Agilent G1978B Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide Agilent Technologies
Notices © Agilent Technologies, Inc. 2008 Warranty No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws. The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions.
In This Guide This guide explains how to install, maintain and troubleshoot your nanoelectospray ion source. 1 Installation This chapter tells you how to install the multimode ion source. 2 Verification This chapter tells you how to install the multimode ion source. 3 Methods This chapter describes basic operation and maintenance for the multimode ion source.
Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide
Content 1 Installation 7 Installation 8 Step 1. Prepare to install 8 Step 2.
Contents 6 Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide
Agilent G1978B Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide 1 Installation Installation 8 Step 1. Prepare to install 8 Step 2. Install the HV control PCA and cables 9 Changing Sources 13 To remove the multimode source 13 To convert from multimode to ESI, APCI or APPI 14 To convert from ESI, APCI or APPI to the multimode source 15 This chapter contains instructions to install the multimode source on a 6100 Series Single Quad LC/MS system, and also to remove and replace the source.
1 Installation Installation Installation This section explains how to install the G1978B multimode source on a 6100 Series Single Quad LC/MS instrument. The G1978A multimode source is not supported on these instruments. The 6100 Series Single Quad LC/MS with multimode source is supported on ChemStation B.03.01 or higher, or the ChemStation B.01.03 with a patch. Step 1. Prepare to install The Multimode Enablement Kit, G1978-60451, is shipped with the multimode source.
Installation Step 2. Install the HV control PCA and cables 1 • Valve BD-APCI supply, p/nG1960-60802 • Valve BD-APCI Needle Interlock, p/n G1960-60856 Figure 2 From left to right: G1946-80058, G1960-60802 and G1960-60856 Step 2. Install the HV control PCA and cables 1 Turn off the system power and remove the system power cord. Keep the power cord intact if the vacuum control switch box is used. The switch box is intended to keep the vacuum on while a CE works on the electronics.
1 Installation Step 2. Install the HV control PCA and cables Figure 4 Connecting the valve PCA to the multimode HV power supply. 6 Install the APCI HV power supply. The APCI HV power supply is located at the end of the AUX Module. 7 Connect ribbon cable between valve PCA and Vcap/Vchamber power supply. Figure 5 Connecting the valve PCA to the Vcap/Vchamber power supply. 8 Connect the Vcap and Vchamber cables to the Vcap/Vchamber power supply.
Installation Step 2. Install the HV control PCA and cables Figure 6 1 Connecting the Vcap and Vchamber cables to the power supply. 9 Connect the long ribbon cable, p/n G1960-60802, from the APCI HV power supply to the valve PCA. Figure 7 Connecting the APCI HV power supply to the valve PCA. 10 Insert one end of the APCI Needle Interlock cable, G1960-60856, through the slot at the front of the system and then plug it to the APCI HV connector.
1 Installation Step 2. Install the HV control PCA and cables Figure 9 Connecting the HV PCA to the chassis. 12 Close the AUX Module cover and reconnect all cables. 13 Install the multimode source to the system and connect all connectors. Figure 10 Installing the multimode source (left) and connecting all connectors. 14 Put back the side, top, front and CDS cover. 15 Plug the system power cord back on and turn the front switch on. The pump down process will start. 16 Start the ChemStation program.
Installation Changing Sources 1 Changing Sources To remove the multimode source Do the following steps to remove the multimode source. 1 Set the source temperatures for vaporizer heater and drying gas heater to minimum values to cool the source. Use the Tune > Instrument > Edit Spray Chamber menu item to display the Edit Spray Chamber dialog box. Set the drying gas flow, nebulizer gas flow, drying gas temperature and the vaporizer temperature to minimum values.
1 Installation To convert from multimode to ESI, APCI or APPI 10 Place the source shipping cover on the source. To convert from multimode to ESI, APCI or APPI WA R N I N G Never touch the source surfaces, especially when you analyze toxic substances or when you use toxic solvents. The source has several sharp pieces which can pierce your skin including the APCI corona needle, vaporizer sensor and counter current electrode.
Installation To convert from ESI, APCI or APPI to the multimode source 1 To convert from ESI, APCI or APPI to the multimode source CAUTION If you are installing this source on this instrument for the first time, follow the steps in “Installation” on page 7. 1 Switch to the MSD Tune view. 2 Select Instrument/Set Spray Chamber and set all gas flows and temperatures to 0.
1 Installation To convert from ESI, APCI or APPI to the multimode source Standard spray shield Capillary cap Figure 11 Standard spray shield and capillary cap for ESI or APCI 10 Remove the capillary cap. If needed, moisten a clean cloth with isopropyl alcohol and wipe the capillary cap. See Figure 12. Capillary cap Figure 12 Spray shield removed. 11 Place the capillary cap back on the capillary. 12 Install the new spray shield with field shaping electrodes. See Figure 13.
Installation To convert from ESI, APCI or APPI to the multimode source Figure 13 1 Multimode spray shield 13 Screw the multimode spray shield into the holder for the spray shield. See Figure 14. Field shaping electrode 9 o'clock position Field shaping electrode 6 o'clock position Figure 14 NOTE Multimode spray shield installed The field shaping electrodes should be in the nine o’clock and the six o’clock position.
1 Installation To convert from ESI, APCI or APPI to the multimode source Figure 15 Multimode Spray Chamber 15 Install the spray chamber on the spray chamber mount. I-Button Figure 16 Multimode source with I-Button 16 Install the nebulizer on the multimode source spray chamber.
Installation To convert from ESI, APCI or APPI to the multimode source Figure 17 1 No nebulizer on top of the multimode source 17 Connect the 1/8-inch nebulizer gas tubing from the LC/MS mainframe to the nebulizer gas fitting. See Figure 18.
1 Installation To convert from ESI, APCI or APPI to the multimode source 18 Connect the LC/MS sample tubing to the LC/MS diverter valve inlet filter. See Figure 19 on page 20. WA R N I N G The LC/MS Liquid Chromatograph diverter valve is an integral part of the G1978B safety system. The LC mobile phase flow must always be connected to the diverter valve inlet filter. Never bypass the diverter valve and connect directly to the nebulizer.
Agilent G1978B Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide 2 Verification To verify sensitivity for 6120 Quad - G1978B Multimode, Positive SIM Modes 22 To verify sensitivity for 6130 and 6140 Quads - G1978B Multimode, Positive SIM Modes 24 To verify sensitivity for 6130 and 6140 Quads - G1978B Multimode, Positive Scan Modes 27 To verify sensitivity for the G1978B Multimode using Multiple FIA method in Mixed Mode operation 30 To do an autotune 32 Example of multimode verification report
2 Verification To verify sensitivity for 6120 Quad - G1978B Multimode, Positive SIM Modes To verify sensitivity for 6120 Quad - G1978B Multimode, Positive SIM Modes NOTE The G6110A instrument does not support the multimode source without the Selection valve. Use the option kit G2735H to enable the G6110A to work with the multimode source. Preparation 1 Transfer 1 mL of 5 ng/µL reserpine (Agilent G2423A) to a 50 mL volumetric flask. Use a clean graduated pipette.
Verification To verify sensitivity for 6120 Quad - G1978B Multimode, Positive SIM Modes Table 1 2 6110 and 6120 Quad Performance Verification Summary Table Method name Performance Specification G1978B ES Positive SIM Mode G1978B APCI Positive SIM Mode 6110SIMES_MM.M (6110 Quad) 6110SIMCI_MM.M (6110 Quad) 6120SIMES_MM.M (6120 Quad) 6120SIMCI_MM.
2 Verification To verify sensitivity for 6130 and 6140 Quads - G1978B Multimode, Positive SIM Modes When the method is finished, a report prints showing the signal-to-noise ratio for the five blank and five sample peaks, and a blank-subtracted average of the sample peaks. The blank-subtracted average signal-to-noise value must be greater than or equal to 20:1 peak-to-peak (100:1 RMS).
Verification To verify sensitivity for 6130 and 6140 Quads - G1978B Multimode, Positive SIM Modes Table 2 2 6130 and 6140 Quad Performance Verification Summary, SIM Mode G1978B ES Positive SIM Mode G1978B APCI Positive SIM Mode Solvent 75:25 methanol/water with 5mM ammonium formate 75:25 methanol/water with 5mM ammonium formate Method name 6130SIMES_MM.M (6130 model) 6130SIMCI_MM.M (6140 model) 6140SIMES_MM.M (6140 model) 6140SIMCI_MM.
2 Verification To verify sensitivity for 6130 and 6140 Quads - G1978B Multimode, Positive SIM Modes experiments to achieve maximum instrument sensitivity 7 Review the results. When the method is finished, a report prints showing the signal-to-noise ratio for the five blank and five sample peaks, and a blank-subtracted average of the sample peaks. The blank-subtracted average signal-to-noise value must be greater than or equal to 20:1 peak-to-peak (100:1 RMS).
Verification To verify sensitivity for 6130 and 6140 Quads - G1978B Multimode, Positive Scan Modes 2 To verify sensitivity for 6130 and 6140 Quads - G1978B Multimode, Positive Scan Modes Preparation 1 Transfer 1 mL of 5 ng/µL reserpine (Agilent G2423A) to a 50 mL volumetric flask. Use a clean graduated pipette. 2 Dilute to the 50 mL mark with 75:25 methanol/water with 5 mM ammonium formate. 3 Transfer 5 mL of the first dilution to a 50 mL volumetric flask. Use a clean graduated pipette.
2 Verification To verify sensitivity for 6130 and 6140 Quads - G1978B Multimode, Positive Scan Modes Table 3 6130 and 6140 Quad Performance Verification Summary, Scan Mode Method name Performance Specification G1978B ES Positive Scan Mode G1978B APCI Positive Scan Mode 6130SCNES_MM.M (6130 Quad) 6130SCNCI_MM.M (6130 Quad) 6140SCNES_MM.M (6140 Quad) 6140SCNCI_MM.
Verification To verify sensitivity for 6130 and 6140 Quads - G1978B Multimode, Positive Scan Modes 2 When the method is finished, a report prints showing the signal-to-noise ratio for the five blank and five sample peaks, and a blank-subtracted average of the sample peaks. The blank-subtracted average signal-to-noise value must be greater than or equal to 20:1 peak-to-peak (100:1 RMS). Sensitivity Verification for Multimode in APCI, Positive Scan Mode 1 Start the ChemStation software.
2 Verification To verify sensitivity for the G1978B Multimode using Multiple FIA method in Mixed Mode operation To verify sensitivity for the G1978B Multimode using Multiple FIA method in Mixed Mode operation Preparation 1 Do an autotune if necessary. After the autotune has completed, you may need to wait up to 30 minutes before continuing to allow the calibrant solution to be pumped out of the Quad instrument. This minimizes any background signal from the calibrant.
Verification To verify sensitivity for the G1978B Multimode using Multiple FIA method in Mixed Mode operation 2 d Click OK. 8 Repeat for the MMCheckSL_CI.M data file. Use the same subdirectory and change Data File to Multi_CI. 9 Repeat for the MMCheckSL_MX.M data file. Use the same subdirectory and change Data File to Multi_MX as the data file name. 10 Click Run to start the sequence. 11 Review the results. When the last method has finished, the report “Multimode Verification Report” prints.
2 Verification To do an autotune To do an autotune Tuning the multimode source is done in MM-APCI mode only. Autotune is done from the same menu as with all sources. • From the MSD Tune view, select Instrument > Autotune menu item. The tune report will have a header with either the title MM-APCI Positive Mode - Standard Scan or MM-APCI Negative Mode - Standard Scan. You can run the check tune after an autotune to validate that the instrument passes check tune criteria.
Verification Example of multimode verification report 2 Example of multimode verification report Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide 33
2 34 Verification Example of multimode verification report Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide
Agilent G1978B Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide 3 Methods To setup a method to use the multimode source 36 To create a method for positive/negative mixed mode operation 37 To create a method for alternating ESI and APCI operation 39 This chapter describes the tasks that you need to set up methods for the multimode source.
3 Methods To setup a method to use the multimode source To setup a method to use the multimode source To have your method use a multimode source, follow these steps: 1 Open the MSD Spray Chamber dialog box by clicking Instrument > MSD Spray Chamber in the Method and Run Control view. 2 Set Method Spray Chamber to MM-ES+APCI. 3 Verify that Installed Spray Chamber is set to MM-ES+APCI. 4 Make any other changes that are necessary for your method. 5 Click the OK button.
Methods To create a method for positive/negative mixed mode operation 3 To create a method for positive/negative mixed mode operation 1 Open the MSD Spray Chamber dialog box by clicking the Instrument > Set Up MSD Signals in the Method and Run Control view. 2 Select MM-ES_APCI from the Method Spray Chamber drop-down list. 3 Check that Installed Spray Chamber is also set to MM-ES+APCI. 4 Make any other changes that are necessary for your method. 5 Click the OK button.
3 Methods To create a method for positive/negative mixed mode operation Polarity options for Signal 1 and Signal 2 Figure 21 38 Positive/Negative polarity switching using Set Up MSD Signals dialog box Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide
Methods To create a method for alternating ESI and APCI operation 3 To create a method for alternating ESI and APCI operation 1 Open The MSD Spray Chamber dialog box by clicking Instrument > MSD Spray Chamber in the Method and Run Control view. 2 Set Method Spray Chamber to MM-ES+APCI. Figure 22 Method Spray Chamber set to MM-ES+APCI. 3 Check that Installed Spray Chamber is also set to MM-ES+APCI. 4 Make any other changes that are necessary for your method. 5 Click the OK button.
3 Methods To create a method for alternating ESI and APCI operation 9 Click the OK button. NOTE In general, use the mixed mode operation (MM-ES+APCI setting with Signal 1) instead of alternating MM-ES (Signal 1) and MM-APCI (Signal 2) mode switching. Two times as many scans are obtained during elution of a chromatographic peak, and no delay is needed between scans, resulting in better data.
Index Index A autotune, 32 C converting from ESI, APCI or APPI, 15 converting to ESI or APCI, 14 D diverter valve inlet filter, 20 E ESI convert from, 15 convert to, 14 I installation, 7, 21 L LC/MSD sample tubing, 20 M method alternating ESI and APCI, 39 basic setup, 36 positive/negative mixed mode, 37 multimode nebulizer, 19 source image, 35 P parts multimode spray shield, 17 S spray shield for multimode source, 17 Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide 41
Index 42 Multimode Source for 6100 Series Single Quad LC/MS Set-Up Guide
www.agilent.com In This Book This book contains installation, operation, maintenance and troubleshooting instruction for the Multimode Source for 6100 Series Single Quad LC/MS. © Agilent Technologies, Inc.
