Agilent Technologies 5975 MSD Bedienungsanleitung

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Scientific Instruments Manufacturer GmbH

D-46149 Oberhausen • +49-208-94 10 78-0 • www.sim-gmbh.de

SERVICE MANUAL

SIM Direct Inlet Probe

for

Agilent 5975 MSD

and

Agilent 7000 Triple Quadrupole

(Firmware V.1.10)

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Scientific Instruments Manufacturer GmbH

D-46149 Oberhausen • +49-208-94 10 78-0 • www.sim-gmbh.de

Document History

Edition 7075e 10/2010, from Firmware / Software Version V1.10 and dip.v.1.2.

The information contained in this document is subject to change without notice.

SIM GmbH makes no warranty of any kind with regard to this material, including, but not limited to, the

implied warranties of merchantability and fitness for a particular purpose.

SIM GmbH shall not be liable for errors contained herein or for incidental or consequential damages in

connection with the furnishing, performance or use of this material.

Reproduction, adaptation, or translation without prior written permission is prohibited, except as

allowed under the copyright laws.

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Scientific Instruments Manufacturer GmbH

D-46149 Oberhausen • +49-208-94 10 78-0 • www.sim-gmbh.de

CONTENT

1 PARAMETER MENU OF THE CONTROLLER (FIRMWARE V1.10) .......................... 4

2 DIP INSTALLATION PROCEDURE............................................................................ 5

2.1 Replacing the ion source ........................................................................................... 5

2.2 Installing the DIP on the Agilent 5975 MSD ............................................................... 5

2.3 Installing the DIP on the Agilent 7000 Triple Q........................................................... 7

2.4 Connecting the DIP and the GC................................................................................. 8

2.5 Configuration of the DIP-Controller ............................................................................ 9

2.6 Installing the DIP Software......................................................................................... 9

2.7 Insert the ChemStation/MassHunter methods for the DIP.........................................10

2.7.1 5975 MSD: ChemStation methods .........................................................................10

2.7.2 7000 Triple Q MS/MS: MassHunter methods .........................................................10

2.8 Adjustment of the CombiPAL to the MS-DIP System (optional) ................................10

2.9 Push rod performance test........................................................................................10

2.10 Tuning of the DIP-MS System...................................................................................10

2.10.1 Autotune 5975 MSD with DIP.................................................................................10

2.10.2 Autotune 7000 TripleQ MS/MS with DIP.................................................................11

2.11 Controller: Update of the firmware ............................................................................11

3 EXACT POSITIONING OF THE PUSH ROD IN THE ION SOURCE .........................12

4 TEMPERATURE CALIBRATION OF THE CONTROLLER ........................................14

4.1 Menu: General Configuration ....................................................................................14

4.2 Temperature Calibration ...........................................................................................14

5 DIP TEST PROCEDURES ........................................................................................16

5.1 DIP Temperature accuracy test ................................................................................16

5.2 Leak test...................................................................................................................17

5.3 Coupling test: CombiPAL with MSD-DIP and GC (optional, for DIP - 45°type with

5975 MSD) ...........................................................................................................................18

5.4 DIP (EI) Performance test.........................................................................................19

5.5 DIP (PCI) Performance test for DIP/5975 MSD Systems ..........................................22

APPENDIX ...........................................................................................................................24

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Scientific Instruments Manufacturer GmbH

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1 Parameter Menu of the Controller (Firmware V1.10)

Parameter

Assignment min value max value default

0 1000 (Password) 10 0x7fff 1000

1 Temp. adjustment (0.1°C) -200 200 -23

2 LCD contrast 0 50 20

3 push rod position outside (min pos) -400 -100 -136

4 push rod position ion source (max pos)

300 550 467

5 cooling position 100 500 300

6 max temperature 350 500 400

7 xp*0.1 10 1000 150

8 tn*0.1 1 100 40

9 inj-position -400 -100 -135

10 ion source position 300 500 444

11 temp correction (*0.001) -200 200 -115

12 damp down heating oscillations td*0.1 0 30 10

13 O-ring change position -400 0 -115

Option bits: 1=useExStart, 2=ready

position inside the DIP, 4=90°position,

8=continuous operation, 16=smoothing

of temperature, 32=early start,

64= CO

cooling

-0x8000 0x7fff 23

15 push rod horizontal position -0x8000 0x7fff 75

16 light barrier change position - - 160

17 tilt angle adjustment - - 12

18 dwell time (in valve after opening to the

ion source; 1min =100, default = 6 s) 0 -001

19 position of light barrier for tube test

(-97 = activated, -1 = deactivated) -97

Additional remarks to parameter 14:

You can combine the items by adding the numbers, e. g. “23” (1+2+4+16) for DIP without autosampler or

“31” (1+2+4+8+16) for DIP with autosampler, “95” ((1+2+4+8+16+64) for DIP with autosampler and CO

cooling

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Scientific Instruments Manufacturer GmbH

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This menu is reserved to qualified service engineers only and needs a password.

Select the parameter menu of the controller in the following way:

1. Press <Enter> and keep it pressed

while pressing <arrow up><arrow down><arrow up><arrow down>

then let off the <Enter> key so that the diagnostic menu appears

press <arrow right> and <Enter> so that the cursor in the parameter menu appears:

the first two numbers represent the parameter number, the selected number is taken

with <Enter>

then the belonging value (to this parameter) will be shown and can be changed

2. Select parameter “00” and enter the password “1000”

3. Change the values of the designated parameter.

2 DIP Installation Procedure

2.1 Replacing the ion source

Please follow the instructions given in the corresponding Agilent Manual to replace the

existing ion source with the provided modified ion source (EI or CI).

2.2 Installing the DIP on the Agilent 5975 MSD

Before installing the DIP System to the Agilent 5975 MSD you have to uninstall the MSD

front panel:

1. After you have

disconnected the required

cables, remove the MSD

front panel carefully.

Please follow the

instructions given in the

5975 MSD manual.

2. Demount the two boards for

the MSD display (see

marking on the left) and put

the MSD front panel aside

and

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Scientific Instruments Manufacturer GmbH

D-46149 Oberhausen • +49-208-94 10 78-0 • www.sim-gmbh.de

3. Remove the DIP front panel

of the DIP System following

the instructions given in the

DIP manual (chapter 7.2).

4. Take the DIP front panel

and mount the display

boards of the MSD onto the

preset positions (see left).

5. Before mounting the DIP

system, remove the glass

plate in front of the MSD ion

source compartment.

6. To mount the DIP system in

front of the MSD, first

deinstall the valve unit by

loosing the two screws (see

marked circles on the left).

Now the adapter plate is

separated and the four

screws are well accessible

for the next step.

7. Take the adapter plate and

mount it in front of the ion

source compartment using

the four screws (see

marked circles on the left,

the screws behind the

motors are not visible on

this photo).

8. Then retighten the valve

unit of the DIP system on

the adapter plate with the

two screws according to the

photo of step no. 6.

9. Replace the original knurled

knob of the MSD valve with

the provided knob for the

DIP System (see marked

rectangle in the photo left).

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Scientific Instruments Manufacturer GmbH

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10. Mount the push rod cover by reversing the instructions in chapter 7.2 of the DIP

manual. Make sure that all cables are correctly connected.

2.3 Installing the DIP on the Agilent 7000 Triple Q

Before installing the DIP System to the Agilent 7000 Triple Q MS/MS you have to uninstall

the MSD front panel. After you have disconnected the required cables, remove the MS front

panel carefully (please follow the instructions given in the Agilent manual.)

1. Demount the two boards of the MS/MS front panel and then put this two-part front

panel aside.

2. Remove the front panel of the DIP System following the instructions given in the DIP

manual (chapter 7.2).

3. Mount the two boards

onto the preset positions

of the DIP front panel

(see marking on the

right photo)

4. Before mounting the DIP

system, remove the

glass plate in front of the

MS/MS ion source

compartment.

5. To mount the DIP system in

front of the MS/MS, first

deinstall the valve unit by

loosing the two screws (see

marked circles on the left).

Now the adapter plate is

separated and the four

screws are well accessible

for the next step.

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Scientific Instruments Manufacturer GmbH

D-46149 Oberhausen • +49-208-94 10 78-0 • www.sim-gmbh.de

6. Take the adapter plate and

mount it in front of the ion

source compartment using

the four screws (see

marked circles on the left,

the two screws behind the

motors are not visible on

this photo).

7. Then retighten the valve

unit of the DIP system on

the adapter plate with the

two screws according to

the photo of step no. 5.

8. Replace the original

knurled knob of the MSD

valve with the provided

knob for the DIP System

(see marked rectangle in the

photo left).

9. Mount the push rod cover by reversing the instructions in chapter 7.2 of the DIP

manual. Make sure that all cables are correctly connected.

2.4 Connecting the DIP and the GC

Please follow the instructions of the Agilent Manual but pay attention to the difference in

installing the DIP controller as you can see in the figures below:

DIP controller rear panel view:

Power cord receptacle

Cooling outOn/Off

Cooling in

RS 232 Cable

LAN Cable

System CableAPG for Start-Remote-Cable

(without autosampler)

for Remotemanager

(with autosampler)

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Scientific Instruments Manufacturer GmbH

D-46149 Oberhausen • +49-208-94 10 78-0 • www.sim-gmbh.de

connecting diagram GC-MS-DIP Controller

GC MSD

DIP

Controller

Diode Cable

B 0613 59 73

Remotemanager

RM 0002 68 90

Start-Remote-Cable

B 0301 40 02

2.5 Configuration of the DIP-Controller

The IP adress is assigned in the menu “Network configuration “ of the DIP controller (see

MSD DIP Manual, 5.5 Network configuration):

1. Turn on the DIP controller.

2. Select the menu “Network configuration” and scroll with the “arrow up” and “arrow

down” key in the parameters.

3. Set the parameter “DHCP Mode” to “Fixed IP”.

4. Select the parameter “IP adress” with the “Enter” key and change the numbers with

the arrow keys.

5. Skip back to the basic display by pressing the “arrow right” key two times.

Or the IP-adress is assigned automatically if the modus “DHCP” is selected (see MSD DIP

Manual, 5.5):

1. Turn on the DIP controller.

2. Select the menu “Network configuration” and scroll with the “arrow up” and “arrow

down” key in the parameters.

3. Set the parameter “DHCP Mode” to “DHCP” (see).

4. Skip back to the basic display by pressing the “arrow right” key two times.

2.6 Installing the DIP Software

Note: You can find all files with software and default methods on the disc enclosed.

1. Copy the files “DIP.exe, dip.enu, dip.deu” into the new folder “DIP”.

2. Copy the default methods in the folder “DIP\Methods”

3. Open the “DIP”-Software.

4. Click on “File” and open the menu “Config.”.

5. Select the DIP controller with a click on the IP adress.

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Scientific Instruments Manufacturer GmbH

D-46149 Oberhausen • +49-208-94 10 78-0 • www.sim-gmbh.de

2.7 Insert the ChemStation/MassHunter methods for the DIP

Note: You can find all the folders with the default methods on the disc enclosed.

2.7.1 5975 MSD: ChemStation methods

1. Copy the folders “DIP_EI_Q1” and “DIP_CI_Q1” into the methods section of the MSD

ChemStation under “Programme\MSDChem\1\Methods”.

2. optional (with autosampler):

Copy the folders “Injection_GC” and “Injection_DIP” into the methods section of the

MSD ChemStation.

2.7.2 7000 Triple Q MS/MS: MassHunter methods

1. Copy the folders “DIP_EI_Scan.M” (and possibly “DIP_CI_Scan.M”) into the methods

section of the MassHunter software under “MassHunter\GCMS\1\Methods”.

2. optional (with autosampler):

Copy the macros (cycles) “DIP-Liquid-Inj.cyx” and “DIP-Solid-Inj.cyx” into the PAL

section under “MassHunter\GCMS\1\PALDATA”.

2.8 Adjustment of the CombiPAL to the MS-DIP System (optional)

1. Define two new DIP positions for a precise co-operation of PAL and DIP (see DIP-

PAL Manual 6.4.3).

2. Create a macro and a new method in the Cycle Composer Software of the

autosampler (see DIP Manual 6.4.4 and 6.4.5) or copy the files of the folder “Cycle

Composer” into

”C:\Programs\PAL\Cycle Composer\Combi PAL”.

2.9 Push rod performance test

1. Select the method “drive.dip” in the DIP-Software and click“OK”.

2. Check the correct insertion of the push rod into the MSD ion source and the

operational sequence backwards in real and even at the status display of the

software.

3. Select the method “heat.dip” in the DIP-Software and click “OK”. The push rod is

inserted into the ion source and heated up to 400 °C. This temperature is maintained

for 1 minute.

4. Check the correct temperature run via the status display.

2.10 Tuning of the DIP-MS System

2.10.1 Autotune 5975 MSD with DIP

1. Verify that the system has been pumping down for at least 2-4 hours and that the DIP

controller is turned on. The DIP push rod status is “Ready”.

2. In the “Instrument Control view”, select “Perform MS Autotune” from the instrument

menu.

The software will perform an autotune and print out the report.

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