LDTD Ionization Source Model S-960 Operating Manual PT.MI.01 Revision G
PhytronixTechnologienc.
337 Saint-Joseph Est Québec (Québec) G1K 3B3 Phone : (418) 692-1414 Copyright 2009 by Phytronix Technologies inc.
LDTD – model S-960
Table of contents TABLE OF CONTENTS............................................................................................................................................. 1 FIGURES LIST............................................................................................................................................................ 3 ABOUT THIS MANUAL ............................................................................................................................................ 4 VERSIONS................................................................................................................................................................... 4 OBJECTIVE OF THIS MANUAL...................................................................................................................................... 4 COMMENTS ................................................................................................................................................................ 4 LIMITED WARRANTY ............................................................................................................................................. 5 SERVICE...................................................................................................................................................................... 5 WARNING ................................................................................................................................................................... 6 SECURITY ................................................................................................................................................................... 6 REGULATORY COMPLIANCE ....................................................................................................................................... 6 LASER ........................................................................................................................................................................ 7 LASER INDICATOR ...................................................................................................................................................... 8 LDTD SAFETY INFORMATION.................................................................................................................................... 8 WASTE ELECTRICAL AND ELECTRONIC EQUIPMENT DIRECTIVE ................................................................................ 9 SETUP......................................................................................................................................................................... 10 OBJECTIVE ............................................................................................................................................................... 10 INTRODUCTION ........................................................................................................................................................ 10 COMPONENTS........................................................................................................................................................... 11 PACKING LIST........................................................................................................................................................... 12 CONDITION OF OPERATION ....................................................................................................................................... 12 GETTING STARTED ............................................................................................................................................... 13 INTRODUCTION ........................................................................................................................................................ 13 INSTALLING THE LDTD FROM THE MASS SPECTROMETER ....................................................................................... 13 REMOVING THE LDTD FROM THE MASS SPECTROMETER ......................................................................................... 14 Caution ............................................................................................................................................................... 14 Procedure ........................................................................................................................................................... 14 GAS CONNECTION .................................................................................................................................................... 14 CONNECTING THE EC BOX AND THE LDTD ............................................................................................................. 15 CORONA DISCHARGE ................................................................................................................................................ 17 LAZSOFT .................................................................................................................................................................. 17 LAZSOFT INSTALLATION .......................................................................................................................................... 17 Computer ............................................................................................................................................................ 17 Instructions......................................................................................................................................................... 17 ANALYST® HARDWARE CONFIGURATION ................................................................................................................. 18 USING THE LDTD ................................................................................................................................................... 23 INTRODUCTION ........................................................................................................................................................ 23 LAZWELL : DESCRIPTION ......................................................................................................................................... 23 Indexation........................................................................................................................................................... 24 SAMPLE LOADING INTO LAZWELL ........................................................................................................................... 24 LOADING THE LAZWELL .......................................................................................................................................... 25 LAZSOFT .................................................................................................................................................................. 26 Introduction ........................................................................................................................................................ 26 Convention.......................................................................................................................................................... 26 Manual Execution v4.2 ....................................................................................................................................... 27
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LDTD – model S-960 ANALYST WINDOW ................................................................................................................................................ 31 LDTD Template .................................................................................................................................................. 31 Export Analyst® batch for LazSoft...................................................................................................................... 32 LazSoft Batch v4.1 .............................................................................................................................................. 33 OPERATING CONDITIONS................................................................................................................................... 37 INTRODUCTION ........................................................................................................................................................ 37 LDTD PARAMETERS ................................................................................................................................................ 37 Carrier gas flow ................................................................................................................................................. 37 Laser pattern ...................................................................................................................................................... 37 MASS SPECTROMETER PARAMETERS........................................................................................................................ 39 CONSUMABLE AND REPLACEABLE PARTS................................................................................................... 41 INTRODUCTION ........................................................................................................................................................ 41 ACCESSORIES AND SERVICES ................................................................................................................................... 41 LDTD SOURCE BOX ................................................................................................................................................. 41 EC BOX .................................................................................................................................................................... 41 CABLES .................................................................................................................................................................... 41 MANUALS ................................................................................................................................................................ 41 MAINTENANCE ....................................................................................................................................................... 42 INTRODUCTION ........................................................................................................................................................ 42 GENERAL CAUTION .................................................................................................................................................. 42 GAS FLOW VERIFICATION ......................................................................................................................................... 42 Procedure ........................................................................................................................................................... 42 LASER IRRADIATION POSITIONING............................................................................................................................ 42 Introduction ........................................................................................................................................................ 42 Procedure ........................................................................................................................................................... 43 X-Y STAGE POSITIONING ......................................................................................................................................... 44 Caution ............................................................................................................................................................... 44 Procedure ........................................................................................................................................................... 44 TRANSFER TUBE CLEANING ...................................................................................................................................... 45 Introduction ........................................................................................................................................................ 45 Procedure ........................................................................................................................................................... 45 TROUBLESHOOTING ............................................................................................................................................ 46 INTRODUCTION ........................................................................................................................................................ 46 FAULT MESSAGES..................................................................................................................................................... 46 FAULT MESSAGE LIST ............................................................................................................................................... 46 TROUBLESHOOTING PROCEDURE .................................................................................................................. 50 INTRODUCTION ........................................................................................................................................................ 50 GENERAL CAUTION AND WARNING .......................................................................................................................... 50 PROCEDURE FOR GAS LEAK DETECTION ................................................................................................................... 51 Procedure ........................................................................................................................................................... 51 PROCEDURES FOR LAZWELL STUCK IN X-Y STAGE ................................................................................................. 52 Introduction ........................................................................................................................................................ 52 Procedure ........................................................................................................................................................... 52 INDEX......................................................................................................................................................................... 54
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LDTD – model S-960
Figures list Figure 1 : Loader front panel and the green indicator....................................................................8 Figure 2 : LDTD model S-960 with loader. ...................................................................................11 Figure 3 : LDTD EC box................................................................................................................11 Figure 4 Rear view of the LDTD housing including the guide pins and the locking levers. ........13 Figure 5 : Laser diode protection A) Disconnected EC box to laser head cable from the LDTD and B) Connected laser diode protection plug...............................................................................14 Figure 6 : Side view of the LDTD A) pneumatic gas line inlet and B) carrier gas line inlet. .......15 Figure 7 : EC box back panel : (A), EC box to laser head cable, (B) Carrier gas outlet, (C) Pneumatic gas outlet, (D) Main gas line inlet, (E) Power cable, (F) EC box to station COM cable, (G) EC box to source DB25 cable connection and (H) EC box to MS start cable..............16 Figure 8 : EC box to source DB25 cable connected under the LDTD box....................................16 Figure 9 : Corona discharge needle positioning ...........................................................................17 Figure 10 Profile creation in Hardware configuration for LDTD ...............................................18 Figure 11 Synchronization Trigger selection for the Mass Spectrometer LDTD device setup. ...19 Figure 12 The Autosampler CTC Pal device addition to the MassSpecLDTD profile. ................19 Figure 13 Simulation mode selection for the Autosampler device setup ......................................20 Figure 14 MassSpecLDTD activation profile window..................................................................20 Figure 15 Synchronization mode selection in the Acquisition Method Properties.......................21 Figure 16 Source Temperature selection. .....................................................................................22 Figure 17 : LazWell........................................................................................................................23 Figure 18: LazWell and A1 position. .............................................................................................24 Figure 19 : Manual sample deposition in a LazWell. ....................................................................24 Figure 20 : LazWell insertion in the loader...................................................................................25 Figure 21 LazSoft Manual Execution v4.1 window. .....................................................................27 Figure 22: LazSoft Manual Execution v4.1 window, Open Laser Pattern. ...................................29 Figure 23: LazSoft Manual Execution v4.1 window, Laser Pattern Editor...................................29 Figure 24 LazSoft Manual Execution v4.1 window, Laser Pattern Editor, how to delete a laser pattern step (row). ..........................................................................................................................30 Figure 25 : Analyst window and the LDTD batch template.........................................................31 Figure 26 : LazSoft Batch v4.1 window .........................................................................................33 Figure 28 : Laser pattern examples. A) low heat, B) medium heat and C) high heat. ..................39 Figure 29 Adequate laser irradiation impregnation view from the inside of a well.....................43
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LDTD – model S-960
About this Manual Versions There are different versions of this manual dependently of the mass spectrometer on which the LDTD is installed. The following table presents the identification numbers of the various operating manuals associated with the different mass spectrometers available on the market. Table 1 : Operating Manual identification number for the different mass spectrometer available on the market.
LDTD model S-960 T-960 W-960 A-960
Operating Manual identification number PT.MI.01 PT.MI.02 PT.MI.03 PT.MI.04
The user must ensure himself to have in hand the good identification number of the Operating Manual.
Objective of this manual Installation and operation of the LDTD are presented in this manual. It includes a description of the LazSoft software accompanying the source as well as a guide for the user in order to realize all the steps before performing a first experiment. Maintenance and troubleshooting procedures are also included in this manual.
Comments Your opinion is important to us and may improve the content of this manual. You can send your comments to the Phytronix Technologies team at the following coordinates : Phytronix Technologies 337 Saint-Joseph Est Québec (Québec) G1K 3B3 Phone : (418) 692-1414 Fax : (418) 692-4940
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LDTD – model S-960
Limited Warranty Phytronix Technologies warrants that the product will be free from defects in materials and workmanship under normal use for one year from the date you receive it. If Phytronix Technologies repairs or replaces a part or the product, its limited warranty term is not extended. This limited warranty is void if any damage has resulted from accident, abuse, misapplication, or service or modification by someone other than Phytronix Technologies. This warranty is limited to the buyer and is not transferable. This limited warranty gives you specific legal rights; you may have others, which vary from jurisdiction to jurisdiction. LDTD is patented in US since January 22nd 2008. LDTD, LazSoft and LazWell are all trademarks of Phytronix Technologies.
Service Our service policy has been designed to offer a suitable service when a problem is encountered with the product. For any question concerning the analytical performances of the source or for any technical problem, please contact Phytronix Technologies team at the following coordinates: Phytronix Technologies inc. 337 Saint-Joseph Est Québec (Québec) G1K 3B3 Phone : (418) 692-1414 Fax : (418) 692-4940
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LDTD – model S-960
Warning Throughout this manual, the following symbol is used to call reader’s attention.
Security Regulatory compliance Phytronix Technologies inc. performs complete testing and evaluation on LDTD model S-960 to ensure full compliance with applicable domestics and international regulations. When your system is delivered to you, it meets all pertinent electromagnetic compatibility (EMC) and safety standards as follow: EMC Certification EN 55011 EN 55014 EN 61000-3-2/3 EN 61000-4-2 EN 61000-4-3 EN 61000-4-4
(2002) (2002) (2002) (2002) (2002) (2002)
EN 61000-4-5 EN 61000-4-6 EN 61000-4-8 EN 61000-4-11 FCC Class A
(2002) (2002) (2002) (2002)
EMC issues have been evaluated by CSA International. Safety Compliance Low Voltage Directive EN 61010-1:2001 Laser Compliance IEC 60825-1 Please be aware that any changes make to your system might void compliance with one or more of these EMC and/or safety standards. Making changes to your system includes replacing a part. Thus, to ensure continued compliance with EMC and safety standard, replacement parts should be ordered from Phytronix Technologies inc. or one of its authorized representatives.
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LDTD – model S-960
FCC compliance statement This equipment has been tested and found to comply with the limits for Class A digital device, pursuant to part 15 of the FC rules. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment. This equipment generates, uses, and can radiate radio frequency energy. If it is not installed and used in accordance with the instrument operating manual, it might cause harmful interference to radio communications. Operation of this equipment in a residential area is likely to cause harmful interference. In this case, the user will be required to correct the interference at his/her own expense.
Laser The LDTD is certified as a Class 1 instrument but contains a Class 4 embedded laser diode. The LDTD is equipped of safety interlocks and require being couple to end system (when properly coupled to a mass spectrometer) to prevent access to potential user to Laser Radiation exceeding Class 1. These safety interlocks should never be override to prevent potential exposition to laser irradiation (20 Watt).
Removing the LDTD from the mass spectrometer will shot down the laser beam operation. This security should not in any case be override by anyone. Case opening may expose the user to laser radiations and induced serious wounds. Only a certified technician can open the LDTD case. The safety interlocks should never been override by anyone. The case should not be open under any consideration when the electronic control (EC) box power cable is connected.
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LDTD – model S-960
Laser indicator The loader blue front panel is provided with a luminous led. When the LDTD is under tension the led is green (Figure 1), and when the laser is in function, it turns red. In the same way, LazSoft contains a visual indicator indicating the operation of the laser.
Figure 1 : Loader front panel and the green indicator.
LDTD Safety information •
Do not put any instrument that release heat above or below the EC box. Heat could damage the electronic components of the source.
•
Always connect the source to a properly grounded electrical outlet.
•
Disconnect the EC box power cable before opening the source.
•
Disconnect the EC box power cable before any repair or maintenance.
•
Before disconnecting the EC box, put the switch at the OFF position to avoid damaging the electronics of the system.
•
Operating procedure, practice, or the like, which, if not correctly performed or adhered to, could result in damage to the product. Always use a LazWell in the ionization source.
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LDTD – model S-960
Waste Electrical and Electronic Equipment Directive Phytronix Technologies has launched a formal product disposal Take-Back and Recycle Program that complies with the European Union Directive 2002/96/EC on Waste Electrical and Electronic Equipment, also known as the "WEEE Directive".
This program will provide self-service instructions for ease of use product takeback and recycling. Equipment that is returned through this program will be handled in an environmentally safe manner using processes that meet the WEEE Directive requirements. This program is for Phytronix Technologies customers who have Phytronix Technologies products that have reached the end-of-life. To know more about Phytronix Technologies WEEE directive contact us.
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LDTD – model S-960
1
Setup
Objective The objective of this chapter is to present the laser diode thermal desorption (LDTD) ionization source for mass spectrometer and its components. All the instructions necessary for the source installation are described and must be performed before using the ionization source.
Introduction This introduction contains a short description of the product as well as an overview of different applications. In the LDTD, samples are thermally desorbed indirectly by a laser. The desorbed neutral compounds are ionized by a corona discharge under atmospheric pressure conditions. The LDTD may be coupled to any mass spectrometer to determine qualitatively and quantitatively the chemical composition of various samples. The unit is made of two components, the source and its electronic control (EC) box. The LDTD is operated by software called LazSoft described later in the document. This software is used to control certain parameters necessary to operate the ionization source and can either be operated in manual mode or in sample batch mode. There are various mechanical adapters of the LDTD, allowing the ionization source to be installed on different mass spectrometers. The LDTD, combined with a mass spectrometer analyzer, may be use in different analytical field such as in environmental, pharmaceutical and food industries.
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LDTD – model S-960
Components The LDTD thermally desorbs neutral species from a dry sample by the interaction of an IR laser with the sample support material and carries them through a transfer tube into a corona discharge region where they are ionized under atmospheric pressure conditions. Formed ions finally enter into the mass spectrometer. The LDTD is equipped with a LazWell (96-well) plate loader that may charge up to 10 plates (see Figure 2).
Figure 2 : LDTD model S-960 with loader.
The LDTD electronic control (EC) box (Figure 3) contains the power supply unit, analogical circuits for the diode laser current and the temperature, gas flow control and embedded processing unit to ensure a real time operation of the source.
Figure 3 : LDTD EC box.
The LazSoft controls both components.
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LDTD – model S-960
Packing list • • • • • • • • • • • • •
LDTD with laser head transport connector EC box LDTD box Polyethylene tubing (1/4 inc. and 12 feet long) Swagelok union 1/4 inch. EC box to laser head cable EC box to source DB25 cable EC box to station COM cable EC box to MS cable Power cable LazWell (minimum of 5 plates) Operation manual Installation CD for the LazSoft The LDTD will arrive at your site packed in one large box, including one or more smaller boxes. Check if all the components mentioned on the FC.05.07 form are present in the box at reception. Check that the received components are in good condition. If it is not the case, please contact Phytronix Technologies immediately.
Condition of operation The LDTD has to be used under those conditions : • • • • • •
Pollution degree 2 class equipment ; Maximum altitude of operation at 2000 m ; Maximum relative humidity of 80 % at temperature up to 31 oC with decreasing linearly to 50 % at 40oC ; Temperature : 5 to 40 ºC ; Indoor use only ; Electrical supply 100-240 Vac ± 10 % Vac, 50/60 Hz and 275 VA.
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LDTD – model S-960
2
Getting Started
Introduction Phytronix Technologies will install the LDTD system on site following its purchase. However, the present section describes procedure you may need to remove, install or move the LDTD.
Installing the LDTD from the mass spectrometer To install the LDTD, follow these steps and make sure to remove the ionization source already present on the mass spectrometer before installing the LDTD : • • • •
Carefully align the two pins on the rear of the LDTD (Figure 4) with the ion source housing guide pinholes on the mass spectrometer. Carefully press the LDTD onto the ion source housing on the mass spectrometer. Rotate the LDTD locking levers 180 degrees to lock the LDTD onto the mass spectrometer. Unplug the Laser Diode Protection plug on the laser assembly (Figure 5). Connect the EC box to laser head cable, the carrier gas tubing line and the pneumatic tubing line (see Figure 6 for the gas line connections). Locking lever(s) Guide pin(s)
Figure 4 Rear view of the LDTD housing including the guide pins and the locking levers.
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LDTD – model S-960
Removing the LDTD from the mass spectrometer You need to remove the LDTD housing as follow before installing any other ion source or for any maintenance on the LDTD. Caution Removing the LDTD from the mass spectrometer will shutdown the laser operation. This security should not be bypassed by anyone in any case. It is important to understand and follow the troubleshooting procedure, including the disconnection of the EC box to laser head cable. Procedure • • • • •
Turn OFF the EC box power. Disconnect the EC box to laser head cable from the source side (Figure 5). Connect the laser diode protection connector on the source (Figure 5). Rotate the LDTD locking levers 180 degrees to release the LDTD from the mass spectrometer. Remove the LDTD by pulling it straight off the mass spectrometer, and place the LDTD in a safe location for temporary storage.
A
B
Figure 5 : Laser diode protection A) Disconnected EC box to laser head cable from the LDTD and B) Connected laser diode protection plug.
Gas connection The main gas line (entering into the EC box) is split inside the EC box to feed two gas lines. One gas line is called the carrier gas line to carry the sample from the LDTD to the MS inlet and the second gas line is use for the pneumatic components. The gas line connections are shown in Figure 7.
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LDTD – model S-960
A
B
Figure 6 : Side view of the LDTD A) pneumatic gas line inlet and B) carrier gas line inlet.
The main gas is connected on the back panel of the EC box and on the side of the LDTD with a Swagelok 1/4 inch. female connector (Figure 7). It is recommended to use medical grade compressed air containing 20.9 % of oxygen (± 1 %) and at least 10 ppmv of water (H2O). The presence of water and oxygen is necessary for positive and negative ionization respectively. Any equivalent gas could also be used. The recommended pressure at the EC box inlet is 60 to 80 psi. Do not use ultra dry compressed air.
Connecting the EC box and the LDTD The LDTD system is exclusively controlled by the LazSoft. Thus, there is no control button on the EC box front panel and on the LDTD. The EC box to laser head cable (D) and the EC box to station COM cable (A or F) are located on the back panel of the EC box (Figure 7). Power cable (E), and gas lines inlet (G) and outlet (H) are also located on the back panel of the EC box, while the gas line inlet are connected on the side of the LDTD (Figure 6) and the EC box to source DB25 cable (C) is located under the LDTD (Figure 8). To connect the EC box to MS (ready, start) cable (B) to the mass spectrometer, see the specifications of the MS for localization. Connections are identified on Figure 7 and Figure 8. Before connecting the cables, check that the power cable provided with the EC box is compatible with the facility electrical installation.
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LDTD – model S-960
Fan
B
A
E
Switch ON/OFF
F
B
D
C
H
G
Figure 7 : EC box back panel : (A), EC box to laser head cable, (B) Carrier gas outlet, (C) Pneumatic gas outlet, (D) Main gas line inlet, (E) Power cable, (F) EC box to station COM cable, (G) EC box to source DB25 cable connection and (H) EC box to MS start cable.
Figure 8 : EC box to source DB25 cable connected under the LDTD box.
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LDTD – model S-960
Corona discharge The corona discharge region is located at the end of the transfer tube inside the LDTD housing, on the backside of the LDTD. A corona discharge needle is used to generate the discharge for the ionization. The corona discharge must be properly positioned, as presented in Figure 9.
Corona discharge needle Transfer tube To MS
4 mm
Figure 9 : Corona discharge needle positioning
LazSoft LazSoft allows controlling the different LDTD parameters. It also synchronize the MS acquisition with the laser desorption. Two operating mode are available, one for the manual operation of the LDTD and a second to performed automated analysis. A complete chapter is devoted to the control and the use of the LazSoft.
LazSoft installation Computer System requirements : • •
Windows 2000 or XP. system. RAM: 256 Mo
It cannot be installed on Window NT operating
Instructions Insert CD and follow instructions.
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LDTD – model S-960
Analyst® Hardware configuration The user must create a new Profile in the Hardware configuration windows of Analyst® with two (2) Device as follow : In Hardware Configuration the user must create a New Profile (named MassSpecLDTD). Under this Profile, the user must click on Add Device, and the user will have to select Mass Spectrometer and click OK (Figure 10).
Figure 10 Profile creation in Hardware configuration for LDTD
Once the Mass Spectrometer device is created the user must setup this device (Figure 11). The Synchronization Trigger must be set to Active low (Figure 11).
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LDTD – model S-960
Figure 11 Synchronization Trigger selection for the Mass Spectrometer LDTD device setup.
The second device under the MassSpetLDTD profile should be an Autosampler CTC Pal (Figure 12).
Figure 12 The Autosampler CTC Pal device addition to the MassSpecLDTD profile.
Once the Autosampler device is created the user must setup this device (Figure 13). In the Advanced window (Figure 13) the Simulation Mode should be selected.
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LDTD – model S-960
Figure 13 Simulation mode selection for the Autosampler device setup
The last action will be to Activate the Profile (Figure 14).
Figure 14 MassSpecLDTD activation profile window.
In addition to the creation of the LDTD instrument profile, the user should select two more hardware specifications for the proper communication and operation of the LDTD. 1. Under Acquire, Build Acquisition Method select Acquisition Method. In the Acquisition Method Properties window select LC Sync as Synchronization Mode (Figure 15).
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LDTD – model S-960
Figure 15 Synchronization mode selection in the Acquisition Method Properties.
2. Under Acquire, Build Acquisition Method, select Acquisition Method and then select Mass Spec. In Edit Parameters, set the Temperature (TEM) under Source/Gas to 22 (Figure 16).
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LDTD – model S-960
Figure 16 Source Temperature selection.
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LDTD – model S-960
3
Using the LDTD
Introduction This chapter presents the different steps required to analyze a sample with the LDTD : • • • • •
The LazWell Sample preparation LazWell loading in the source LazSoft Analyst parameters
LazWell : description LazWell (Figure 17) has been designed to correspond entirely to the 96-wells standards established by the industry. However, LazWell is specifically designed for the LDTD. The plates are identified by bar code located on the edge side of the plate. This bar code is read by the LDTD automatically for GLP purpose. LazWell are ready to use when received.
Figure 17 : LazWell.
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LDTD – model S-960
Indexation The LazWell has different points of reference (Figure 18). The plate enters only in one way in the LDTD loader where the bar code should be readable by the user (Figure 20). The A1 position is the one located near the semi-truncated corner. 1 A
A1
2
3
3
4
4
5
5
6
6
7
7
8
8
9
9
10
1
11
1
12
1
B C D E F G H
Figure 18: LazWell and A1 position.
Sample loading into LazWell Sample deposition can be made automatically via an automatic preparation system or it can be done manually (Figure 19). The sample is deposited (1 to 10 µL) and dried at room temperature into the well. Drying time may vary depending of the solvent used to prepare the sample. Sample preparation environment should be free from dust. Unloaded LazWell should be protected from dust at all time and from light in case of photosensitive sample.
Figure 19 : Manual sample deposition in a LazWell.
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LDTD – model S-960
Loading the LazWell The user must position the plate with its bar code upwards as shown in Figure 20. The loader may handle 1 to 10 plates. Loading a plate will automatically eject the previously loaded plate in the LDTD. A door located beneath the LDTD will open and the plate will be ejected. It is recommended to place the used LazWell containers provided beneath the LDTD to avoid plate drooping on the floor. LazWell has to be inserted with the bar code upwards.
Figure 20 : LazWell insertion in the loader.
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LDTD – model S-960
LazSoft Introduction The LazSoft is divided in tree (3) sub-software : LazSoft Manual Execution, LazSoft Batch, and LazConfig. This latter software being installed for maintenance and service only and the user needs to contact Phytronix Technologies service team to require procedure to use it. The LazSoft Manual Execution is a software tool for LDTD method development. It allows the user to create laser desorption patterns and to optimize the gas flow while the MS inlet parameters are optimized by the MS software in the same way the user would proceed with another ionization source. The LazSoft Batch allows the user to analyze batch sample by importing the sequence previously created in Analyst by taking care to add specific information on the plate bar code number, the laser pattern and the gas flow.
Convention The following text concerning the software explanations adopts the following convention: Bold : bold characters indicate that the user can click on them Italic : italic characters indicate that the user may enter a specific value Underlined : underlined characters indicate the state of the system. There is no way to modify those data.
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LDTD – model S-960
Manual Execution v4.2 Manual execution window (Figure 21) is used to manually define and optimize the parameters of the sample desorption. It is appropriate to use the Manual Execution to analyze one or few samples. Manual Execution is also very helpful for method development. Here is a view of the Manual Execution window and a brief description :
Figure 21 LazSoft Manual Execution v4.1 window.
A) LazWell displacement panel • LazWell displacement : LazWell displacement tool. Each well can be selected manually by clicking with the cursor on the wanted well position. Following the LazWell displacement, the schematic well turns blue and the position is shown in the Actual position space. • Actual position : Well selected from the LazWell. Each well is identified by A to H and by 1 to 12. Well number is also indicated. For example, B2 corresponds to position 14. • Home : The positioning system goes directly to the mechanical alignment position (different from A1) then positions itself at the A1 position. • Load/Eject : Use to load a LazWell and/or to eject a LazWell.
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LDTD – model S-960
• Serial number : LazWell serial number (6 digits bar code). • Displayed used wells : Clicking in the check box will display, in red, the wells that have already being shoot by the Laser diode on the loaded LazWell. • Gas Temp : Carrier gas temperature status. The heating cartridge temperature is set to 50 °C as default. When this temperature is reach and maintains within 1 °C the indicator is Green. The temperature indicator turns red when the temperature is outside the tolerance. • Gas Flow : Carrier gas flow in L/min. This can be modified by the arrows. The Gas Flow indicator flickers red/blue when the interval of gas flow observed between the desired value and the one read is higher than 1.0 L/min. • MS Start : The user can manually start the mass spectrometer acquisition. B) Laser panel Laser • This visual indicator becomes red when the laser is in function. The laser diode power in real-time is displayed into the status window. • Start : This button starts the laser desorption pattern according to preset parameters. Laser Pattern • The user may open, or edit a laser desorption pattern. By clicking on the Open button the user will be asked to select the laser desorption pattern (Figure 22). To edit (create or modify) a laser desorption pattern, the user click on the Editor button. The actual laser pattern will open (Figure 23) and the user will have the opportunity to modify the laser pattern. To delete a laser step (row) the user must right click and select delete row (Figure 24). Once the pattern is edited, the user may Save the pattern on its actual name or save the laser pattern as a new file (Save as). • Laser power(%) vs Time(s) : This graph represents ramp/plateau laser power according to time for the experiment in progress. When the diode laser is in function, a yellow cursor on the graph moves according to the progress of the experiment.
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LDTD – model S-960
Figure 22: LazSoft Manual Execution v4.1 window, Open Laser Pattern.
Figure 23: LazSoft Manual Execution v4.1 window, Laser Pattern Editor.
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LDTD – model S-960
Figure 24 LazSoft Manual Execution v4.1 window, Laser Pattern Editor, how to delete a laser pattern step (row).
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LDTD – model S-960
Analyst Window In order to analyze batch sample, the user should create a sequence in the Analyst software. When this operation is performed for the first time, the user should open the LDTD batch template (instruction will follow) which contains the proper field for the LDTD. The user will then create the appropriate sequence as usual with the exception of the following field which need to be fill (Figure 25) :
1
2
3
4
Figure 25 : Analyst window and the LDTD batch template.
1
Vial Position : Sample position in the LazWell (1 to 96).
2
Laser pattern : File name in the « Pattern editor » (from LazSoft).
3
Gas Flow : Carrier gas flow in L/min. Determined by the user.
4
Serial number : LazWell serial number.
LDTD Template A template is available with the proper fields for the use of the LDTD in : \program files\LazSoft 4.2\LazSoft 4.2 template.dab.
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LDTD – model S-960
Export Analyst® batch for LazSoft The Analyst® batch needs to be exported as text (.txt) file to be handle by the LazSoft Batch as follow : •
In the Batch Editor, click on File then on Export. Give a name to the batch file and save it. This .txt file will then be imported in the LazSoft Batch (see next section for more information).
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LDTD – model S-960
LazSoft Batch v4.1 LazSoft Batch is used to analyze batch samples according to the LDTD operating conditions (laser pattern and carrier gas flow) previously developed in the manual execution mode and to the sequence created in the Analyst (see p. 17 for further information on Analyst sequence). Here is a view of the LazSoft Batch window (Figure 26) separated in two main parts, one showing sample and operating condition information and the other following-up the experiment in real time. Some brief descriptions of the window’s functionalities are also presented.
Figure 26 : LazSoft Batch v4.1 window
A) Import Batch: LazSoft imports the mass spectrometer software data for an acquisition batch. By clicking on this button, the software will open the open sequence file window. The user selects the right sequence file from Analyst® (.txt file). The imported Batch information will be displayed as follow : • Identification : Sample name as defined in the mass spectrometer software. • LazWell serial number • Position : Well position corresponding for the sample on the LazWell. • Laser Pattern : The pattern that will be used to analyze the corresponding sample. It can be edited from the Manual Execution window.
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LDTD – model S-960
• Gas Flow : The value, associate to each sample, will appears when the analytical sequence will be started. NOTE : All these information are imported from the sequence created in Analyst. They cannot be changed in the LazSoft window. To modify any parameters, the user should do the modification in the created sequence in Analyst and imported the new sequence into LazSoft Batch. B) Start / Pause / Abort • Start : To start acquisition click on the Start button. If the plates inserted in the loader are in a different order than the one defined in the LazSoft Batch, an error message will appear: « Expected LazWell is different than the loaded ». The user will have the choice to modify the order in the loader (Load Next) or to abort the sequence (Abort). NOTE : When clicking on Start, two files (.txt) are recorded in the same directory then the batch template .txt file. The file names are as follow : LDTDBatch-BatchFileName-YYYYMMDD-HHMMSS.txt and LDTDBatch-BatchFileName-YYYYMMDD-HHMMSSchk.txt. The first file contains all the information regarding the launch bath (sample name, sample position, laser pattern, gas flow and serial number) and the second is the checksum associate to that file. Therefore, the date-time information containing in the file name might be used to trace the launch batch information. •
Pause : Clicking on the Pause button will pause the sequence at the end of the sample being analyzed at the moment the button have been click on. To resume the sequence, the user needs to click back the Pause button.
•
Abort : Stop an acquisition at any time. All data acquired before the abort procedure are saved. LazSoft will ask the user to eject the plate.
C) Sample acquisition selection •
The user have the choice between tree ways to synchronize the data acquisition with the mass spectrometer software leading to tree ways to acquire the data : i-One sample / data file : This default setting will synchronize the sample analysis of the LDTD with the data acquisition of the mass spectrometer software leading to 1 data file per sample.
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LDTD – model S-960
•
On the two following settings, the user will have to create 2 different sequences in Analyts®. One sequence with all the samples as usual (export as .txt and imported in LazSoft Batch) and one sequence that will be submit in Analyst®. The way to built the sequence that will be submit in Analyst® depend on the user selection : i-All samples / data file : With this settings, the user will have to submit a sequence in Analyst® with only 1 sample but with an associate acquisition method where the run time should be long enough to acquire all the sample and record them in a single file. ii-One plate / data file : With this settings, the user will have to submit in Analyst® a sequence with the number of sample matching the number of LazWell. The associate acquisition method run time should be long enough to acquire all the samples contained in the LazWell in a single data file. Therefore, 1 data file will be created for each analyzed LazWell plate samples.
D) LazWell sample layout Identified by A to H and by 1 to 12, this schematic plate corresponds to the inserted LazWell in the LDTD loader. Blue colored wells correspond to well containing a sample and once the analysis is completed a white X appears. E) Task progress indicates the number of analyzed sample in the batch sequence. F) Stabilization delay : This function allows to add a time delay before performing the first sample after the LazWell loading. It allows the stabilization of the corona discharge and the carrier gas flow. The recommended delay is 10 seconds. G) Gas Temp : Carrier gas temperature status. The heating cartridge temperature is set to 50 °C as default. When this temperature is reach and maintains within 1 °C the indicator is Green. The temperature indicator turns red when the temperature is outside the tolerance set at 1 °C. H) Gas Flow : Carrier gas flow status. I) LazWell : Serial number plate list. The highlighted serial number is the one that is currently analyzed. Plates order into the loader should be the same as defined in the LazSoft. J) Laser Pattern : same description as in Manual Execution v4.2.
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LDTD – model S-960
The submit laser pattern should have already been edited and saved in LazSoft the batch could not be run. K) Laser power (%) vs. Time (s) panel : This graph represents ramp/plateau laser power according to time for the experiment in progress. The yellow cursor on the graph moves according to the progress of the experiment. L) Visual indicators • Laser in function : This indicator becomes red when the laser is in function. • Power : Laser power follow-up in percentage.
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LDTD – model S-960
4
Operating conditions
Introduction This section contains operating conditions to adequately operate the LDTD source. These conditions are described in two sections one for the LDTD and one for the mass spectrometer inlet parameters. As the thermal desorption process, the ionization and the ion transfers into the mass spectrometer are compound dependant, the describe setup may vary. However, Phytronix Technologies recommends using these parameters as general operating conditions.
LDTD parameters Carrier gas flow The carrier gas plays two major roles: 1) It allows the transfer of the desorbed neutral species from the well to the corona discharge region through the transfer tube. 2) It thermalyzes the thermal desorption process by lowering the internal energy of the desorbed species by inelastic collisions. Its optimal value is within 2 and 3 L/min. Setting the carrier gas within these values provides the best signal-to-noise ratio combine to a low signal variability. Lowering or increasing the flow will decrease the signal and/or increase the variability. For highly reactive compound, like explosives, the carrier gas flow may be increase. Laser pattern The effect of the laser pattern vary from compound to compound (compound dependent). As a thumb rule, the laser power in % value will give you less or more energy transfer into the sample. The laser power slope may be modify to optimize the compound desorption. A smooth laser power ramp (increasing the power over 2 to 4 seconds) will damp the matrix effect, allows time for the thermal transfer to the analyte and lowers the matrix non-volatile compounds to decompose. Therefore, it increases the analyte signal-to-noise ratio. The first step in the laser pattern optimization is to determine the thermal desorption behavior of the compound (compound dissolve in neat solvent). The user may use the following laser patterns (Figure 28) for it (low, medium or high heat). The goal here is to evaluate how much energy your compound needs to desorbs. Once the temperature behavior have been determine the user may
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LDTD – model S-960
increase or lower the ramping slope to adequately desorbed the compound from the matrix (here use a real sample solution at a concentration around 100 ng/mL). The reproducibility should also be evaluated during this laser pattern optimization process. Here, the user will play with the laser to obtain the best signal to noise ratio (S/N) combine to a raw signal variation less than 15 % (or less than 10 % with the internal standard correction). Keep in mind that the higher signal will not necessarily gives the best signal reproducibility.
A
B
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LDTD – model S-960
C
Figure 28 : Laser pattern examples. A) low heat, B) medium heat and C) high heat.
Mass Spectrometer parameters The mass spectrometer parameters, optimized with the ESI source, for a specific compound, might mainly be keeping when operating with the LDTD source. The declustering potential and the curtain gas must however be adjust to obtain the best signal-to-noise ratio when the LDTD source is used. The others parameters might also be optimized to increase the overall performance of your analysis.
Declustering potential The declustering potential (DP) is an important inlet parameter to be optimized when the LDTD ion source is used. As no mobile phase is introduced into the corona discharge region, the cluster formation is drastically reduced using the LDTD source. As a result, the DP must be optimized with the LDTD source. Using the DP obtained from ESI effusion optimization will affect the ions transfer into the mass spectrometer when the LDTD source is used. It is recommended to optimize the DP with a real sample at an analyte concentration around 100 ng/mL. The user creates a MRM table with several lines but with the same Q1-Q3 transition keeping all the settings the same except the DP value. The acquire file will then contain several signal being different only from the DP value. Therefore, in 1 LDTD analysis, the DP will be optimized.
Curtain gas The curtain gas (CUR) should be set to its minimal value when the LDTD source is used as compared to an ESI source. This setting will increase the signal and a minimal value will be sufficient to prevent dust material to block the mass spectrometer inlet hole.
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LDTD – model S-960
Source temperature The LDTD ion source electronics simulate a source temperature (TEM) of 22 °C. Therefore, the source temperature should be set to 22 °C for the mass spectrometer being ready to operate.
Ion source gas The ion source gas 1 and 2 (GS1, GS2) should both be set to 0 in normal operating condition. To purge the ion source housing could be performed using higher ion source gas values if needed.
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LDTD – model S-960
5
Consumable and Replaceable Parts
Introduction This section contains part numbers for consumable and replaceable parts for the LDTD system. For the service or the maintenance, order only parts listed or their equivalent. To order consumable and replaceable part, contact Phytronix Technologies.
Accessories and Services LazWell………………………………………………………..……… Gas flow calibration kit……….…………………………………….... Clomifen Standard 100ug/ml……………………………….….……... Applicator (swabs) Transfert Tube……………………………….…...
LazWell96 100100 100142 97000017
LDTD source box Screw Kit…………………………………………………………..…. Fuse Kit……………………………………………………………..… Transfer tube Kit Thermo……..…………………………………..….. Transfer tube O-ring…………...………………………………….….. LDTD-APCI needle…..……………………………………….……....
100143 100109 100117 92100002 100128
EC box Screw Kit………………………………………….………………..… 100143 Fuse Kit…………………………………………………………….… 100109
Cables EC box to laser head cable…………………………………………..... EC box to source DB25 cable……………………………………..….. EC box to station COM cable……………………………………..….. EC box to MS (Start) cable………………………………………..….. Power cable Americas……………………………………………..….. Power cable United Kingdom……………………………………..….. Power cable Europe……………………………………………….…..
100030 100039 100032 100031 72080017 72080018 72080019
Manuals LDTD, Model S-960, Operating Manual…………..……………...…. 100101 41
LDTD – model S-960
6
Maintenance
Introduction This section describes routine LDTD maintenance that must be performed. The performance of the LDTD depends on the maintenance on your system. It is your responsibility to maintain your system properly by performing the maintenance procedure on a regular basis. The maintenance frequency depends on the type and amount of sample introduced into the instrument.
General caution Removing the LDTD to the mass spectrometer will shot down the laser beam operation. This security should not be override by anyone. It is important to understand and follow the procedure, including the disconnection of the EC box to laser head cable.
Gas flow verification Procedure • • • • •
Remove the LDTD attached to the mass spectrometer as described in the topics Removing the LDTD from the mass spectrometer on page 14. Place the LDTD on a flat surface and secure it to make sure the source cannot lie down on the laser assembly. Adjust the gas flow to 2.0 L/min and monitor the flow with a certified flowmeter. The flow should be within more or less 0.5 L/min. Reinstall the LDTD on the mass spectrometer as described in the topics Installing the LDTD from the mass spectrometer on page 13.
Laser irradiation positioning Introduction The following procedure is used to verify the positioning of the laser irradiation on the backside of the LazWell.
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LDTD – model S-960
Caution The procedure includes the laser operation. To prevent the user to be exposed to any laser irradiation, the LDTD should be installed on the mass spectrometer. It is forbidden to remove the source from the mass spectrometer for the laser irradiation positioning. Procedure • • • •
• • • • •
Load an empty LazWell into the LDTD. In the Manual Execution window of the LazWell go to the well A1. Adjust the gas flow to 0 L/min. Open the laser pattern name “footprint” : o 1 sec at 0 % o 1 sec to 60 % o Hold at 60 % for 3 sec. o 0 sec to 0 % Start an analysis in the empty A1 well. Repeat this procedure for the well A12, H1 and H12 Eject the LazWell. The laser irradiation impregnation inside the wells should be as shown in Figure 29. If the laser irradiation positioning is incorrect call service. Laser impregnation
0.5 mm
Figure 29 Adequate laser irradiation impregnation view from the inside of a well.
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LDTD – model S-960
X-Y stage positioning Caution Removing the LDTD to the mass spectrometer will shot down the laser beam operation. This security should not in any case be override by anyone. It is important to understand and follow the procedure, including the disconnection of the EC box to laser head cable. Moreover, the user will be asked to look through the transfer tube. This step SHOULD NOT be performed if the source is connected to the EC box. A LazWell should be present at all time when performing this maintenance procedure. Procedure • • • • • • • • •
Load an empty LazWell into the LDTD. In the Manual Execution window of the LazSoft go to the well A1. Close the LazSoft. Turn OFF the EC box. Remove the LDTD attached to the mass spectrometer as described in the topics Removing the LDTD from the mass spectrometer on page 14. Place the LDTD on a flat surface and secure it to make sure the source cannot lie down on the laser assembly. Look through the transfer tube. The inside diameter of the transfer tube is supposed to be centered in the well. Reinstall the LDTD on the mass spectrometer as described in the topics Installing the LDTD from the mass spectrometer on page 13. If the X-Y stage positioning is not as it should be call service.
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LDTD – model S-960
Transfer tube cleaning Introduction The glass transfer tube should be exempt of solid particles (dust). Dust may affect the sample transfer and even block the MS entrance. A periodic cleaning of the transfer tube is recommended. Procedure The cleaning procedure should always be performing with an empty LazWell loaded into the LDTD. The transfer tube alignment should not be modified during the cleaning procedure. • • • • • • • •
Load an empty LazWell into the LDTD. In the Manual Execution window of the LazSoft go to the well A1. Close the LazSoft. Turn OFF the EC box. Remove the LDTD attached to the mass spectrometer as described in the topics Removing the LDTD from the mass spectrometer on page 14. Place the LDTD on a flat surface and secure it to make sure the source cannot lie down on the laser assembly. Clean the transfer tube by wiping the inside with an applicator impregnated with dichloromethane followed by methanol. Reinstall the LDTD on the mass spectrometer as describe in the topics Installing the LDTD from the mass spectrometer on page 13.
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LDTD – model S-960
7
Troubleshooting
Introduction Information about error messages and how to troubleshoot the LDTD is listed in this section. The information found in this section is not exhaustive, if you have any doubt about the procedure listed in this section or facing unlisted problem contact the Phytronix Technologies service team at the following coordinates : Phytronix Technologies 337 Saint-Joseph Est Québec (Québec) G1K 3B3
[email protected] Phone : (418) 692-1414 Fax : (418) 692-4940
Fault messages Fault message appears in a window as part of the LazSoft. Pushing the OK button can close fault message window. However, if a fault is still present and/or have not been fixed, the fault message will generally come back. Information about fault solving is listed below (fault messages list). If the information provided in the list is not sufficient to solve the problem or if the problem you are encountering with the LDTD is not listed, contact the Phytronix Technologies service team.
Fault message list 9000 :
Command unknown The command sent to the EC box is unknown. The LazSoft version may not be compatible with the LDTD following software upgrade. Call service.
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LDTD – model S-960
9001 :
Bad command checksum Communication failure with the EC box. The RS-232 cable may be disconnected or damaged. If the RS-232 is correctly connected and not damaged and the problem is still present call service
9005 :
Door (or box) error The source box or the source door is blocked. Check if the source box is open. All eight (8) screws should be fully screwed. Check if any object does not obstruct the source box door. Check if the source box loader panel is opened. If the problem persists, call service
9006 :
Bar code unreadable or missing The bar code reader is unable to read the LazWell bar code. Check if the LazWell’s bar code is present. Check the bar code on the LazWell and make sure it is in the right position and fully stuck on the plate side. If the problem persists, call service
9008 :
System locked, laser aborted The source box or the source door was opened while the laser was in function. The laser stopped and the sequence aborted. Close the source box or the source door and restart the sequence.
9009 :
No LazWell present Check if the LazWell is blocked in the loader.
9010 :
Plunger down error The plunger is enabled to move into the selected well or there is no LazWell loaded. Load a LazWell into the LDTD. Check if the gas pressure upstream the EC box is sufficient (the pressure must be between 60 and 80 psi). Check for possible gas leaks (follow the procedure described in the section troubleshooting procedure). Check the LazWell position into the stage (follow the procedure described in the section troubleshooting procedure). If the gas pressure is correct and the LazWell is in the right position into the stage, the X-Y stage may be unaligned, call service.
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LDTD – model S-960
9011 :
Plunger up error The plunger is enabled to move in and out the well. Check if the gas pressure upstream the control box is sufficient (the pressure must be between 60 and 80 psi). Check for possible gas leaks (follow the procedure describe in the section troubleshooting procedure). Check the LazWell position into the stage (follow the procedure describes in the section troubleshooting procedure). If the gas pressure is correct and the LazWell in the right position into the stage the X-Y stage may be unaligned, call service.
9012 :
Gas pressure too low Check if the gas pressure upstream the EC box is sufficient (the pressure must be between 60 and 80 psi). Check for possible gas leaks (follow the procedure described in the section Troubleshooting procedure).
9015 : 9016 :
Stall motor X (position) Stall motor Y (position) The X or Y displacement motor has stalled at the position mentioned. A LazWell may be stuck in the X-Y stage. Follow the Procedure for stall X-Y stage (below) to fix the problem. If the stage still stall call service.
9017 : 9018 :
Motor X moving timeout (30 sec) Motor Y moving timeout (30 sec) Motor configuration erroneous or hardware failure. Contact Service.
9019 : 9020 :
Motor X read parameter timeout (5 sec) Motor Y read parameter timeout (5 sec) The communication to motor failed. Restart the LDTD (close LazSoft and turn the power OFF of the EC box). If the problem persists, call service
9021 :
Laser data not valid (LASER T P command) Software error. Call service.
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LDTD – model S-960
9022 :
Laser data insufficient (only 1 point received) The laser pattern is invalid as it contains only 1 point (time and power). Change the laser pattern.
9023 :
Well # invalid (MOVEW) Well number requested invalid. Check if the well number in the sequence is properly written (6 digits).
9024 :
Laser head cable defective The EC box to laser head cable is unplugged or defective. Plug the cable (both ends are identical). Check the cable connections. Check if the cable is not damaged. If the problem persists, call service.
9100 :
Error (second attempt will be made) Motor error. Call service.
9200 :
Serial Read Timeout LazSoft is unable to communicate with the EC box. Check if the EC box is turned on. Check the connection of the EC box to station COM cable. If the problem persists, call service.
9505
Unable to set gas flow to desired value (Batch) The gas flow is not reached to the target value. Check the gas line connections. Check for possible gas leaks (follow the procedure described in the section Troubleshooting procedure). If the problem persists, call service.
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LDTD – model S-960
8
Troubleshooting procedure
Introduction Information needed for LDTD troubleshooting can be found in this section. The work can be done safely and accurately by a person with no experience in instrumental service, but only if all warnings are read and understood and all procedures are carefully followed. To avoid unnecessary and costly repairs, read and understand all of the appropriate information in this section before attempting any troubleshooting. Be sure you THROUGHLY understand all the information before proceeding. The information found in this section is not exhaustive, if you have any doubt about the procedure listed in this section or facing unlisted problem with the LDTD contact the Phytronix Technologies service team at the following coordinates : Phytronix Technologies 337 Saint-Joseph Est Québec (Québec) G1K 3B3
[email protected] Phone : (418) 692-1414 Fax : (418) 692-4940
General caution and warning CAUTION WARNING LASER PRESENT
To avoid damage to the instrument, turn power OFF before opening the source box or the EC box Removing the LDTD from the mass spectrometer will shut down the laser beam operation. This security should not in any case be override by anyone. It is important to understand and follow the troubleshooting procedure, including the disconnection of the EC box to laser head cable.
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LDTD – model S-960
Procedure for gas leak detection Introduction Gas is used in the LDTD : 1) for the pneumatics which control the LazWell ejection door, the transfer tube displacement into or out the LazWell’s wells and in the LazWell loading procedure, 2) as carrier gas transporting the desorbed gazeous species from the sample through the transfer tube into the APCI region. Gas leak may affect the system in different ways depending on its location. Caution Cases (EC box and LDTD) opening may expose the user to laser radiations and to electric devices. The power should be turned OFF before opening cases. Procedure • • •
Load an empty LazWell into the LDTD. In the Manual Execution window go to the well A1 and set the gas flow to 2 L/min. Disconnect the carrier gas line on the side of the LDTD source box (Swagelok 1/8 inch female connector, Figure 6). o The gas flow on the carrier gas flow should be 2 L/min ± 0.5 L/min (or the on selected in the LazSoft Manual Execution window). o If the gas flow is not within ± 0.5 L/min, the leak is located in the EC box ; o If the gas flow is within ± 0.5 L/min, the leak is located in the LDTD source box.
•
The leak is located in the EC box : o Turn OFF the EC box power. o Open the EC box (6 screws). o Verify all the tubing connections. Tubing should be fully inserted into connections and nuts should be tightened. o Close the EC box (do not forget to screw all 6 screws).
•
The leak is located in the LDTD source box : o Remove the LDTD attached to the mass spectrometer as described in the topics Removing the LDTD from the mass spectrometer on page 14. Place the LDTD on a flat surface and secure it to make sure the source cannot lie down on the laser assembly. o Unscrew the 8 Hex screws on the back panel of the LDTD. o Open the LDTD back panel.
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LDTD – model S-960
Cables and mechanical parts are connected to the back panel and should not be disconnected. Special care should be taken to prevent to damage them. o Secure the back panel in a way where cables and mechanical parts could not be damaged. o Verify all the tubing connections. Tubing should be fully inserted into connections and nuts should be tightened. o Close the LDTD back panel (do not forget to screw all 8 Hex screws). o Reinstall the LDTD on the mass spectrometer as describe in the topics Installing the LDTD from the mass spectrometer on page 13. If the leak is still present contact the service team of Phytronix Technologies
Procedures for LazWell stuck in X-Y stage Introduction Improper LazWell loading may stop the X-Y stage from function. In such case the loader or the X-Y stage may be unaligned. In both cases, removing the stuck LazWell and loading a new LazWell is necessary to point out the origin of the problem. Caution LDTD opening may expose the user to laser radiations and to electrical devices. The power should be turn OFF before opening cases.
Procedure •
• •
Remove the LDTD attached to the mass spectrometer as describe in the topics Removing the LDTD from the mass spectrometer on page 14. Place the LDTD on a flat surface and secure it to make sure the source cannot lie down on the laser assembly. Unscrew the 8 Hex screws on the back panel of the LDTD. Open the LDTD back panel. Cables and mechanical parts are connected to the back panel and should not be disconnected. Special care should be taken to prevent to damage them.
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LDTD – model S-960
• • • • • • •
Remove the LazWell. Close the LDTD back panel (do not forget to screw all 8 screws). Install the LDTD on the mass spectrometer as describe in the topics Installing the LDTD from the mass spectrometer on page 13. Turn the power ON on the EC box. Load an empty LazWell into the LDTD. In the Manual Execution window of the LazWell go to the well A1. The LazWell should be loaded properly. If the X-Y stage is still stalled contact the service team of Phytronix Technologies.
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LDTD – model S-960
9
Index
A Analyst window, 31
B Bar code, 23, 25, 28, 47 Batch traceability, 34
C Cable connections, 15 Carrier gas, 14, 51 Carrier gas flow, 37 Cleaning, 45 , 15 Computer, 17 Condition of operation, 12 Consumable parts, 41 Corona discharge, 17 Curtain gas, 39
G Gas connection, 14 Gas flow, 28, 31, 35 Gas flow calibration, 41 Gas flow verification, 42 Gas leak, 51 Gas pressure, 15, 48 Gas temperature, 28, 35 Getting started, 13
H Hardware, 18 Home, 27
I Import batch from LazSoft, 33 Indexation, 24 ion source gas, 40 Ionization, 17
D Declustering potential, 39 Door, 47 Dust, 45
E EC box back panel, 15 Error, 46 Export, 32
F Fault message, 46 Figures List, 3
L Laser centering, 42 Laser diode protection, 14 Laser impregnation, 43 Laser indicator, 8 Laser pattern, 28, 35, 37 Laser radiations, 7, 51, 52 LazSoft, 17, 26 LazSoft batch v4.1, 33 LazSoft manual execution v.4.2, 27 LazWell, 25 LazWell description, 23 LDTD, 53 LDTD installation, 13 LDTD removing, 14 54
LDTD – model S-960
LDTD safety information, 8 Limited, 5 Loading problem, 52 Loading the LazWell, 25
M Maintenance, 42 Motor, 48 MS entrance, 45
O Operating conditions, 37 Oxygen, 15
P Packing list, 12 Plunger, 47, 48 Pneumatics, 14
R Regulatory compliance, 6 Relative humidity, 12 Replaceable parts, 41
S Security, 6 Setup, 10 Software, 26 Source temperature, 40 Stage error, 52 Stage positioning, 44
T Table of contents, 1 Temperature, 12 Template, 31 Traceability, 34 Transfer tube, 41, 45 Troubleshooting, 46 Troubleshooting procedures, 50
W Waste, 9 Water, 15 WEEE, 9 Well loading, 24
X X-Y displacement, 44
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