing into the threaded port on the spray head and tighten appropriately NOTE When using the DESI 2D cover assembly, the gas line tubing must be cut with sufficient length to be routed through the opening at the front of the cover and to the spray head. See section 6.4 for details on using the cover with the DESI 2D system. The nitrogen gas input connection to the DESI 2D system is made at the gas manifold at the end of the drawer guide rails using a ¼ inch Swagelok fitting. Prosolia does not supply this tubing as the necessary length will vary according to the location of the gas supply in your laboratory. Ensure that the ¼ inch tubing used to make the connection between your high pressure nitrogen source and the DESI 2D system is rated to a working pressure of at least 250 PSI. 24 Gas Connection #2
Gas Manifold and
Shut-off Valve
Gas Connection #1
Figure 5.4.2 Gas connections on the DESI 2D system 25 5.5 Cable and Tubing Routing The DESI 2D system features cable and tubing routing locations on the spray head arm and ion source flange to help keep wires and tubing neat and out of the way. Routing cables and tubing through these locations also keeps cables out of the way when using the system cover. Figure 5.5.1 shows these routing locations. When using the routing points, be sure to have enough slack in the connections to operate the spray head arm through its full range of motion. Figure 5.5.1 DESI 2D system cable and tube routing locations, circled 26 6 DESI 2D System Installation The initial installation of the DESI 2D system may be performed by the end user, Prosolia, or its authorized representatives. This manual details installation and removal, the user controls, operation, and safety aspects of the DESI 2D system for normal, daily use. The manual also details maintenance procedures and spare/replaceable components of the system All tools necessary to install and maintain the DESI 2D system have been included in the system’s accessory kit. In addition to the components included with the system, operation of the system requires a compatible mass spectrometer, a source of high purity nitrogen gas, and common LC‐MS grade solvents and modifiers. The DESI 2D System has been designed to attach to the mass spectrometer in a similar manner to the instrument’s original electrospray ionization source, with minimal modification to the mass spectrometer. This section of the manual will acquaint the user with the installation procedure for the DESI 2D system. Users should fully read and understand the entire manual before beginning the installing and using the system on their mass spectrometer. 6.1 Preparation of Waters Xevo Mass Spectrometers Prior to the installation of the DESI 2D system onto a Waters mass spectrometer, the existing ionization source must be removed. Remove the original ionization source from the mass spectrometer according to the procedure described in the mass spectrometer hardware manual. Ensure all gas and liquid flows have been shut off, the lines are depressurized, and the interface temperature has cooled before removing the ionization source. CAUTION The mass spectrometer interface components are hot. Reduce the temperature of the interface and allow to cool before removing the ionization source. ATTENTION Les composants de l’interface de l’appareil de spectrométrie de masse sont chauds. Laissez les composants refroidir avant de retirer la source d’ionisation. 1. Ensure the instrument has been placed in Standby mode. 2. With the ionization source removed and the interface cooled to room temperature, close vacuum isolation valve. 3. Remove the ion sampling cone/cone gas nozzle by rotating the components clockwise to release them from the ion block. 4. Carefully remove the ion sampling cone/cone gas nozzle. Use caution to avoid dropping the ion sampling cone 5. Remove the ion sampling cone and o‐ring for use with the bazooka inlet tube. 27 Figure 6.1.1 shows the Waters Synapt G2 mass spectrometer with the ion source removed and the removal of ion sampling cone. CAUTION Do not install the extended Bazooka inlet tube at this time. The DESI 2D source must be installed prior to installation of the inlet tube. ATTENTION Ne pas installer le tube d'entrée Bazooka étendu à ce moment. La source DESI 2D doit être installé avant l'installation du tube d'entrée. Figure 6.1.1 Z‐Spray interface of the Synapt G2 with ion sampling cone installed (left) and removed (right) 6.2 Mounting the DESI 2D System After preparing the mass spectrometer, installation of the DESI 2D system can proceed. Installation requires the use of a 5 mm hex key which should be located for use prior to beginning installation. Installation of the Latch Mounting Block 1. Remove the retaining pin from the latch mounting block by completely unscrewing from the mounting block. 2. Place the latch mounting block over the source latch hook on the right hand side of the Xevo interface with the ‘foot’ pointing towards the ion block (see Figure 6.2.1). 28 Gas Plugs
Latch Mounting Block
Figure 6.2.1 Xevo interface flange with latch mounting block and gas plugs installed. Note the orientation of the latch mounting block. 3. Insert the retaining pin into the latch mounting block and tighten completely. 4. Insert a gas plug (P800‐00271‐01) into each gas port on the upper left side of the Xevo interface (see Figure 6.2.1). The plugs should fit snugly into the port. a. On some systems, the gas plugs may fit tightly into the port. A twisting action may be required to inset and remove the plug. b. Certain systems require the use of a larger o‐ring (3x1mm, part number P100‐00088‐01 ). If the plug fits loosely into the port, exchange the o‐ring for the 3x1mm o‐ring provided with the kit. 5. Replace o‐rings when they show signs of wear. TIP Choose the gas plug o‐ring that best fits your mass spectrometer. The fit should be snug. Small – 2.5 x 1 mm – Part Number P100‐00086‐01 Large – 3 x 1 mm – Part Number P100‐00088‐01 29 Installation of the DESI 2D System The system is now prepared for the installation of the DESI 2D system hardware. If you are unable to safely lift 20 pounds (9 kg), obtain the help of a second person for this step of the installation process. 1. If installed, remove the DESI system cover and set aside. 2. Prepare the DESI 2D system for mounting by sliding the source interlock slider towards the back of the system flange (see Figure 6.2.2) and loosening the mounting screws on the left hand side of the flange. Do not completely remove these screws. Figure 6.2.2 Interlock slider in the proper rearward position for mounting the DESI system to the mass spectrometer CAUTION Do not attempt to install the ion source with the extended capillary in place. Doing so may lead to damage to the capillary and the potential for electrical shock. ATTENTION Ne pas essayer d'installer la source d'ions avec le capillaire prolongé en place. Cela peut entraîner des dommages au capillaire et le potentiel de choc électrique. 3. Holding onto the sides of the 2D stage (see Figure 6.2.3), carefully mount the DESI 2D system by placing the system over the mounting pins of the Xevo interface and sliding downwards to seat the system on the interface. This procedure is done in a similar manner as mounting the standard Xevo ion source. 4. Insert the right hand mounting screw (located near the spray head hinge) through the flange and into the latch mounting block. It may be necessary to adjust the system position slightly to align the holes. 5. Tighten all mounting screws (three) using the 5 mm hex key to secure the DESI 2D system to the mass spectrometer. 6. Push the source interlock slide towards the instrument to close the source interlock switch (Figure 6.2.2). This slider satisfies only one of the interlock requirements for the instrument. See section 8.5 for details. 30 Figure 6.2.3 Mounting the DESI 2D system to the mass spectrometer by sliding the system over the mounting pins of the Xevo interface. Once the DESI 2D system has been mounted onto the mass spectrometer, additional connections for gas and electronics can be made. 1. The source interlock cable is plugged into the Blue socket under the sliding door, located directly above the ion source region. This connection is keyed to be inserted in one orientation only. 2. The high voltage cable is then plugged into the High Voltage socket located above the upper left corner of the ion source. 3. Finally, the nitrogen and other electrical connections (cameras, LED Lamp, etc.) to the system can be made (see Section 7). 31 Figure 6.2.4 Location of the source interlock and high voltage cable connections 6.3 Ion Transfer Capillary Installation Efficient collection of the ions generated in the DESI 2D system requires a close proximity of the ion inlet of the mass spectrometer to the sample being analyzed. The standard ion sampling cone used on the Waters Z‐Spray interface restricts one to analyzing only a very small sample without the use of an inlet extension capillary. A large diameter, bazooka ion transfer capillary has been included with the system to allow for analysis of larger sample areas with Waters mass spectrometers. In addition, the ion transfer capillary is slightly inclined such that there is clearance for samples to pass below the capillary. To install the bazooka capillary ion inlet, the ion sampling cone and the cone gas nozzle must have first been removed from the instrument following the instructions given in Section 6.1. IMPORTANT The installation of the extended ion transfer tube MUST be performed after mounting the DESI 2D system to the mass spectrometer. 1. Carefully assemble the bazooka extension by placing the ion sampling cone into the bazooka fitting in the same manner in which it fits the original desolvation gas cone. 2. Place the o‐ring around the base of the ion sampling cone as in Figure 6.3.2. 32 Figure 6.3.1 Bazooka extension components showing proper orientation of parts Figure 6.3.2 Bazooka extension with ion sampling cone and o‐ring installed 3. Slide the ion transfer capillary assembly into receiving slot on the ion block with the inlet tubing pointing straight upwards. The ion sampling cone will insert into the ion block. This part fits the same manner as the ion sampling cone/cone gas nozzle. 4. Carefully place the 5 mm wrench provided with the system kit over the wrench flats on the bazooka inlet cone. 5. Rotate the bazooka inlet counter clockwise (downwards) until the front edge of the bazooka cone is aligned with the front edge of the ion block. The capillary will have a slight (5°) downward slope when installed. 6. Slowly turn the handle of the vacuum isolation valve to its open position. 7. Return ion block temperature to its normal operating value. 33 Figure 6.3.3 Finished installation of the ion transfer capillary. 6.4 Installation of the DESI 2D System Cover and Exhaust Line The DESI 2D system for Waters Xevo mass spectrometers includes a system cover to prevent access to the source components will in operation and the help shield users from solvent vapors and sample aerosols when connected to a proper exhaust system. The use of the system cover is required. The lid of the cover is interlocked and must be closed for the instrument to operate. For more details, please see Section 8.5. CAUTION The cover and exhaust line connection are provided to reduce, but will not eliminate exposure to any solvent or sample aerosols created by DESI 2D system. Additional personal protective measures may be necessary to eliminate operator exposure to aerosols created by the source. ATTENTION La connexion de la ligne d'échappement et la couverture sont prévus pour réduire, mais pas éliminer l'exposition à des aérosols ou de solvants échantillons créés par la source d'ions DESI 2D. Mesures de protection personnelle supplémentaires peuvent être nécessaires pour éliminer l'exposition de l'opérateur aux aérosols créés par la source. 34 Exhaust Line Connection The exhaust line connection, shown in Figure 6.4.1 below, is located on the bottom of the source platform. An external exhaust or vacuum system should be attached to this connection to assist in capturing aerosols generated by the DESI 2D system. A ¾” or 1” hose can be attached to the vent line connector. Users MUST perform a hazard risk assessment to evaluate the need for additional personal protective equipment when operating the DESI 2D system. The use of varied sample types and varied spray solvents can lead to hazards not anticipated in the design of the product. Consult your organizations Environmental, Health, and Safety (EHS) personnel and Prosolia for more information regarding these hazards. Figure 6.4.1 Location of DESI 2D system vent fitting. Installation of the System Cover The DESI 2D system cover is connected to the instrument mounting flange via two pins located on the top surface of the flange as shown in Figure 6.4.2. To install the cover: 1. Move the 2D stage to the middle of its travel in both directions. 2. Holding the cover by the side handles, carefully place the cover onto the mounting pins using care to avoid pinching cables or tubing. Lift straight upwards and avoid tipping the cover as it is removed. TIP Due to the close fit between the cover and the mounting pins, the cover must be lifted straight upwards to avoid binding on the mounting pins. 35 Figure 6.4.2 Location of system cover retaining pins NOTE It may be necessary to move the sample stage position prior to installing/removing the system cover. The cover cannot be installed /removed with the stage at the home position. When properly installed, a gap is left between the cover and the system flange for passage of the spray head solvent and gas supply lines as well as the camera and LED cables. Care should be taken when installing or removing the cover not to pinch or damage these lines and cables. Operation of the Cover Lid The system cover features a hinged lid for easy access to the system components. The lid is opened using the cover on the front of the cover as shown in Figure 6.4.3. When in the opened position, the cover lock can be moved into a locked position to prevent the lid from closing unexpectedly. To lock and unlock the lid, simply push the locking mechanism in the desired direction. 36 Cover Lock
Figure 6.4.3 Handle for opening of the system lid (left) and location of the cover locking slide (right) Opening the lid will trip the mass spectrometer interlock, disabling the electrospray and cone voltages. The lid must be in the closed position to operate the mass spectrometer. Figure 6.4.4 Photograph showing the DESI 2D system and cover installed on a Waters Synapt G2 HDMS mass spectrometer 37 6.5 Removal and Storage of the DESI 2D system Removal of the DESI 2D system from the mass spectrometer is the reverse of the installation procedure. Before removing the system, allow the interface of the mass spectrometer to cool. 1. Reduce the interface temperature of the mass spectrometer and place it in Standby mode. 2. Turn off the power to the DESI control electronics. 3. Turn off the nitrogen gas to the DESI 2D system and allow the gas lines to depressurize. 4. Remove the DESI 2D cover and set aside. 5. Remove the syringe pump connection from the syringe needle and place the union on top of the 2D stage. 6. Unplug the LED light and Camera connections from the from the DESI control electronics. 7. Unscrew and remove the 25 pin motor control cable from the bottom of the DESI 2D stage. 8. Remove the exhaust line if connected. 9. Unplug the Interlock and high voltage connections from the mass spectrometer. 10. Close the vacuum isolation valve on the mass spectrometer and remove the extended ion transfer tube. 11. Slide the source interlock slider away from the mass spectrometer (see Figure 6.2.2). 12. Completely remove the mounting screw on the right hand side of the flange. 13. Loosen the left hand mounting screws and slide the system upwards on the face on the mass spectrometer to remove. 14. Remove the latch mounting block. Reinstall the retaining pin and right hand mounting screw to prevent these components from becoming lost. 15. Remove the gas plugs from the mass spectrometer interface by pulling and twisting. The DESI 2D system is intended to be stored on a shelf or table top in the upright position, sitting the lower portion of the instrument mounting flange and the bottom components of the system. The cover can be placed on the system while in storage to prevent damage to the DESI spray head. CAUTION Do not lift the DESI 2D system by the handles of the source cover. The cover is not attached to the source and it will separate and fall, damaging the system and potentially causing personal injury. ATTENTION Ne pas soulever la source DESI 2D par les poignées du couvercle de la source. Le couvercle est pas attaché à la source et il va se séparer et tomber, endommager le système et qui pourrait causer des blessures. 38 7 Electrical Connections Electrical connections for control of the automated sample stage of the DESI 2D system, power to the camera, LED lamp, USB communication to the instrument data system, and the I/O cable for triggering of the mass spectrometer are made at the DESI 2D control box. The following section details the electrical connections to the control electronics and mass spectrometer. Figure 7.1.1 Photograph of the DESI 2D motion control box. 7.1 Electrical Mains Connection The DESI 2D system requires one wall outlet to be available at the mass spectrometer for system power. The mains power for the system shall meet the requirements outlined in Section 4.1. Plug the mains power cord into the power supply before connecting to line power. In the case of an emergency, the mains power cord serves as the disconnecting device and should be removed from the wall outlet to remove the mains power from the system. CAUTION When installing the equipment, position the unit such that the power cord can easily be unplugged from the mains voltage (outlet) in an emergency. ATTENTION Assurez que l’interrupteur général ainsi que le connecteur pour le câble électrique soient facilement accessibles et qu’ils se trouvent le plus proche possible de l’operateur de l’appareil. 39 CAUTION Place the DESI control box and power supply away from areas where flammable liquids are likely to be spilled. Spilling flammable liquids onto the control box or power supply may result in a fire. ATTENTION Place la boîte de commande DESI et bloc d'alimentation loin des zones où des liquides inflammables sont susceptibles d'être déversé. Tout déversement de liquides inflammables sur la boîte de commande DESI ou bloc d'alimentation peut provoquer un incendie. The DESI control box is designed to be operated at a nominal voltage of either 120V or 230V AC, 50/60 Hz. Your system will be shipped complete with the appropriate power cord as listed in Section 4.1 7.2 Rear Panel Connections The rear panel of the DESI control box contains the connections for the control electronics power, the USB communication port, and video connection from the camera. In addition, the 1 ampere protection fuse is also located on the rear panel of the control electronics. USB
Fuse
DC Power
Video
Figure 7.2.1 Electrical connections made on rear panel of the DESI control electronics box Communications Connection: 1. Insert B‐type plug end of the supplied USB communications cable into the ‘COMPUTER’ connection on the rear panel. 2. Insert A‐type plug end of the supplied USB communications into any USB port on the back of the computer (Figure 7.2.2). 40 NOTE The USB connection to the instrument data systems should be made directly to a USB port on the data system computer, not through a USB expansion hub (such as those common on monitors). Failure to connect directly to the computer may result in communication errors between the computer and control electronics. USB Ports
Figure 7.2.2 Typical serial port location on rear I/O panel of computer Video Capture Card / Camera Connection The video image from the camera is displayed within the DESI control software window on your computer monitor. This requires the installation of the ViewCast Osprey 210 video capture card and drivers provided with your system. To install the video capture card, consult your IT Support personnel and follow the manufacturer’s installation instructions provided with the video card. Camera Connection to the DESI Control Electronics To connect the video camera to the video capture card, begin by connecting one end of the supplied BNC‐BNC video cable to the VIDEO 1 OUT connector located on the rear panel of the DESI control electronics. The opposite end of the cable will be connected to the video capture card as described below. Camera Connection to the Video Capture Card 1. Install the video capture card and drivers in the computer per the manufacturer’s instructions. An installation manual is included on the CD with the video capture card. NOTE When installing the video capture card software, select NTSC as the video format. 2. Attach the breakout cable supplied with the video capture card to the 15 pin D‐sub connector on the video capture card. 3. Connect the free end of the supplied video cable to the yellow BNC jack of the video capture card’s breakout cable 41 7.3 Front Panel Connections The front panel of the DESI control box contains the connections for the video camera, the LED light source, the trigger cable to the mass spectrometer, and the DESI 2D stage. In addition, the front panel also contains a power status lamp built into the power switch. Some connections at the front panel are made using locking Lemo connectors, which are keyed to ensure the proper orientation of the plug. To make connections at the front panel, simply hold the connector with the red dot facing up and insert it into the proper socket on the front panel. A ‘click’ will be heard when the connector has been locked into place. To remove the plugs, simply pull back on the locking sleeve to unlatch and remove the plug. Figure 7.3.1 Insertion (left) and removal(right) of the Lemo connections on the front panel of the DESI control electronics box. VIDEO 1 IN – The supplied video camera should be connected to the control electronics though this video input connection LIGHT – This connection provides power to the LED light source. I/O – This connection is used to trigger the mass spectrometer for automated data collection. The end of the supplied cable with the Lemo connector should be plugged into this socket. The other end of the cable should be plugged into the I/O port of the mass spectrometer (see section 7.4). MOTOR CONTROL – This connection provides power to the motors which drive the motion of the sample stage in the both the X and Y directions. A 25 pin, D‐subminiature cable has been supplied to connect the control box to the 2D stage for control of the X and Y axis stages. Each end of the cable locks to the mating fitting by thumbscrews. 42 7.4 I/O (Trigger) Cable Connection The DESI System control electronics are capable of triggering the mass spectrometer to collect data from multiple samples much like a standard autosampler in LC‐MS. The connection to the proper port on the mass spectrometer must be made to use this function. A cable with the proper termination for the instrument specified at the time of order has been included with the source. With the five pin Lemo connector plugged into the I/O port on the front of the control box, plug the opposite end of the cable into the I/O port of the mass spectrometer. To make this connection, you may need to unplug any connection from an LC system that may be plugged into the I/O port of the mass spectrometer. CAUTION To avoid electric shock, all electrical connections to the I/O connector must be separated from hazardous voltages by double or reinforced insulation. Circuits of this type are classified as safety extra low voltage (SLEV). ATTENTION Pour éviter les chocs électriques, toutes les connexions électriques pour le connecteur d'e/s doivent être séparées de tensions dangereuses par une isolation double ou renforcée. Circuits de ce type sont qualifiés de safety extra low voltage (SLEV). Pin I/O Cable Color Description Trigger signal – Do not apply external voltage to 1 Start + White pin 5 Ground Black Digital Ground Table 7.4.1 Pin out of the I/O port and cable. Pin ID 43 8 Operation of the DESI 2D System DESI 2D Systems are simple to operate. This section details the operation of the system including positioning of the spray head arm, operation of the sample stage Z‐axis, movement of the manual manipulators, operation of the automated X and Y stages, insertion/removal of samples, and source interlock functions. Prior to operating the system, the DESI control software must be installed on the mass spectrometer’s data system computer and the electronics connected. See the Omni Spray Ion Source 2‐D Automation Software Installation and Reference Manual for further information on software installation. 8.1 Spray Head Manipulators Proper positioning of the spray head is critical to maximizing the performance of the DESI 2D system. Not only can the position of the spray head change in the X, Y, and Z axis, its angle is also variable. To change the angle at which the spray head is positioned, turn the rotational knob to the desired angle as shown in Figure 8.1.1. The manipulator is capable of providing a spray head angle anywhere between 40 – 80 degrees. The actual spray head angle is indicated by the mark that is just visible on the rotational arm as it exits the holder. Angle
Indicator
Adjustment
Knob
Figure 8.1.1 Spray head angle adjustments The spray head arm also has an X‐Y‐Z manual manipulator as shown in Figure 8.1.2. This three axis manipulator is used to position the spray head relative to the sample and capillary inlet. See Section 9 for a detailed discussion of the optimal angle and position settings of the spray head. 44 Each axis on the three axis manipulator has a locking screw. There is a lock symbol next to each screw and an arrow that indicates the direction to lock down the manipulator. It is recommended that these manipulators are locked once the spray head position has been set. However, it is important to loosen these screws before adjusting the manipulator. Failure to loosen the locking screw will result in damage to the manipulator. Y Axis, Z Axis, X Axis
Figure 8.1.2 Spray head X‐Y‐Z position adjustment Z Axis Locking Screw
Figure 8.1.3 Manipulator locking screws 8.2 Motion of the X and Y Stages The X‐direction and Y‐direction of the sample positioning has been automated to provide computer controlled movement. Control of the sample position is achieved using the Omni Spray 2‐D Control Software. The X and Y stages can be positioned manually within the software or through several automated motion profiles for analysis of multiple 45 samples. Please see the Omni Spray Ion Source 2‐D Automation Software Installation and Reference Manual for further information on the types of motion available. In general, there are two operating modes that can be used to position the sample by moving the X and Y stages which are described below. Manual Motion Control Operation under manual motion control allows for the free movement of the sample surface. In this mode of operation, commonly used for investigating new samples, source optimization, etc., continuous data collection is the preferred method for saving results. Movement of the stages is driven by dragging of the position indicator within the software window. Automated Motion Control Under automated motion control, the automated DESI 2D system can reproducibly collect data from individual samples, much like an autosampler of a typical LC/MS system. Typically, three steps are necessary to perform an automated sequence analysis. 1. Construction of the motion sequence within the Omni Spray control software ‐ The sample analysis sequence is constructed in the DESI software under the desired automated motion profile. 2. Development of the mass spectrometer analysis method ‐ Using the calculated acquisition time from the automated motion sequence, mass spectrometer methods are developed using the appropriate data analysis time. 3. Construction of sample sequence in mass spectrometer data system – A sample analysis sequence is created in the mass spectrometer data system to match the number of samples in the Omni Spray control software using the methods developed in step 2. Following the creation of both a sample sequence within the mass spectrometers data system and the motion sequence within the Omni Spray control software, the sample plate can be analyzed. 1. The DESI 2D system must be in the proper operating position (optimized positions previously determined), with the sample placed in the sample holder. 2. The sample sequence is started within the mass spectrometer’s data system. Users must wait until the mass spectrometer is ready to receive a start trigger from the DESI 2D system before preceding the step 3. 3. The motion sequence is started within the Omni Spray control software. The mass spectrometer will trigger automatically and begin analysis of the sample. 46 8.3 Manual Positioning of the Sample Stage Z Axis Unlike the movement of the X and Y axis, the Z axis of the sample stage can only be adjusted by manually. The location of the Z axis adjustment knob is shown in Figure 5.3.1. By turning the adjustment screw, the entire X and Y stage is raised or lowered allowing for different sized samples to be analyzed. When raising the sample stage, use caution to avoid crashing the spray head into the sample and possibly damaging the spray nozzle/emitter. Z Axis
Adjustment
Figure 8.3.1 Location of the Z axis adjustment screw near the 2D stage 8.4 Spray Head Arm The spray head arm on the DESI 2D system pivots near the ion source flange to allow for access to the sample surface for easy sample changing. The arm is locked into the operating position using a cam/lever mechanism. To rotate the spray head from its operating position, turn the handle on top of the hinge approximately ¼ turn clockwise, as shown in Figure 8.4.1. The handle will point to the Z axis adjustment knob when the hinge is released. With the hinge released, simply push the spray head arm to the right to rotate it out of position. To put the spray head arm back into operating position, simply return the spray hard arm to position and turn the locking handle counter clockwise to secure. Turning the handle will lock the hinge mechanism and pull it into alignment with the ion source flange. 47 Figure 8.4.1 Rotate the locking handle (left) ¼ turn clockwise to release the locking mechanism on the hinge Figure 8.4.2 Spray head arm rotated to allow access to the sample surface 8.5 High Voltage Interlock The DESI 2D System maintains the safety interlock features of the mass spectrometer such that when the system is taken out of its operating position (removed from the mass spectrometer or the enclosure lid is opened), the high voltage from the mass spectrometer is disabled. For Waters Xevo mass spectrometers, there are two interlock requirements that must be met for the system to operate properly. The first interlock switch that must be closed is located within the mounting flange of the mass spectrometer. This interlock requirement is met using a manually actuated mechanism when the system is installed onto the mass spectrometer. The interlock slider (see Figure 6.2.2), located at the top of the interface flange MUST be pushed fully forward after the system has been installed for the mass spectrometer to operate. 48 This model of the DESI 2D system features an interlocked system enclosure to prevent user access to high voltage components of the system and mass spectrometer during operation. This enclosure must be in place with the lid closed for the instrument to operate. Both interlock requirements must be met for the mass spectrometer to operate properly. CAUTION To avoid a possible static like shock, do not touch the mass spectrometer interface components or the spray head while the instrument is in Operate Mode. ATTENTION Pour éviter un choc statique semblable, ne touchez pas les composants de l'interface du spectromètre de masse ou la tête de pulvérisation alors que l'instrument est en Operate Mode. To allow for adjustment of the spray head position and the sample stage height while the instrument is operating, the system enclosure features tool access holes. To make these adjustments, hex drivers with insulating handles have been provided with the DESI 2D system kit. To make the adjustments, simply insert the proper insulated handle hex driver through the proper opening in the system enclosure and into the hex socket of the manipulator handle. Use caution when adjusting the spray head manipulator. If excess resistance is felt, stop and ensure the locking screws are not tightened to prevent damage to the manipulator. CAUTION Use the insulated hex drivers provided to make position adjustments while the instrument is operating. NEVER insert other tools or objects into the adjustment holes due to risk of electrical shock. Figure 8.5.1 Adjusting the sample stage height (left) and Y‐axis of the spray head manipulator using the insulated hex drivers 49 8.6 Slide Holder Operation The sample holder of the DESI 2D system is designed to hold up to two standard 76 x 26 mm microscope slides or one slide fitting the microtiter plate standard footprint (127.76 mm X 85.48 mm). The each location in that can accept a slide in the sample holder has a spring clip which is used to secure the sample slide(s) in the holder and prevent vibrations during automated motion. To insert a sample into the slide holder, pull the spring clip back while placing the slide in place. Release the spring clip to secure the slide (see Figure 8.6.1). Slide(s) already in the holder can be removed by the finger groove provided. Always be careful not to touch the sample area while installing or removing the slide(s). Periodically, dust and debris will need to be removed from the slide holder to allow surfaces to sit flat on the holder. The slide holder may be cleaned with 70% isopropyl alcohol to remove contamination. A gentile stream of nitrogen or clean compressed air can be used to blow dust from the slide holder surface. Care should be taken to avoid blowing this dust and debris onto the precision guide rail or motor lead screws of the 2D automated stage. Sample Holders for
76 x 26 mm slides
Spring Clip
Figure 8.6.1 Sample holder showing spring clips and locations for 76 x 26 mm slides 50 8.7 Automating Data Collection with MassLynx™ To utilize automated data collection using MassLynx and your DESI 2D system, you must first ensure that the instrument is configured properly to accept the contact closure signal through MassLynx. The contact closure type is through the ‘Inlet Method’ editor as described below. 1. Select the Inlet Method editor from the left hand column under the ‘Instrument’ tab in the MassLynx window 2. Select ‘Instrument Configuration…’ from the Tools menu 3. Remove any configured devices (LC Systems, detectors, etc.) by selecting the ‘Configure’ button and selecting ‘None’ for each component. See Figure 8.7.1 4. Configure the instrument to accept the contact closure input by selecting the ‘Events & Triggering’ button 5. Check the box next to ‘Event In 1’ to enable the instrument to accept the contact closure. See Figure 8.7.2 Figure 8.7.1 Screen shot of Inlet Method window showing configuration for the DESI 2D System 51 Figure 8.7.2 Screen shot of Inlet Method window showing configuration of the instrument to accept a contact closure Creating an MS method in MassLynx with your DESI 2D system In this section, important considerations when creating a MS method to be used with your DESI 2D system are discussed. TIP In most cases, the instrument should be properly tuned in MS Tune prior to executing a sample sequence. Parameters (voltages, syringe pump flow rate, etc.) set in the MS Tune program will be used in the MS method for analysis 1. Select the MS Method editor from the left hand column under the ‘Instrument’ tab in the MassLynx window 2. Edit the MS method to include the desired MS experiments. It is suggested to use voltages from the MS Tune page The total acquisition time should be set in accordance with the calculated sample acquisition time for your experiments in the DESI control software. See Figure 8.7.3. NOTE The DESI 2D system has a 5 second post‐acquisition delay by default. If the acquisition time in MassLynx is set too long relative to the calculated acquisition time established in the DESI 2D motion system, data acquisition steps will not be synchronized. 52 Figure 8.7.3 MS Method editor in MassLynx. Note total run time circled in figure must match the calculated acquisition time in the DESI software to maintain synchronization between MassLynx and the DESI 2D system Creating a sample sequence in MassLynx for automated data acquisition Please follow the instructions detailed in the MassLynx software manual for information on how to set‐up a sample sequence. Your MassLynx sequence should match the motion sequence in the DESI control software in the number of samples to be run. 1. Add samples to the sample queue in the MassLynx window 2. For each sample, choose the appropriate MS Method 3. An inlet method is not necessary if the instrument has been configured as described above. The MS Status display will show a contact closure is configured See Figure 8.7.4 Once you have set‐up a sample sequence in Mass Lynx, follow these steps to execute the sequence. 1. Select ‘Start from the ‘Run’ toolbar in MassLynx. 2. In the Start Sample List Run window, enter the row numbers to analyze and click ‘OK’ See Figure 5.7.4 NOTE The number of rows of the sample sequence must match the number of rows in the motion sequence in the Omni Spray control software to maintain synchronization between the mass spectrometer and the DESI 2D System. 53 3. The instrument status located in the lower left of the MassLynx window should now read “Waiting for inlet start 1” See Figure 8.7.5 4. Return to the DESI automation software, click ‘Start’ to begin sample analysis. TIP Follow the steps outlined in Section 6.4 Sample Spot Calibration prior to executing the sample sequence. NOTE If the data acquisition system does not begin collecting data (i.e. it is still waiting on the contact closure), ensure that your DESI 2D hardware is properly installed. Refer to Section 7 of this manual for connection information. Figure 8.7.4 Screen shot of the MassLynx ‘Start Sample List Run’ window 54 Figure 8.7.5 Screen shot of the MassLynx window indicating the mass spectrometer is waiting for the contact closure signal. 55 9 DESI 2D System Testing The procedures and instructions in this section of the manual are intended to help new users become familiar with performing DESI experiments on the DESI 2D system and to guide them through the initial testing of the system. If problems arise with the operation of the system, performance testing using the following procedures is suggested. 9.1 General Operating Parameters When operating your DESI 2D system there are many degrees of freedom that when changed will vary the geometry of the experiment. These parameters include the spray impact angle (α), the tip to surface distance (d1), the tip to inlet distance (d2), and the surface to inlet distance (d3). Recommended operating parameters are displayed below in the table Typical Operating Parameters. Figure 9.1.1 below shows the relative location of the sample, spray tip, and instrument inlet using the suggested operating parameters given in the table. In general, the spray head angle can be positioned between 40‐90 degrees, with the tip at a distance of 1‐5 mm from the sample surface. The distance from the sample to the instrument inlet is around 2‐5 mm. As mentioned previously, the nitrogen pressure for the nebulizing gas is varied between 80‐200 PSIG. For each type of sample and for different solvent compositions, these variables may need to be adjusted to get the optimal results. Figure 9.1.1 Relative Position of the Sample, Spray Head, and Instrument 56 Parameter Electrospray voltage Solvent flow rate Gas pressure Tip to surface distance (d1) Tip to inlet distance (d2) Surface to inlet distance (d3) Spray impact angle () MS inlet temperature Table 9.1.1 Typical operating parameters Setting 2.75 kV 2.0 L/min 100 PSI 2 mm 3‐4 mm ~0.5mm 55° 150 °C 9.2 Standards Preparation Dried chemical standards have been included with the DESI 2D system to be used for initial testing and familiarization with the system. The following reagents will be necessary to reconstitute the dried standards: 


Acetonitrile (HPLC Grade) Water (HPLC Grade) Formic acid (HPLC Grade) Preparation of bradykinin Peptide Standard 

Reconstitute the bradykinin peptide standard (MW: 1060.1) (part # P900‐00307‐01) provided in your DESI 2D system kit by pipetting 1.00 mL of 80:20 acetonitrile:water directly into the glass vial to give a 1 mg/mL stock solution of bradykinin. Vortex or shake to ensure standard is dissolved. Prepare a working standard solution of bradykinin at10 µg/mL by pipetting 10.0 µL of the stock solution into the provided glass vial. Add 990.0 µL of 80:20 acetonitrile:water and vortex or shake to ensure mixing. 57 9.3 Preparing and Using the Omni Slide for Analysis Omni Slide™ Sample Surfaces are disposable sample surfaces for use with Prosolia’s DESI systems. Omni Slide sample surfaces are designed to aid the user in executing reproducible experiments from a standardized surface. They are available in a variety of sizes and formats to meet different experimental needs. This section describes the use of two formats on Omni Slide Hydrophobic Arrays. The Omni Slide Hydrophobic Array substrates allow for reproducible sample spotting and improved signal stability in high‐
throughput and quantitative studies. These arrays also provide discrete sample spotting locations and position references which can be easily programmed into the Omni Spray control software. Omni Slide Micro‐24 Sample Arrays – The Omni Slide Micro‐24 Sample Array substrates (shown in Figure 9.3.1) are a76 x 26 mm microscope glass slide with a printed 24 spot array. The slides have sample locations of 3 mm diameter and a center‐to‐center separation of 4.00 mm. The large white surface at the end of the slide is writable and intended to be the end handled by the user. 4.00 4.00 3 mm dia.
4.00 4.00
Figure 9.3.1 Layout of 24 well Omni Slide Micro‐24 Array MT‐96 Sample Arrays – The Omni Slide MT‐96 Sample Array substrates (shown in Figure 9.3.2) are a microtiter format glass slide with a printed 96 spot array. The slides have sample locations of 3 mm diameter and a center‐to‐center separation of 9.00 mm. The sample location pattern meets the microtiter format standard. The white bar at the bottom of the slide is writable for noting sample information. 58 5.50 9.00 9.00
5.50 3 mm dia.
Figure 9.3.2 Layout of 96 well Omni Slide MT‐96 hydrophobic array Sample Deposition Direction ‐ The automated motion sequences performed by the DESI 2D system begins from a neutral point in the margin area. As such, when a sequence is started, the sample stage will first move to the neutral point, followed by approaching the first sample from the left. In general, samples are analyzed from left to right, front to back. When possible, as a matter of good practice, samples should be placed in an order in which the lowest concentration samples are analyzed first, followed by samples of increasing concentration, to prevent the possible contamination of the mass spectrometer inlet. Use of the Origin Feature – The origin feature is commonly used to create a relative origin from which sample positions are measured. For example, when using an MT‐96 Omni Slide sample substrate, samples are spotted in an array at regular intervals. The Omni Slide features and alignment cross such that the spray can be aligned with the surface and an origin can be applied to take into account the manufacturing variance of sample spot locations on the glass substrate. This method removes the need to modify sample positions for variance in the spot location if the origin is set to align each surface placed in the sample holder using the same reference point on the sample slide. 59  Align sample surface to a reference point such as the center of the alignment cross or the center of a sample spot.  Set the origin at this point  Program the location of the samples into the Omni Spray 2‐D control software Align inlet/spray to cross
Set origin location
When placing next sample slide in holder: Samples at regular intervals
 Using same reference point, align the next sample slide  Set the offset origin at this point to adjust for differences in the spot location relative to the first slide  The previous sample locations entered will now be valid for this sample slide Figure 9.3.3 Layout of 96 well Omni Slide MT‐96 hydrophobic array 60 9.4 Testing Prior to beginning your experiments using the DESI 2D system, the mass spectrometer should be calibrated and tuned for best sensitivity for the type(s) of compound(s) of interest (i.e. small molecules, proteins, etc.), and free of contamination in the ion interface/optics. All solvents used with your system should be HPLC grade and free from contamination/impurities. Use caution when preparing solutions to avoid the introduction of contaminants such as plasticizers. It is recommended that users follow the procedure outline below in order to familiarize one with operating the DESI system. It is recommended that users become familiar with the given references about DESI to learn the implications of varying the parameters of the experiment. The example experiments given in this section are performed using the geometric parameters described in Section 9.1 and use 50:50 acetonitrile:water + 0.1% formic acid (v/v) as the spray solvent. NOTE The data presented in section 6.4 represents typical data collected on Waters Synapt G2 for the standards supplied with the DESI system. Results on other instruments will vary based on the age and condition of the instrument, the level of contamination in the interface region, instrument tuning, etc., as well as the exact model of instrument onto which the system is installed . Omni Slide Preparation (76 x 26 mm) 1. Mark the center of the first spot (furthest spot to the left) on an Omni Slide using the red Sharpie provided to you in your DESI 2D system kit. Refer to Figure 9.3.1. 2. Deposit 1µL of bradykinin peptide standard working solution onto the center of the second, third, and forth spots on the Omni Slide. NOTE Be sure to pipette consistently across the row on the Omni Slide as too much deviation in droplet location will significantly affect your results. 3. Allow all spots to dry completely prior to analysis. Omni Slide Preparation (Microtiter Plate Format) 1. Mark the center of the cross located at the top right hand corner of an Omni Slide (position 0,0) using the red Sharpie provided to you in your DESI 2D system kit. Refer to Figure 9.3.2 2. Deposit 1µL of bradykinin peptide standard working solution onto the center of spots A1, A2, and A3 on the Omni Slide. 61 Sample Spot Calibration Follow the procedure below to align the spray head using the DESI 2D motion system with the row where you deposited the standard solutions. 1. Turn‐on the power to the DESI motion control power supply. 2. Double click Omni Spray 2‐Dicon from the start menu. The motion system should initialize, execute a ‘calibration’ routine, and return to home. NOTE Please refer to the Omni Spray Ion Source 2‐D Automation Software Installation and Reference Manual for instructions on loading the Omni Spray 2‐D automation software. 3. Using the Omni Slide prepared in the previous section place the surface in the slide holder of your DESI 2D system according to the orientation suggested above. 4. Turn on the spray solvent delivery system (typically a syringe pump) and nitrogen gas flow to your DESI 2D system. These examples use 50:50 acetonitrile:water: 0.1% formic acid (v/v) as the spray solvent. Allow the flows time to stabilize. 5. Turn on the mass spectrometer. TIP Wait approximately 1 minute for the spray to stabilize. 6. With the motion system set at the default origin (2, 2 mm), establish geometrical parameters according to the suggested operating parameters in Section 9.1. 7. Using the Omni Spray 2‐D Motion Control software, move the surface to the location where the red dye was deposited using the manual motion control buttons (see Figure 9.4.1). Goal Position
Current Stage Position
Current Origin Location
Set Origin Button
Return to Origin Button
Manual Motion Control
Figure 9.4.1 Manual positioning parameters in the Omni Spray control software window 62 1. Optimize the signal intensity of the ion at mass/charge (m/z) 443 by finely adjusting the spray head to inlet distance (d2). An example mass spectrum of the red dye is shown in Figure 6.4.2 below. 2. Set the origin at this location using the Set Origin button and proceed to sample analysis. NOTE Data presented in this section is from a single scan of the MS, choosen at the peak intensity of the ion of interest. Combining spectra, as is typically done, will improve both ion intensity and in most cases S/N. Sharpie - 50/50 ACN/H2O w/ 0.1% FA
DESI_STD_RG6_04 3 (0.068)
TOF MS ES+
2.81e4
443.3006
28130
%
100
444.3036
7981
149.0471
4767
445.3078
1822
301.1912
1687
0
100
150
200
250
300
350
400
450
500
550
600
650
700
750
800
850
900
950
m/z
1000
Figure 9.4.2 DESI mass spectrum of the red Sharpie marker on the Omni Slide hydrophobic surface. The ion at mass/charge 443 corresponds to the intact cation of rhodamine 6G. NOTE This example shows typical results when the procedure above is followed. If you do not observe the signal at 443, ensure that:  The syringe pump is ‘ON’ and the spray solvent is flowing without obstruction.
 The capillary emitter is protruding out of the nozzle according to the recommendations in Section 2.4.  All operating parameters are similar to the recommendations in Section 6.3. 63 Sample analysis The DESI 2D system gives users the option of several different motion profiles, as detailed in the Omni Spray Ion Source 2‐D Automation Software Installation and Reference Manual. Additionally, the Omni Spray 2‐D automation software is set‐up to sync with the instrument’s data acquisition system using the contact closure feature. This feature allows automated data acquisition on a spot by spot basis, if desired. Please refer to Sections 3 and 4 of this manual for details about the installation of the DESI motion control hardware and connecting the contact closure cable. Bradykinin peptide standard – The analysis of bradykinin peptide standard deposited onto an Omni Slide should produce signal intensities comparable to that shown in Figure 9.4.2. Multiply‐charged ions corresponding to the triply‐, doubly, and singly‐protonated forms of bradykinin will be present. Additionally, some adduct formation with sodium and/or potassium ions may also be present, as indicated in Figure 9.4.2. DESI_STD_BKTEST_05 54 (0.939)
TOF MS ES+
2.11e3
530.8535
2111
100
2+
[M+2H]
%
531.3669
1052
0
100
150
200
250
300
350
400
450
500
550
600
650
700
750
800
850
900
950
m/z
1000
Figure 9.4.2 DESI mass spectrum (centroid) of bradykinin (10ng/spot) 64 9.5 Additional Experimental Examples The following section shows additional experimental examples utilizing your automated DESI 2D system. Note that the data presented here was not collected using a Waters mass spectrometer, but is intended to serve as a demonstration of the automated capabilities of the DESI system. Point to Point – Dwell Typical results when using the point‐to‐point dwell mode (a typical setup is shown in Figure 9.5.1) for consecutive 10ng deposits of bradykinin peptide standard are shown in Figure 9.5.2. The selected ion current for bradykinin at m/z 530.9±1 is displayed for three consecutive spots. The data from each spot was collected in one data file. The integrated peak areas show an inter‐spot variability of approximately 10% RSD. Figure 9.5.1 Example 96 sample point to point – dwell motion profile 65 RT: 0.00 - 0.67 SM: 7G
RT: 0.05
MA: 705977
100
NL:
9.96E4
RT: 0.64
MA: 663343 m/z=
528.77533.08 MS
bradykinin_
ptopdwell_0
4
95
90
0.09
85
75
0.30
70
0.15
65
Relative Abundance
0.50
RT: 0.32
MA: 597726
0.12
0.51
0.52
0.14
80
0.35
0.36
0.19
0.56
0.59
0.62
0.39
60
55
0.41
50
45
40
35
30
25
20
15
10
5
0.01
0
0.00
0.05
0.10
0.15
0.20
0.25
0.30
0.35
Time (min)
0.40
0.45
0.50
0.55
0.60
0.65
Figure 9.5.2 Selected ion current of 10ng bradykinin [M+2H]2+ in triplicate using a point to point – dwell Point to Point – Oscillate The oscillate motion profile allows you to move the surface beneath the spray head at defined velocities and intervals. This feature is advantageous when locating a ‘sweet spot’ within the sample analysis area and also enables averaging over a larger surface area than in the point to point – dwell mode. The results of a typical point to point – oscillate experiment (a typical setup is shown in Figure 9.5.3) for consecutive 10ng deposits of bradykinin peptide standard are shown in Figure 9.5.4. The selected ion current for bradykinin at m/z 530.9±1 is displayed for three consecutive spots. The data from each spot was collected in one data file. 66 Figure 9.5.3 Example 66 sample point to point‐oscillate motion profile RT: 0.00 - 1.36 SM: 7G
RT: 0.12
MA: 354851
100
95
0.59
RT: 1.03
MA: 347060
0.55
0.17
90
NL:
2.47E4
m/z=
530.35531.35
MS
bradykinin_
cv_osc_03
RT: 0.62
MA: 391154
0.88
85
0.71
80
0.27
75
0.46
0.21
0.75
0.80
1.18
1.08
0.84
1.10
1.27
1.24
0.35
70
0.96
0.37 0.39
0.40
65
Relative Abundance
1.05
0.98
0.66
0.33
60
1.13
0.95
55
50
45
40
35
30
25
20
15
10
5
1.34
0.03
0
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
Time (min)
0.8
0.9
1.0
1.1
1.2
1.3
Figure 9.5.4 Selected ion current of 10ng bradykinin [M+2H]2+ in triplicate using the point to point oscillate motion profile shown in Figure 9.5.3 Point to point – constant velocity (CV) The point to point – CV motion profile allows you to move the surface beneath the spray head at defined velocities and intervals. This feature is advantageous as it allows for rapid data collection and when scanning across 67 deposited samples, reproducible peak shapes for integration. The results of a typical point to point – CV experiment (a typical setup is shown in Figure 9.5.5) for consecutive 10ng deposits of bradykinin peptide standard are shown in Figure 9.5.6. The selected ion current for bradykinin at m/z 530.9±1 is displayed for an experiment with four consecutive spots. The data from all spot was collected in one data file. Figure 9.5.5 Example 96 sample point to point – constant velocity motion profile 68 RT: 0.00 - 2.00 SM: 7G
NL:
1.58E5
RT: 1.08
AA: 615484
100
RT: 0.60
AA: 570844
95
m /z=
530.38531.38
MS ICIS
bk_ptopcv_
05
RT: 1.58
AA: 630854
90
85
80
75
RT: 0.10
AA: 394590
70
65
Relative Abundance
60
55
50
45
40
35
30
25
20
15
10
5
0
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
1.1
Tim e (m in)
1.2
1.3
1.4
1.5
1.6
1.7
1.8
1.9
2+
Figure 9.5.6 Selected ion current of 10ng bradykinin [M+2H] in quadruplicate using a point to point continuous velocity scan 69 10 Maintenance The DESI 2D system requires little maintenance during normal use. During the initial system installation, system users will be trained in the proper maintenance and test procedures. This section details the routing cleaning and maintenance needs of the DESI system, including the replacement of the spray nozzle and spray head emitter. To minimize the risk of injury these procedures should be performed only by qualified and trained individuals knowledgeable of the risks of both the maintenance procedures and any samples/chemicals used with the system. CAUTION Maintenance and test procedures should only be performed by trained and qualified individuals. ATTENTION La maintenance et les tests de procédures doivent être effectués par un personnel de maintenance qualifié 10.1 General Cleaning During operation, the surfaces of the DESI 2D system may become soiled or contaminated. The system should be disconnected from the mass spectrometer and from power before cleaning. All surfaces of the DESI system may be wiped with a soft, lint free cloth or wiper dampened with water. For more aggressive contamination, a mild solvent such as 70% isopropanol in water may be used. Use caution when cleaning and do not oversaturate the wiper or otherwise flood the system with cleaning agents. Do not allow liquid to enter the AC/DC power supply or the control electronics. Instruments that have been used with biological samples or might otherwise contain biohazards, toxic, carcinogenic, mutagenic, corrosive, or irritating chemicals must be decontaminated prior to service work performed by the user or by Prosolia and its affiliates. Please contact Prosolia to discuss decontamination of the system. Always wear appropriate personal protective equipment (PPE), including gloves, lab coats, and safety glasses when decontaminating and servicing the system. Adhere to your institutions Chemical and Biological Safety Procedures when handling chemical and biological hazards, decontamination solutions, and waste. Follow all local regulations for the disposal of waste. 70 CAUTION Systems which are contaminated with biological, carcinogenic, mutagenic, corrosive, toxic, or irritant hazards must be decontaminated before servicing. ATTENTION Systèmes qui sont contaminés par des dangers biologiques, cancérigènes, mutagènes, corrosives, toxiques ou irritants doivent être décontaminés avant l'entretien. 10.2 Preventative Maintenance During the routine use of the DESI 2D system, the following items should be inspected on a daily basis to ensure the system is operating properly. 

Solvent supply tubing – Inspect tubing for damage, including kinks that may affect performance of the system. 2D Stage – Home the stage and exercise it in both directions observing movement for issues. The following should be inspected on a weekly basis: 

Electrical cables – Check cables for signs of wear or other damage. Replace as necessary. Exhaust tubing – Inspect the tubing for signs of deterioration from the spray solvent. Replace tubing as necessary. When the system is installed onto the mass spectrometer: 
Gas Plug O‐Rings – Check o‐rings for wear. Replace as needed. 10.3 Spray Head Nozzle/Emitter Replacement Please note that replacement of spray nozzle/emitter requires care and improper installation can affect the quality of the experimental results. Nozzles and emitters are delicate, handle with care. 1. Place the instrument in standby mode and ensure the high voltage is turned off 2. Turn off high pressure nitrogen gas to the system and allow time for the gas lines to depressurize 3. Remove the spray head from the DESI 2D system 4. Remove the gas connection from the spray head and unscrew the nozzle adapter/nozzle from the PEEK tee connector 71 a. If the spray head nozzle is being replaced, unscrew the nozzle using the 4 mm wrench provided b. Insert the new nozzle (with o‐ring) into the nozzle adapter and begin tightening by hand. Use caution to prevent cross threading parts. c. Tighten nozzle using the 4 mm wrench provided, until o‐ring is within the nozzle adapter d. Continue with emitter replacement/spray head reassembly 5. Remove and discard the old emitter from the PEEK sleeve 6. Inspect the o‐ring on the ferrule for signs of wear or cracking and replace if necessary 7. Using the 4 mm wrench provided, turn the spray nozzle clockwise until the rear of the wrench flats is flush with the front surface of the nozzle adapter as shown in Figure 10.3.1 Figure 10.3.1 Position of the nozzle within the nozzle adapter for replacement of the emitter 8. Carefully insert the new emitter through the aperture in the tip of the nozzle until approximately 3 mm is left protruding from the nozzle as shown in Figure 10.3.2 Figure 10.3.2 Emitter protrudes 3 mm from the nozzle 9. Carefully grip the emitter (avoid damaging the tip of the emitter) and the tip of the nozzle between your thumb and forefinger to prevent the emitter from moving while inserting the distal end of the emitter into the PEEK tubing sleeve 72 Figure 10.3.3 Insertion of the distal end of the emitter into the PEEK sleeve 10. Insert the sleeve and ferrule completely into the nozzle adapter and while holding the ferrule in place, gently push the emitter further into the nozzle 11. The distal end of the emitter should be made flush with the end of the PEEK sleeve protruding from the ferrule Figure 10.3.4 Positioning of the emitter at the end of the sleeve and ferrule 12. Assemble the nozzle adapter with the new emitter onto the tee connector while keeping the ferrule from moving Figure 10.3.5 Assembly of the spray head 73 13. Upon tightening, the proximal end of the emitter will protrude from the tip of the nozzle 14. Using the 4 mm wrench, turn the nozzle counter clockwise until the emitter protrudes approximately 1 mm beyond the tip of the nozzle. Figure 10.3.6 Adjustment of the emitter protrusion using a 4 mm wrench Figure 10.2.7 shows a disassembled spray head and its different components. Nozzle Adapter
PEEK TEE
Ferrule/Sleeve
Pt Electrode
Nozzle
Figure 10.3.7 Disassembled view of the DESI 2D System spray head 74 10.4 Spray Head Cleaning The spray head of the DESI 2D system can be cleaned if chemical contamination of the spray head is suspected. Care must be used to avoid damaging the o‐ring seals of the spray head. Simple cleaning of the outer surfaces of the spray head can be accomplished by wiping the spray head using a wipe saturated in methanol. The spray head must not be submerged in solvents. A complete cleaning of the spray head requires disassembly and removal of the o‐ring seals. All parts of the spray head can be cleaned by sonication in methanol except for the electrode assembly. After removing the spray head from the system, follow the procedure below to dissemble and clean the spray head. 1. Remove the platinum ‘liquid junction’ assembly from the tee by unscrewing the retaining nut and set aside 2. Remove the nut and ferrule from the liquid entry side of the tee and set aside 3. Unscrew nozzle adapter from tee 4. Remove 3 x 1.25 mm o‐ring from the ferrule behind the nozzle adapter and discard 5. Unscrew nozzle from the nozzle adapter. Remove the 1 x 3 mm o‐ring from the nozzle using pointed tweezers and discard 6. Remove spiral retaining ring from the nozzle adapter assembly by carefully prying end out of groove with sharp tweezers of a small screwdriver and remove using tweezers or small pliers. Use caution to avoid damaging PEEK parts 75 B
A
C
D
E
F
Figure 10.4.1 Removal of the spiral retaining ring (A and B) Carefully pry end of ring from groove at gap (circled) (C) End of ring pulled from groove (D) Using pliers to ‘unwind’ ring from groove (E) beginning to remove spiral ring (F) Ring removal near completion 7. Separate components of the nozzle adapter by twisting the outer ring while pulling pieces apart. Remove and discard o‐rings from this assembly 8. Place the spray head components into a beaker containing methanol. Sonicate parts for 10 minutes. IMPORTANT Do not sonicate the platinum ‘liquid junction’ assembly. IMPORTANT The spray nozzle is delicate, handle with care. Do not drop or otherwise bang the tip of nozzle against hard surfaces or damage may occur. 76 9. Remove components from methanol and allow to dry 10. Clean the platinum electrode by carefully rinsing only the tip of the electrode with methanol using a spray bottle When components of the spray head have been cleaned and allowed to completely dry, the spray head can be reassembled. It is suggested that new o‐rings be used upon reassembly. 1. Place new 7 x 1 mm o‐rings into the appropriate grooves on the nozzle adapter by gently stretching the o‐ring over the part Figure 10.4.2 Placing 7 x 1 mm o‐rings onto nozzle adapter 2. Place the slip ring component of the nozzle adapter over the barrel component with the chamfer facing the o‐rings as in Figure 8.3.3 77 Figure 10.4.3 The slip ring should be placed over the barrel with the chamfered edge facing the o‐ring to ease assembly 3. Push the slip ring component of the nozzle adapter over the barrel and o‐rings until it seats against the shoulder of the barrel. A gentle twisting of the ring will help to slip the ring over the o‐rings 4. Place a spiral retaining ring over the barrel of the nozzle adapter 5. The retaining ring can be started in the groove by gently pulling the end of the ring and stretching it into the groove. The remainder of the ring can then be stretched into the groove by gently pulling the ring into the groove working in a circle around the barrel 78 Figure 10.4.4 Replacement of the spiral retaining ring 6. Place a 3 x 1.25 mm onto the ferrule placed behind the gas adapter. 7. Continue assembly of the spray head as described in Section 10.3 79 10.5 Extended Transfer Capillary Cleaning During normal use, the extended ion transfer capillary will become dirty and require routine cleaning. While cleaning the capillary, it is important to handle the capillary with care to avoid bending or otherwise damaging the tube. Damage to the tube can lead to changes in the experiment geometry and can affect system sensitivity and performance. Before removing the system, allow the interface of the mass spectrometer to cool. 1. Reduce the interface temperature of the mass spectrometer and place in Standby mode. 2. Close the vacuum isolation valve on the mass spectrometer. 3. Using the 5 mm wrench provided, remove the extended ion transfer tube by rotating the base upwards until free. 4. Carefully remove the o‐ring and ion sampling cone from the backside of the extended ion transfer tube assembly. CAUTION Systems which are contaminated with biological, carcinogenic, mutagenic, corrosive, toxic, or irritant hazards must be decontaminated before servicing. ATTENTION Systèmes qui sont contaminés par des dangers biologiques, cancérigènes, mutagènes, corrosives, toxiques ou irritants doivent être décontaminés avant l'entretien. When cleaning the ion transfer tube, use appropriate PPE and dispose of all waste according to local regulations. For general cleaning, sonicate the capillary in an appropriate HPLC grade solvent for the samples/analytes the capillary has been exposed to. For more thorough cleaning, the following protocol can be used. 1. Sonicate in Alconox solution (prepared to the manufacturer’s directions) for 15 minutes with the tube pointed upwards in an appropriate container. 2. Rinse with clean tap water ensuring tube has been flushed. 3. (Optional) For parts with oxidation, sonicate in a Citranox solution (prepared to the manufacturer’s directions) for 15 minutes with the tube pointed upwards in an appropriate container. 4. Rinse with clean tap water ensuring tube has been flushed. 5. Sonicate in clean tap water for 10 minutes. 6. Rinse with HPLC grade water ensuring tube has been flushed. 7. Sonicate in HPLC grade water for 10 minutes. 8. Rinse with HPLC grade methanol. 9. Sonicate in HPLC grade methanol for 10 minutes. 80 10. Allow tubing to drain over the wash container. Dry accessible surfaces carefully with lint free wipes. 11. Reinstall onto the mass spectrometer following the instructions of Section 6.3. 10.6 Fuse Replacement Under normal operation, the fuses protecting the DESI 2D control electronics should not need replacing. Should the fuses of the control electronics burn out, follow the procedure below for proper fuse replacement. 1. Unplug the DESI 2D control electronics from the main power. Ensure there is no power to the unit before continuing 2. Using the flat head screwdriver provided with the system, turn the grey fuse cover counter clockwise until it springs out. 3. Pull the grey fuse cover out from the back of the control box. The fuse should come out with the cover. Insert screwdriver here
Figure 10.6.1 Removing fuse carrier from the fuse holder 4. Replace the blown fuse with the appropriate fuse for the voltage indicated on the enclosure (Nominal voltage = 400V DC, Current = 1A, Fuse = 5 X 20 MM Type T or equivalent (e.g. Littelfuse 0477001.MXP). See Section 11 for Prosolia part number. 5. Insert fuse and grey fuse cover back into the back of the control box. Using the screwdriver, push the grey fuse cover into the control box while turning clockwise to engage the cover back in place. 6. Reapply power to the control electronics. If the fuses continue to burn out, this is an indication of a larger problem with the electronics. Please contact Prosolia ([email protected]) for further assistance. 81 10.7 Decommissioning and Disposal The DESI 2D system must be properly prepared prior to disposal/recycling of the equipment. Spray solvents shall be emptied from the syringe and all tubing and disposed of according to local regulations. Wearing the proper PPE, the instrument must be decontaminated when exposed to chemical or biological hazards arising from samples or the spray solvents used prior to disposal or recycling to minimize risk of exposure to others. If the instrument cannot be properly and completely decontaminated, the system must be disposed of as hazardous waste following all applicable laws and regulations. Please contact Prosolia for additional information or with concerns on the safe disposal of the DESI 2D system. 82 11 Replacement Parts The following spare parts that can be ordered from Prosolia for use with the DESI 2D system. Please contact us for price and availability. Spray Head Item 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 Part Number P100‐00031‐01 P100‐00087‐01 P100‐00088‐01 P100‐00089‐01 P200‐00035‐03 P200‐00036‐02 P200‐00101‐01 P300‐00001‐01 P300‐00002‐01 P300‐00003‐01 P300‐00004‐10 P300‐00005‐01 P300‐00006‐01 P800‐00057‐01 P900‐00051‐05 Description Oring, 3X1.25mm, NB70 Retaining Ring, 3/8” Ext. Spiral Oring, 3X1mm, NB70 Oring, 7X1mm, NB70 Nozzle, Spray Head, SS, Rev C Spray Head Gas Adapter Rev B Slip Ring, Nozzle Gas Inlet Tee, Microtight, PEEK Nut, Microtight, 5/16‐24, PEEK Ferrule, Microtight, 0.025”, PEEK Sleeve, Microtight, 0.180mm, PEEK, 10 Pcs Nut, Short Vacutight, 10‐32 UNF, PEEK Ferrule, Vacutight, 1/16”, PEEK Assembly, Banana Plug Emitter, 0.05 X 0.15 X 40, Fused Silica, 5 ea 83 Capillary Extension Item 1 2 3 Part Number N/A P100‐00139‐01 P800‐10000‐28 Description Waters Ion Sampling Cone (Contact Waters for replacement)
Oring, 10X1.5, Viton Assembly, Bazooka Inlet ‐ Waters Xevo 2D Tools Part Number P900‐00101‐02 P900‐00102‐01 P900‐00112‐01 P900‐00113‐01 P900‐00114‐01 Description Wrench, 4mm X 5mm, Open Wrench, Hex Head, Metric, Set Insulated Hex Driver, 2.5 mm Insulated Hex Driver, 5/64 in Cutter, Fused Silica Omni Slide Sample Surfaces Part Number P900‐00015‐05 P900‐00016‐05 P900‐00018‐00 P900‐00020‐00 Description Slide, Omni Slide MT‐96, 5 pk. Slide, Omni Slide MT‐IMG, 5 pk. Slide, Omni Slide Micro‐24, 100 pk. Slide, Omni Slide Micro‐IMG, 100 pk. Chemical Standards Part Number P900‐00307‐01 P900‐00302‐01 Description Bradykinin Standard, 1 Milligram, Dry Sharpie, Fine Point, Red 84 Plumbing/Fluidics Part Number P300‐00200‐01 P300‐00030‐01 P300‐00015‐01 P300‐00004‐10 P300‐00018‐10 P300‐00013‐01 P300‐00011‐99 P300‐00047‐01 P300‐00010‐03 P300‐00016‐01 P300‐00017‐02 P300‐00029‐01 P800‐00271‐01 P100‐00086‐05 P100‐00088‐05 Description Syringe, 250 uL, Removable Needle, 22/2”/3 Union, Microtight Adapter,1/16”X1/32”, Red PEEK Union, 1/16”X0.007”, SS Sleeve, Microtight, 0.180mm, PEEK, 10 Pcs Sleeve, 1/16”X0.007”, FEP, 10 Pcs Tubing, 1/16” X0.030”X40mm, FEP Tubing, 0.05X0.150X1000 MM, FS Tubing, 1/32”X0.010”X1.5 M, PEEK Tubing, 1/16X0.30”X1.5 M, ETFE Nut, Fingertight, 1/16”, Delrin Ferrule, Fingertight, 1/16”, Tefzel Ferrule, Fingertight, 1/32”, PEEK Plug, Gas Port, Xevo Oring, 2.5X1mm, NB70, 5Pcs (small o‐ring for gas plug) Oring, 3X1mm, NB70, 5 Pcs (large o‐ring for gas plug) Electrical Part Number P400‐00349‐01 P400‐00037‐01 P400‐00038‐01 P400‐00039‐01 P400‐00040‐01 P400‐00302‐01 P400‐00311‐01 P400‐00075‐01 P400‐00042‐01 P400‐00094‐01 P800‐00013‐03 P800‐00131‐02 P400‐00045‐02 P800‐00066‐02 P400‐00074‐06 Description Fuse, 5 X 20 mm, 400VDC/1A, Type T Cord, USA/Japan, 10A/125V, 2 M Cord, UK, 10A/250V, 2.5M Cord, Europe, 10A/250V, 2.5M Cord, Australia, 10A/250V, 2.5M Cord, Swiss, 10A/250V, 2.5M Cord, China, 10A/250V, 2.5M USB Cable, 10 ft Cable, CCTV, BNC‐BNC, 10 ft 2‐D, 25 Pin D‐Sub Connector Cable Assembly, Camera, WAT‐704R w/Mirror Assembly, LED Lamp, 2D Waters Video Capture Card w/Ferrites Waters High Voltage Cable Assembly, I/O Cable, 2‐D Xevo 85 12 Troubleshooting This section details information on correcting issues or malfunctions with the DESI 2D system. If you experience a malfunction, this information will assist in identifying and correcting the problem. If you experience a problem not discussed in this section, please contact Prosolia’s technical support for more information. Hardware Errors The 2D sample stage has been designed for years of trouble free use. Common issues seen with the stage include binding due to damage, inability to home the stage in one or both axes, and erratic movements when the motor control cables in not completely plugged into the system. In all cases, these malfunctions do not present a hazard to the user and will not likely lead to permanent damage to the system. If you experience a malfunction, note the conditions leading to the malfunction including which axis is affected, if the error occurs during a particular function (such as homing), and any other relevant details before contacting Prosolia’s technical support for assistance. Common issues and suggested solutions are located below. No power Check power cable is properly inserted into the control electronic Ensure power cable is plugged into live power outlet Check that power switch is in the ON position Check fuses Check for obstruction
Ensure motor control cable is secured at both ends Power status lamp not lit Stage motion stalls Stage motion is erratic Stage does not stop trying to Home limit needs adjustment. Contact Prosolia for details.
move when the home position is reached Ensure motor control cable is secured at both ends
86 Communications Errors The DESI 2D system must be in constant communication with the control software for operation. The connection and communication requirements are discussed in Section 7 of this manual and in the Omni Spray Ion Source 2‐D Automation Software Installation and Reference Manual. Communications Error Check that power switch is in the ON position Check that USB is properly inserted into both the control electronics and the computer Ensure the control electronics are plugged into a root USB port, not through a USB hub Experimental Errors Some common experimental issues are noted below. For more detailed troubleshooting information on system performance as well as application dependant information, application notes, and other reference information, please visit Prosolia’s website at www.prosolia.com. Synchronization error – sample Adjust pre‐acquisition delay parameter (Pre_Acq) in the moves to analysis position motion parameters window to a shorter time period before data acquisition begins Synchronization error – sample Adjust pre‐acquisition delay parameter (Pre_Acq) in the moves to analysis position after motion parameters window to a longer time period data acquisition begins Synchronization error – Adjust post‐acquisition delay parameter (Post_Acq) in the Instrument not ready when motion parameters window to a longer time period trigger is sent Weak/no signal recommended standards for Ensure the syringe pump is ‘ON’ and the spray solvent is flowing Ensure nitrogen gas pressure is sufficient and gas is flowing Check that the capillary emitter is protruding out of the nozzle according to the recommendations in Section 5.3. Ensure all operating parameters are similar to the recommendations in Section 9.1 Ensure instrument is functioning properly (tuned and calibrated If the above suggestions do not solve issues related to the DESI 2D System or control software, please contact Prosolia ([email protected]) for further assistance. 87