IONSCAN -LS. Quick Start Guide. Revision A, April 2005 Part Number USA

Transcription

1 IONSCAN -LS Quick Start Guide Revision A, April 2005 Part Number USA

2 IONSCAN-LS IM-Station Software version: IONSCAN-LS Firmware Version: Autosampler Firmware: 4.38 OPTIC Firmware 1.07 The following trademarks are used in this document: IONSCAN -LS is a registered trademark of Smiths Detection Scientific. Drierite is a registered trademark of W. A. Hammond Drierite Co. Hydroguard is a trademark of Restek Chromatography Products. Kimwipes is a registered trademark of Kimberly Clark Corp. Teflon is a registered trademark of EI du Pont de Nemours & Co. Merlin Microseal is a trademark of Merlin Instrument Co. Microsoft and Windows are registered trademarks of Microsoft Corporation This manual describing IONSCAN -LS Detection System contains proprietary concepts and embodiments, which are the subjects of patents and patents pending. No part of this manual may be reproduced or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, or otherwise, without prior written permission of the publisher. To obtain permission for reprints, or to obtain additional copies of this manual, please contact your local Smiths Detection office.

3 Contents Contents i PREFACE Safety Precautions iii CHAPTER 1 Start Up Operations Mechanical Checks Basic Cabling Air Purification Unit (APU) Autosampler HPI Syringe Start Up Log On Set Preferences IONSCAN-LS Quick Start Guide i

4 Contents System Parameters Select a Method Acquire Data Program Peaks Program Data Acquisition Parameters Program Autosampler Procedures Set up the HPI Configuring HPI Hot Injection Cold Injection Increase Acquisition Time CHAPTER 2 Reference Information Conventions Acronyms Filenames and Directories Method Files Sample Files Index ii IONSCAN-LS Quick Start Guide

5 PREFACE Safety Precautions General Read all of the safety information in this chapter before using the IONSCAN-LS. Compressed Gas The IONSCAN-LS flow and cooling uses compressed gas cylinders, air or nitrogen. Note: Gas controls are not designed for operation with explosive, corrosive, or toxic gases IONSCAN-LS Quick Start Guide iii

6 Safety Precautions. Warning! High pressure gas can cause rapid suffocation. Store and use only with adequate ventilation. Use equipment rated for cylinder pressure. See the rating on the gas cylinder for maximum temperature. Close valves when not in use or empty. Secure cylinders both during use and in storage. Use in accordance with the appropriate Materials Safety Data Sheet (MSDS). Hot Surfaces Warning! Burn Hazard. The IONSCAN-LS components operate at high temperatures. Never service these areas until they have cooled to room temperature. Turn the unit off and allow it to cool before servicing. The IONSCAN-LS default operating temperatures are shown in the following table. Negative Mode Positive Mode IMS tube 114 C 225 C Inlet 240 C 280 C Desorber 233 C 285 C HPI Injector could reach temperatures of C HPI Transfer line 280 C 280 C iv IONSCAN-LS Quick Start Guide

7 Radiation Hazard Because of the high operating temperatures of the parts shown in the preceding table, the inlet cover and sample tray may also become very hot during operation. Always allow the IONSCAN-LS to cool to room temperature before servicing. Radiation Hazard Warning! Radiation Hazard. The IMS inlet, radiation source, and drift tube must never be opened by untrained personnel. UNDER NO CIRCUMSTANCES should an attempt be made to open or clean the IONSCAN-LS detector, inlet, or drift tube. In the event of fire, explosion, malfunction, damage or suspected damage, contact a Smiths Detection Scientific Service Engineer immediately. The IONSCAN-LS Detection System contains a sealed nickel-63 ( 63 Ni) foil radioactive source of 555 MBq (15 mci) activity. The source is fully enclosed inside the detector module resulting in no direct radiation hazard. Perform a radiation leak test periodically (refer to the IONSCAN-LS User Guide), or in the event of damage to the IONSCAN-LS to ensure radiation safety. IONSCAN-LS Quick Start Guide v

8 Safety Precautions In the event of a fire or explosion involving damage or suspected damage to the IMS detector cell or any area containing the IMS detector cell: 1. Cover the IONSCAN-LS with an appropriate container. 2. Return it to the manufacturer. In the event of a malfunction with the IMS detector cell: 1. Cease use of the device. 2. Place the IONSCAN-LS in an appropriate container. 3. Return it to the manufacturer for repair. In the event of suspected damage to the IMS detector cell: 1. Cease use of the device. 2. Cover the IONSCAN-LS with an appropriate container. 3. Arrange for a leak test to be conducted on the IMS Detector Cell. 4. Return it to the manufacturer for repair. The equipment must be handled in accordance with the licensing requirements of the applicable nuclear regulatory agency. Refer to APPENDIX A Handling of Radioactive Sources (USA) in the IONSCAN-LS User Guide. Should the IONSCAN-LS require disposal, return it to Smiths Detection Scientific. vi IONSCAN-LS Quick Start Guide

9 Electrical Shock Electrical Shock Warning! Risk of Electrical Shock. Observe the same precautions as for any electrically-powered appliance. Check for frayed cables or broken connectors. Never operate the IONSCAN-LS on wet surfaces. Never attempt service of any components until the main power supply has been disconnected. The IONSCAN-LS, Autosampler, and HPI operate on 110 VAC to 240 VAC. Do not turn on the HPI injector control box with the HPI injector disconnected as this can result in serious damage. Do not remove the housing of any of the components. If you suspect an electrical problem, contact your local Smiths Detection Scientific Service Engineer. IONSCAN-LS Quick Start Guide vii

10 Safety Precautions Fumes Warning! Avoid inhaling vapors of solvents used while operating or cleaning the IONSCAN-LS. Acetone is the recommended solvent for cleaning IONSCAN-LS parts. Use with adequate ventilation and avoid inhaling solvent vapors. When possible direct exhaust port fumes to a fume hood. Dispose of solvents in accordance with local regulations. Do not use chlorinated solvents for cleaning IONSCAN-LS parts. viii IONSCAN-LS Quick Start Guide

11 Mechanical Mechanical Warning! Risk of Pinching/Bruising. Moving parts on the Autosampler present an injury risk. The Autosampler system moves rapidly. This movement may prove hazardous to untrained personnel. They syringe may move at any time. Always keep the syringe path clear. IONSCAN-LS Quick Start Guide ix

12 Safety Precautions x IONSCAN-LS Quick Start Guide

13 CHAPTER 1 Start Up Operations This Guide is designed to get the user operational on the IONSCAN- LS quickly. It provides step-by-step instructions for starting up the system, acquiring data, and programming peaks. It also gives instructions for setting up the High Performance Injection (HPI) unit. For further information, refer to the IONSCAN-LS User Guide, which provides complete details on all aspects of the IONSCAN-LS. 1.1 Mechanical Checks Before using the IONSCAN-LS, perform the following mechanical checks Basic Cabling The connections between the IM-Station PC and the IONCAN-LS, Autosampler, and HPI are serial connections. These connections are IONSCAN-LS Quick Start Guide 1

14 Start Up Operations made by connecting the USB port on the PC to a four-port USB serial hub. The three devices are then connected to the hub using serial cables. Check that the COM port connections are correct as shown in the following table. Port Unit Speed COM Port 1 HPI 19,200 bps COM Port 2 Autosampler 19, 200 bps COM Port 3 IONSCAN-LS 57,600 bps Air Purification Unit (APU) Check the Drierite in the Air Purification Unit (APU) located in the back of the IONSCAN-LS and change the APU if there is less than 1 of blue Drierite remaining at the bottom. Air Line/ Connector Bottle Velcro Strap Velcro Strap Air Line/ Connector To change the APU: 2 IONSCAN-LS Quick-Start Guide

15 Mechanical Checks 1. Place the IONSCAN-LS in Standby mode using the front panel Ready/Standby button. 2. Disconnect the two air line quick connectors. 3. Release the Velcro straps and remove the APU bottle. 4. Unscrew the top and bottom aluminum fittings and set them aside. 5. Discard or recycle the Drierite, charcoal, and plastic bottle according to local regulations. 6. Remove the top foil from a new bottle (part number ) and replace it with the top aluminum fitting from Step Reconnect the top air line quick connector. 8. When the bottom foil on the new APU bottle begins to bulge due to air pressure, remove the foil and attach the bottom aluminum fitting, and insert the APU bottle into the IONSCAN-LS. 9. Secure the new APU with the Velcro straps. 10. Reconnect the bottom air line quick connector. Note: If the Drierite was completely spent, the ION- SCAN-LS must be purged of possible moisture con- IONSCAN-LS Quick Start Guide 3

16 Start Up Operations tamination. Refer to the IONSCAN-LS User s Guide for this procedure Autosampler The Autosampler should be checked for mechanical operation (overall ease of movement) and targeting as described in this section Mechanical Operation Check the movement of the Autosampler: 1. Turn the Autosampler power switch, located on the back of the unit, to OFF. 2. Refer to the following figure and check the movement of the parts of the Autosampler. Plunger driver Syringe arm Needle Guide Foot 4 IONSCAN-LS Quick-Start Guide

17 Mechanical Checks a. Manually move the syringe arm back and forth along its axes: forward/back right/left vertical b. Manually move the plunger driver up and down. c. Manually move the needle guide foot up and down. 3. Manually move the slide tray on the IONSCAN-LS back and forth using the slide tray lever. Slide tray Slide tray lever 4. All motions should be smooth with little resistance. Resistance or a shaking motion indicates a need for cleaning or adjustment. If a cleaning is indicated, refer to the IONSCAN-LS User Guide Targeting After turning on the Autosampler, use the procedures in this section to make sure the targeting is correct for the following positions: Sample 1 vial, Waste 1 vial, Rinse 1 vial, Inject A and Inject B. Targeting is done at the time of installation. However, it is best to check Autosampler targeting before running it. Even a small misalignment can break the syringe and damage the system. IONSCAN-LS Quick Start Guide 5

18 Start Up Operations To check the Autosampler targeting use the Autosampler keypad shown in the following figure: Remove the syringe from the Autosampler for approximate targeting. Once the target is approximated as correct, install a syringe and repeat the process. 1. Be sure there is a vial in the sample 1, rinse 1, and waste 1 positions on the sample tray. The vials may be empty for this procedure. Recommended: Position 1: clear sample vial with cap but no septum. 2. Make sure the sample tray is firmly installed; that is, pressed down and seated on its mounting area. Waste 1 Sample 1 Rinse 1 Note: The sample tray has 120 sample positions and four rinse/waste positions with position numbers 6 IONSCAN-LS Quick-Start Guide

19 Mechanical Checks marked in a grid as shown in the figure. The rinse/ waste positions are larger than the vial positions. The waste/rinse vial holders are shown on the right hand side in the preceding figure; however, these holders may be mounted on the left side of the sample tray if an HPI unit is not installed. 3. Press the Prog key on the Autosampler (Cobra L/S) keypad. The procedure can be stopped at any point by pressing the red Hold/Stop button. 4. Select Cobra Setup using the arrow keys. 5. Press Enter. 6. Select Configuration and press Enter. 7. Use the arrow keys to select Sample Press Enter. Observe the movement of the syringe arm. It should move to the center of the vial in sample position 1. For/Back Vertical Right/Left Sample Vial 1 Waste 1 Rinse 1 Inject A Inject B 9. Record the observed values for the target in the table above. 10. Press Enter. The syringe arm will return to its home position. 11. Use the arrow keys to select Waste. 12. Press Enter. Observe the movement of the syringe arm. It should move to the center of the vial in Waste position Record the observed values for the target in the table above. 14. Press Enter. The syringe arm will return to its home position. 15. Use the arrow keys to select Rinse. 16. Press Enter. Observe the movement of the syringe arm. It should move to the center of the vial in Rinse position 1. IONSCAN-LS Quick Start Guide 7

20 Start Up Operations 17. Record the observed values for the target in the table above. 18. Press Enter. The syringe arm will return to its home position. 19. Use the arrow keys to select Inject A. 20. Press Enter. Observe the movement of the syringe arm. It should move to the Teflon substrate. 21. Record the observed values for the target in the table on page Press Enter. The syringe arm will return to its home position. 23. Use the arrow keys to select Inject B. 24. Press Enter. Observe the movement of the syringe arm. It should move to the HPI injection port. 25. Record the observed values for the target in the table on page Press Enter. The syringe arm will return to its home position. If the targeting for any of the vials or targets is not correct, refer to the IONSCAN-LS User Guide. (If any targeting coordinates are changed they must be manually entered into the Control Parameters on the IM-Station software.) If the approximate targeting for all of the vials and targets is correct, replace the syringe in the syringe arm, and repeat the procedure for exact targeting HPI Before turning on the High Performance Injection (HPI) unit, check the OPTIC liner and replace it if necessary. Refer to the following figure (which shows a top view of the HPI injection port) to check the liner. 1. Remove the inlet cap using the large nut near the top. 8 IONSCAN-LS Quick-Start Guide

21 Mechanical Checks 2. Wearing gloves, pull the glass OPTIC liner out of the HPI injector area. Unscrew large nut to remove inlet cap 3. When the liner is removed, the sealing O-ring may come out with it. If it does not, remove it with a forceps and put it on a clean surface. 4. Visually inspect the tube for particle build-up on the central glass frit and on the inside of the glass. 5. If the liner has a glass bead frit, look down the length of the liner to check whether the frit is intact. 6. If contaminants are present or if the frit is damaged, discard the liner and obtain a new one. 7. Slide the O-ring over the new or clean liner. 8. Replace the new or clean liner in the injector. Once the O-ring is seated, push down gently to seat the liner properly in the injector. Excessive force can damage the liner. 9. Replace the inlet cap and tighten the nut finger tight. 10. If you use a new liner, it should be baked out at C for thirty minutes before use. The bake out should be done in Standby mode with the split open at about 50 ml/min. For details on bake out, refer to the IONSCAN-LS User Guide. IONSCAN-LS Quick Start Guide 9

22 Start Up Operations Syringe A dirty syringe is the most common cause of inconsistent data when using the IONSCAN-LS. Test the syringe by manually raising and lowering the plunger. If there is any resistance, either use a new syringe or clean the dirty one with methanol and acetone and verify that the plunger moves freely. 1.2 Start Up Turn on the system using the on-off switches on the back of the three components: IONSCAN-LS Autosampler HPI. The front panel keypad and display area of the IONSCAN-LS is shown on page 3. After turning on the system, the Standby LED on the front panel will light indicating that the system is in Standby mode. To bring the system to operational mode, press the Ready/Standby button on the IONSCAN-LS front panel. The Ready LED will flash as the ION- SCAN-LS comes to the ready state. When the Ready LED is on steady, the system is ready Log On 1. Turn on the IM-Station PC. 2. Open the IM-Station software. The Login dialogue window will be displayed. 3. Log onto the system using the appropriate User ID and password (assigned by the master user or security officer). 10 IONSCAN-LS Quick-Start Guide

23 Start Up 4. Verify that the software is communicating with the IONSCAN-LS. Idle should be displayed on the IM-Station PC status line. Refer to the following figure. Status line If Offline is displayed (as shown above), select Instrument from the top menu bar of the software and click Connect Set Preferences Supervisor level users can set supervisor and production preferences. 1. After logging in, as described in Section Log On, click on File on the main menu bar. IONSCAN-LS Quick Start Guide 11

24 Start Up Operations 2. Select Preferences to set supervisor-level preferences or select Production Preferences to set production operator-level preferences. Either selection will display a screen similar to the one shown below. Note: The screens and options are identical for Supervisor and Production Preferences except for the screen title. 3. The suggested selections on the General tab in the figure above are to set the date and time format and take the default for the Automatically close active documents field. Note: Detailed descriptions of all entry fields are described in the IONSCAN-LS Software Manual; however, the suggestions in this section are a good starting point. More experienced users may wish to change the values. 12 IONSCAN-LS Quick-Start Guide

25 Start Up 4. Click on the Layout tab in the preceding figure to display the following screen. 5. Click on the Advanced Defaults button and make sure Enable algorithm options is checked. This selection gives the user the maximum viewing options on the sample files. 6. Click OK to save the values System Parameters The IONSCAN-LS software includes many control parameters. These parameters are discussed in detail in the IONSCAN-LS Software Manual. The following parameter sets should never be changed: HPI: System Configuration HPI: IMS and Autosampler Input/Output Parameters HPI: Transfer Line Parameters The following parameter sets should only be changed by advanced users: IONSCAN: Miscellaneous Parameters IONSCAN: Calibrant Parameters Autosampler: General Parameters IONSCAN-LS Quick Start Guide 13

26 Start Up Operations The exceptions are: 1. Autosampler general parameters may be changed to amend targets as necessary. 2. Calibrant reference may be changed to bring the IONSCAN-LS into ready mode. 3. The desorber and inlet temperatures may be changed if required. Changes to control parameters are generally outside the scope of this document. Refer to the IONSCAN-LS User Guide and the IONSCAN- LS Software Manual before modifying control parameters Desorber and Inlet Temperatures The desorber temperature is adjusted to vaporize the analyte completely without decomposition, and the inlet temperature is set either at the temperature of the desorber or higher to ensure that the analyte remains in the vapor state as it travels into the drift tube. These temperatures are set on the Miscellaneous tab (shown below) as described in the IONSCAN-LS Software Manual. 14 IONSCAN-LS Quick-Start Guide

27 Select a Method 1.3 Select a Method There are two available polarities: negative ion mode and positive ion mode. Note: The drift tube temperature in positive mode (230 C) is higher than in negative mode. The system will take about 30 minutes to reach this temperature. The drift tube temperature in negative mode is approximately 110 C. The system will take about one to two hours to cool to this temperature. Check the temperature at any time by pressing the Status button on the front panel. The IONSCAN-LS will switch to the polarity of the method selected. To select the method open the IM-Station software as described in Section Log On and continue as follows: 1. Make sure all windows on the IM-Station are closed. 2. Go to Setup on the top menu bar of the software. 3. Click Select Method. 4. Select the method from the pull down menu that corresponds to the mode (positive or negative) the IONSCAN-LS is operating in. Click OK. 5. Wait for the Ready LED on the front panel to remain on steady. If the system is not ready, the Ready LED will continue to blink. This may take a few minutes or a couple of hours if the mode of the selected method is different than the previous operating mode of the IONSCAN-LS. 6. When the Ready LED is on steady, continue with Section 1.4 Acquire Data. Note: If the Ready LED continues to blink, refer to the IONSCAN-LS User Guide. IONSCAN-LS Quick Start Guide 15

28 Start Up Operations 1.4 Acquire Data After performing the steps in Section 1.2 Start Up and after selecting a method as described in Section 1.3 Select a Method, data can be acquired using the steps below 1. Select Instrument from the top menu bar of the software: 2. Select Acquire Sample. 3. Place a clean Teflon filter on the sampling tray. 4. Slide the sample tray to the right, into the inlet (refer to the figure on page 5). The system will immediately begin to acquire the data. Once it has finished a beep will sound. 5. When the beep sounds, slide the sampling tray to left, out of the inlet. 6. In a few seconds the plasmagram will be displayed on the PC. The main peak displayed is the calibrant peak. Zoom in on any section of the plasmagram by dragging the cursor across the area of interest. The following figure shows two views of a plasmagram run on a clean Teflon filter in positive mode. 7. Repeat Steps 4 to 6 two to three times to clean out any extraneous peaks from the new filter. 16 IONSCAN-LS Quick-Start Guide

29 Program Peaks 1.5 Program Peaks Note: If the method selected in Section 1.3 Select a Method already has peaks programmed for the compounds you are running and the compounds have been successfully detected, you may skip to the next section. After performing the steps in Section 1.2 Start Up and after selecting a method as described in Section 1.3 Select a Method, peaks can be programmed using the steps below. 1. Select Instrument from the top menu bar of the software. 2. Select Acquire Sample. 3. Deposit the sample on the clean Teflon filter. 4. Slide the sample tray to the inlet. 5. View the 2-D plasmagram and decide which peak to program. As an aid in selecting a peak, zoom in to increase the size of the peaks by dragging the cursor through the peak area of interest. 6. Select Single Segment from the pull-down menu near the center on the top of the 2-D plasmagram (refer to the following figure). Record values Select Single Seg Scroll segments Right click for Gaussian Fit 7. Scroll through the segments using the up/down scroll buttons on the Segments/DesTime selection window on the top of the 2-D plasmagram until the peak of interest is at its maximum height. IONSCAN-LS Quick Start Guide 17

30 Start Up Operations 8. Move the cursor inside the peak and right click on it. 9. Select Gaussian Fit. The 2-D plasmagram will now display the gaussian fit, similar to the one shown above. Record the values shown for FWHM, Peak DTime, and Peak K 0 displayed on the 2-D plasmagram 10. Stop the Acquiring Data Process by clicking on the x on the Automatic Sampling window. 11. Go to Setup on the top menu bar of the software; select Control Parameters. 12. Click on the IONSCAN tab on the upper row of tabs. 13. Click on the Det Alg tab on the lower row of tabs. This will display a screen similar to the one shown below: 14. Create a channel: Right click in the Channels column. A selection window will pop-up (similar to the one shown in Step 16). Select Create channel. Another window will pop up (similar to the one shown in Step 16). 18 IONSCAN-LS Quick-Start Guide

31 Program Peaks Enter a name. Click OK. 15. Create a substance: Right click in the Substances column. A selection window will pop-up (similar to the one shown in Step 16). Select Create substance. Another window will pop up (similar to the one shown in Step 16). Enter a name. Click OK. 16. Create an alarm: Right click in the Alarms column. A selection window similar to the one shown below will pop up. IONSCAN-LS Quick Start Guide 19

32 Start Up Operations Select Create alarm. Another window will pop up as shown below. Enter a name. Click OK. 17. Input values for the peak you are programming: a. Right click on the name of the channel added in Step 14 in the Channels column. b. Select Modify channel parameters from the pop-up window. This will display the Channel Parameters dialogue window as shown below. c. Make the following entries for the channel: K 0 value obtained in Step 9 Vr blty enter 50 Blok Th enter 1 Amp Th enter 15 FWHM enter the value obtained in Step 9 Seq Hits enter 1 20 IONSCAN-LS Quick-Start Guide

33 Program Peaks ExtAmp Th enter 4095 Note that Rpt Mthd is not implemented in this version of the IM Station software. 18. Link the Alarm, Substance, and Channel: a. In the Substances column right click on name of the substance entered in Step 15: Select Add Channels. b. In the Channels column, right click on the name of the channel entered in Step 14: Select Add to Substance. c. In the Alarms column, right click on the name of the alarm entered in step Step 16: Select Add Substances. d. In the Substances column right click on name of the substance entered in Step 15: Select Add to Alarm. Note: Multiple channels (Step 14) and substances (Step 15) can be defined for a compound that generates multiple ion peaks. Additionally, channels and substances can be defined as mandatory or optional for an alarm. For procedures on these topics, refer to the IONSCAN-LS User Guide. 19. Confirm Usage: In the Channels column, right click on the name of the channel entered in Step 14 and select Highlight Usage to check that the peak, has been properly linked in the Channels, Substances, and Alarms columns. If it is not, repeat Step At this point the user may choose to turn off any unused alarms by right-clicking on the unused alarm in the Alarms column and selecting Turn alarm off for each unused alarm. 21. Click Apply. 22. Save the method: IONSCAN-LS Quick Start Guide 21

34 Start Up Operations a. Select File from the top menu bar of the software. b. Select Save As... This will display the following screen: c. Select the option: File (new production method) d. Select the option: Instrument (method is selected on the active mode) e. Click Save. 22 IONSCAN-LS Quick-Start Guide

35 Program Data Acquisition Parameters 1.6 Program Data Acquisition Parameters Note: If the method selected in Section 1.3 Select a Method already includes the desired acquisition parameters, you may skip to the next section. After performing the steps in Section 1.2 Start Up and after selecting a method as described in Section 1.3 Select a Method, data acquisition parameters can be programmed using the steps below. 1. Go to Setup on the top menu bar of the software; select Control Parameters. 2. Click on the IONSCAN tab on the upper row of tabs. 3. Click on the Data Acq tab on the lower row of tabs. This will display a screen similar to the one shown below. 4. Check the Scan period (ms) field. This value must be long enough to allow the slowest ions to reach the detector. To change the value: IONSCAN-LS Quick Start Guide 23

36 Start Up Operations Click in the field entry box, type in the new value and press the Enter key on the PC keyboard. 5. Check the Number of co-added scans per segment field. This is the number of scans added together before data processing. It is used to increase the signal-to-noise ratio. To change the value, refer to Step Check the Analysis duration (s) field. This value must be long enough to allow detection of all peaks of interest and prevent carryover. In order to set the Analysis duration (s) to a value greater than the current value of the Maximum analysis duration (s), the value of the Maximum analysis duration (s) must first be increased. To change the values, refer to Step The analysis duration can be split into two or three stages by clicking on the down arrow to the right of 1 Stage in the preceding figure. For each stage the user can select the Number of co-added scans per segment and the Analysis duration. 8. Check the Delay (ms) before start of sampling for each scan field. This field allows you to define when data sampling starts in each scan. It is used to discard early scan data to reduce file size as no useful data will be available this early. To change the value, refer to Step Make changes to any of the other fields on this screen as required. 10. After all changes have been made, click Apply. 11. Save the values as described in Step 22 under Section 1.5 Program Peaks on page IONSCAN-LS Quick-Start Guide

37 Program Autosampler Procedures 1.7 Program Autosampler Procedures Note: If the method selected in Section 1.3 Select a Method already includes the desired Autosampler parameters, you may skip to the next section. After performing the steps in Section 1.2 Start Up and after selecting a method as described in Section 1.3 Select a Method, Autosampler procedures can be programmed using the steps below. 1. Go to Setup on the top menu bar of the software: 2. Select Control Parameters. 3. Click on the AUTOSAMPLER tab on the top row of tabs. 4. Click on the A/S Method tab on the bottom row of tabs. You will see a default method (installed by the Smiths Detection Scientific representative at the time of system installation). a. Go to the Dispense to Target field and select either Target A for Teflon substrate sampling or Target B for HPI. b. Go to the Operation Mode field and select either Continuous or HPI Triggered from the drop down menu. With Continuous selected, the Autosampler will make its injection once it receives a ready signal from the ION- SCAN-LS. If HPI Triggered is selected in this field, the Autosampler will not make an injection until it receives a ready signal from both the IONSCAN-LS and HPI. IONSCAN-LS Quick Start Guide 25

38 Start Up Operations Continuous is generally used for Teflon sample introduction and HPI hot injection. HPI Triggered is generally used for HPI cold injection. c. Click Apply. 5. Click on the A/S Procs tab on the bottom row of tabs to display the following: 6. In the Procedure Name field enter a name for your procedure. 7. Click in the value box for A/S Method Name ; a drop down menu will appear. 8. You will see the default method developed by the Smiths Detection Scientific representative. Select this method. Note: You can view the values associated with the default method using the A/S Methods tab at the bottom row of tabs as described in Step In the Number of Repetitions per Sample field, enter the number of injections to be made from each vial. 10. In the Start Sample Vial Number field, enter the vial number of the first vial to be sampled according to its position in the sample tray. Note: The sample tray has a grid of 120 numbered sample positions. Vials may be placed in any of the 26 IONSCAN-LS Quick-Start Guide

39 Program Autosampler Procedures positions between numbers 9 and 112. When running more than one vial, they must be in sequential positions. 11. In the End Sample Vial Number field, enter the vial number of the last vial to be sampled according to its position in the sample tray. This position must either be higher than or the same as the position entered in the previous step. (If the start and end vial numbers are the same, only one vial will be sampled.) LAST may be entered, which will use the last vial previously specified in the A/S Samples tab. Refer to the IONSCAN-LS User Guide for details. Note: When selecting start and end vial numbers, the start position must be the lower number. For example, the Autosampler can start a run from vial 70 and finish at vial 73 but it cannot start a run from vial 73 and finish at vial 70. Example: As an example, in the case in which 70 is entered as the start vial and 73 is entered as the end vial and 3 is entered as the number of repetitions, the Autosampler will first make three injections from vial 70, then three injections from vial 71, then three injections from vial 72, and finally three injections from vial 73. This is the simple Autosampler method recommended for the beginner. For more advanced methods, refer to the ION- SCAN-LS User Guide. 12. Set the Cal Standard Vial field on the A/S Procs screen to Click Apply. IONSCAN-LS Quick Start Guide 27

40 Start Up Operations 14. Click on the A/S Samples tab on the bottom row of tabs. This will display the following fields: 15. Enter a name in the Batch Name field. A batch name is optional. 16. Delete all entries in the Cal Standards and Spikes Standards fields. 17. Fill in the vial numbers and descriptions of your samples in the Samples field. Vials must be entered in numerical order and numbers cannot be skipped. If the numbers of all the vials programmed in Steps above are not entered, the method will not work. Note: The Description field is not required, however, it will be helpful in analyzing plasmagrams if the description and concentration of samples are entered in this field. If a description is not entered, the corresponding plasmagram will not have a title and it may be difficult to identify. 18. Click Apply. 19. Save the values as described in Step 22 under Section 1.5 Program Peaks on page IONSCAN-LS Quick-Start Guide

41 Set up the HPI 1.8 Set up the HPI The HPI can be used for hot injection or cold injection of samples. Cold injection uses a low initial temperature and ramps the temperature up during the analysis. Hot injection maintains a high temperature throughout the analysis. Select the HPI injection type (hot or cold) based on the vaporizing tendency of the analyte. In general, for chemicals that vaporize easily use cold injection and for chemicals that are more difficult to vaporize, hot injection should be used. Before starting to work with HPI, make sure that the nitrogen cylinder is hooked up properly and all valves are open. The outlet pressure should be about 60 psi. After performing the steps in Section 1.2 Start Up and after selecting a method as described in Section 1.3 Select a Method, the HPI can be set up using the procedures in this section. Note: If either the Control Parameters or Plasmagrams window is displayed, Select Method will not be available on the Setup pull down menu. In that case, close the display by selecting Close All from FIle on the main menu bar Configuring HPI Before configuring HPI, acquire data and program peaks as described in Section 1.4 and Section Go to Setup on the top menu bar of the software and click on Control Parameters IONSCAN-LS Quick Start Guide 29

42 Start Up Operations 2. If the top row of tabs includes IONSCAN, Autosampler, and HPI, continue with the procedures in Section or Section below. 3. If the top row of tabs does not include the HPI tab continue with Step Go to Setup on the top menu bar of the software and click on Use HPI to select it. 5. Close the software by clicking the x in the top right hand corner of the screen. 6. Open the IM-Station software and log on as described in Section Log On Hot Injection The following procedures are for an HPI hot injection run with the HPI in standby mode. 1. Go to Setup on the top menu bar of the software and click on Control Parameters. 2. Click on the HPI tab on the top row of tabs. Note: if the HPI tab is not present, perform the steps 4 through 6 in Section Configuring HPI above to get the HPI tab. Once the HPI tab is displayed, start again from Step 1 in this procedure. 30 IONSCAN-LS Quick-Start Guide

43 Set up the HPI 3. Click on HPI Parameters on the bottom row of tabs. This will display four sets of parameters as shown in the following figure. 4. In the Standby Parameters field, set the following parameters with the values listed in the table below. Timeout 15 minutes Injector Temperature Control YES Standby Temperature as needed (operating range ) Standby Transfer Line Flow as needed (range 0 30 ml/min) Standby Split Valve State Splitless Standby Split Flow 0 Injector Cooling OFF Transfer Line Control YES TL Temperature 280 Note: It is very important to keep the transfer line temperature high to prevent condensation of materials in the transfer line. We recommend 280, however, if you see the product is decomposing at high temperature, adjust this value to a more suitable level. IONSCAN-LS Quick Start Guide 31

44 Start Up Operations Check the values on the HPI faceplate at any time. 5. Click Apply. 6. Click on the Autosampler tab on the top row of tabs. a. Click on A/S Methods tab on the bottom row of tabs. b. Make sure the value in the Dispense to Target field is set to the HPI target, Target B. c. Set the Post Dispense delay field to -1 to allow the tray to slide over to the sampling position before the injection is made. d. Make sure the value in the Operation Mode field is Continuous. e. Click Apply. 7. Program the sequence you will be using as described in Section 1.7 Program Autosampler Procedures earlier in this Guide. 8. Click on Setup on the top menu bar of the software and select Control Parameters. 9. Click on the IONSCAN tab on the top row of tabs. 10. Click on Det Alg on the bottom row of tabs. Make sure the peak of interest in is programmed and its alarm is on. To program the peak, go to Section 1.5 Program Peaks. 11. Save the values as described in Step 22 under Section 1.5 Program Peaks on page IONSCAN-LS Quick-Start Guide

45 Set up the HPI 12. Go to Setup on the top menu bar of the software and click on Use HPI to uncheck it. 13. Close the software by clicking the x in the top right hand corner of the screen. 14. Open the IM-Station software and log on as described in Section Log On. 15. Go to Setup on the top menu bar of the software and click on Select Method. 16. Select the name of the method you want from the pull-down menu. Click OK. 17. Go to Instrument on the top menu bar of the software. a. Select Auto Sample. The following window will be displayed: b. Select Procedural Mode. c. Click OK. A window similar to the following will be displayed: IONSCAN-LS Quick Start Guide 33

46 Start Up Operations d. Using the drop down menus, select the appropriate procedure names in the Start Procedure and End Procedure fields. e. Select the appropriate numbers in the Start Vial and End Vial fields. f. Click OK. 18. You will begin to acquire plasmagrams according to your programming once you have completed these procedures. The first plasmagram (used for programming) was based on the Teflon substrate. It is a good point to start; however, in some cases it is observed that the peaks differ in the plasmagrams obtained from the Teflon substrate and from HPI. For that reason, peaks may have to be reprogrammed, which can be done based on plasmagrams obtained in HPI using the procedure in Section 1.5 Program Peaks Cold Injection 1. Go to Setup on the top menu bar of the software and click on Control Parameters. 2. Click on the HPI tab on the top row of tabs. Note: if the HPI tab is not present, perform the steps 4 through 6 in Section Configuring HPI above to get the HPI tab. Once the HPI tab is displayed, start again from Step 1 in this procedure. 3. Click on the HPI Methods tab on the bottom row of tabs. This will display a screen similar to the one shown in the next figure. 4. Enter a name in the Method Name field and enter the values shown in the table for the other fields. Note: The ISO Time1, Carrier Flow Time1, and Split Flow Time1 fields are automatically set by the software. 34 IONSCAN-LS Quick-Start Guide

47 Set up the HPI. Method type splitless (select from a pull-down menu) End time 20 Initial Temperature about 5 C below the solvent boiling point Delay Time 0 Ramp Rate1 60 ISO Temperature1 280 Sample Sweep Carrier Flow 5 Start Carrier Flow1 5 End Carrier Flow1 5 Vent Time 0 Initial Split Flow 0 Split Flow1 0 Split Flow1 0 TL Temp 280 IONSCAN-LS Quick Start Guide 35

48 Start Up Operations 5. Click Apply. 6. Click on the Autosampler tab on the top row of tabs. a. Click on A/S Methods tab on the bottom row of tabs. b. Make sure the value in the Dispense to Target field contains the correct target for HPI, Target B. c. Set the Post Dispense delay field to -1 to allow the tray to slide over to the sampling position before the injection is made. d. Make sure the value in the Operation Mode field is HPI Trigger. e. Click Apply. 7. Program the sequence, check that the peaks are programmed, and save the values as described in Step 7 through Step 11 in Section Hot Injection. 8. Define the procedure and acquire data as described in Step 17 and Step 18 in Section Hot Injection Increase Acquisition Time In cold injection, peak acquisition may be longer than in other methods used in the IONSCAN-LS. If peaks are observed to appear very near the end of the run or if a peak is not seen because the run is not long enough, adjusting the acquisition time can remedy the problem. To do this: 1. Go to Setup on the top menu bar of the software, select Control Parameters. 2. Click on the IONSCAN tab on the upper row of tabs. 36 IONSCAN-LS Quick-Start Guide

49 Set up the HPI 3. Click on the Data Acq tab on the lower row of tabs. This will display the fields shown below: 4. Change the values as follows: Maximum Analysis Duration 30 Analysis Duration Click Apply. 6. Click on the HPI tab on the top row of tabs. 7. Click on the HPI Methods tab on the bottom row of tabs. 8. Change the End Time field to Click Apply. 10. Save the values as described in Step 22 under Section 1.5 Program Peaks on page 21. Note: Acquisition time can also be increased by increasing the post-dispense delay (on the A/S Methods tab). IONSCAN-LS Quick Start Guide 37

50 Start Up Operations 38 IONSCAN-LS Quick-Start Guide

51 CHAPTER 2 Reference Information This chapter provides a limited amount of reference information for this Guide. For complete details on the IONSCAN-LS refer to the IONSCAN-LS User Guide and the IONSCAN-LS Software Manual. 2.1 Conventions Selections available from the PC menu bar and pull-down menus are listed in bold typeface throughout the text. Screen titles and onscreen field titles are presented in quotation marks, e.g., Alarms. Keys and buttons on the IONSCAN-LS, Autosampler, and HPI keypads and display screens are presented in quotation marks, e.g., Prog. Options and items displayed on the Autosampler keypad display are presented in italic typeface. For example: High Voltage. IONSCAN-LS Quick Start Guide 39

52 Reference Information 2.2 Acronyms The following acronyms are used in this Guide. A/S APU FWHM HPI ID ISO LED PC Autosampler Air purification unit Full width half maximum High Performance Injection identification Isothermal Light emitting diode Personal computer 2.3 Filenames and Directories This section gives a brief overview of IONSCAN-LS files and directories. For a complete description, refer to the IONSAN-LS Software Manual. Note: Supervisor-level users set preferences for directories in which files are saved. A typical file structure for the IONSCAN-LS is shown below. 40 IONSCAN-LS Quick-Start Guide

53 Filenames and Directories Method Files Every method generates a method file. Each modification is stored as a separate method instance and, therefore, a separate method file. Each method instance is stored in a separate method directory. Method files are stored in the production method directory and use the file extension.icp. The filename has the form: For example: <prefix>-[generic method name]-<instance number> prefix is the serial number of the IONSCAN-LS. generic method name is a descriptive name for the method. instance number is automatically incremented by the IM-Station software [positive ion] icp Method files prepended with a T are test method files. Production operator level users can only access method files from the production directory Sample Files Every analysis performed on the IONSCAN-LS using the IM-Station software generates a sample analysis file (often called a plasmagram). These files are stored in the method directory of the method that was used to perform the analysis. The sample files use the extension.pos for samples run in positive polarity, or.neg for samples run in negative polarity. IONSCAN-LS Quick Start Guide 41

54 Reference Information For sample analyses run on the Autosampler, the filename has the form: For example: $nnnnnnn-mmm-[v-#].xxx $ indicates the sample is a production sample nnnnnnn is the 7-digit automatic sample count mmm is the vial number V is a 1 to 30 character vial description # is the sample injection number $ [20percentdiazapam-1].pos For samples run by selecting Acquire Sample from Instrument on the main menu bar, the sample name has the form: For example: $nnnnnnn.xxx $ pos For samples run by selecting Free Run from Instrument on the main menu bar, the sample name has the form: For example: nnnnnnn-freerunmode.xxx FREERUNMODE.pos Note that these files are not prepended with a $ and are therefore, not production files. 42 IONSCAN-LS Quick-Start Guide

55 Index A A/S 40 Acquire data 16 Acquisition time increase 36 Acronym list 40 Air Purification Unit (APU) 2 Alarms 18 APU 2, 40 Autorun 27 samples 42 Autosampler example procedure 27 keypad 6 mechanical operation 4 parameters 13 program procedures 25 targeting 5 B Bake out 9 C Cabling 1 Calibrant parameters 13 Channels 18 Cold injection HPI 34 COM Ports 2 Continuous 25 Control parameters 13 advanced users 13 modifying 14 Conventions 39 D Data acquisition 16 parameters 23 Desorber temperature 14 Document conventions 39 Drierite 2 IONSCAN-LS Quick Start Guide 43

56 Index F Faceplate HPI 32 Front panel keypad 10 FWHM 40 H Hot injection HPI 30 HPI 25, 29, 40 cold injection 34 configuring 29 control parameters 13 hot injection 30 injection port 8 OPTIC liner 8 parameters 13 set-up 29 HPI Triggered 25 I ID 40 Inlet temperature 14 ISO 40 K Keypad Autosampler 6 HPI 32 Keypad, front panel 10 L LED 40 M Mechanical checks 1 Mechanical operation checkinig 4 Method files 41 polarity 15 select 15 Miscellaneous parameters 13 O OPTIC liner (HPI) 8 P Parameters system 13 Password 10 PC 40 Plasmagram 16, 17, 34 Plunger arm 4 Polarity method 15 Preferences setting 11 Procedural run 33 Program peaks 17 S Sample files 41 Sample tray 6 Substances 18 Syringe 10 System parameters 13 T Targeting Autosampler 5 U User advanced 13 User ID 10 V Vial numbers IONSCAN-LS Quick Start Guide