Home

AutoTrace SPE Workstation User`s Manual

1. 31 SPE Parameters 74 Air Factor Ee 74 Autowash Vol 74 Push Delay 73 SPE Process Flow Charts 35 Specifications Collection Container Racks 161 Electrical 160 Gas Regulator 161 Liquid Management 160 Sample Pumps 161 Solid Phase Extraction 160 Weight aa 160 SIartUP Kile tos a KAG GA LG 11 20 Stop Continuous Routines 115 Supplies List 163 Switching Valves 31 Syringe Motors Chattering Sound 117 Syringe Problems 114 Syringe Stalls 119 Doc 065296 01 1 09 Index 171 T Technical Support Contacting S Testing Changes 107 Testing Operation 68 Troubleshooting 116 Cannot Download Method 118 Clicking Sound from Syringe 119 Column Holder LED Not Lit 122 Cross Contamination 123 Elution Station Not in Correct Position 124 Error Light On During Method 118 Leak on Column Holder O ring 122 Liquid Buildup in 10 mL Air Syringe 121 Low Recovery of Volatile Compounds 122 Method Does Not Run 117 Nothing Out of Elution Manifold Nozzle 020008 124 Ready Light Flashing 117 Ready Light NotLit te Run Light Not Lit after Loading 117 Sample Pump Fails to Start 123 Syr
2. DIONEX AutoTrace SPE Workstation User s Manual Now sold under the Thermo Scientific brand Thermo SCIENTIFIC Part of Thermo Fisher Scientific Document No 065296 Revision 01 January 2009 2009 by Dionex Corporation All rights reserved worldwide Printed in the United States of America This publication is protected by federal copyright law No part of this publication may be copied or distributed transmitted transcribed stored in a retrieval system or transmitted into any human or computer language in any form or by any means electronic mechanical magnetic manual or otherwise or disclosed to third parties without the express written permission of Dionex Corporation 1228 Titan Way Sunnyvale California 94088 3603 U S A DISCLAIMER OF WARRANTY AND LIMITED WARRANTY THIS PUBLICATION IS PROVIDED AS IS WITHOUT WARRANTY OF ANY KIND DIONEX CORPORATION DOES NOT WARRANT GUARANTEE OR MAKE ANY EXPRESS OR IMPLIED REPRESENTATIONS REGARDING THE USE OR THE RESULTS OF THE USE OF THIS PUBLICATION IN TERMS OF CORRECTNESS ACCURACY RELIABILITY CURRENTNESS OR OTHERWISE FURTHER DIONEX CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION AND TO MAKE CHANGES FROM TIME TO TIME IN THE CONTENT HEREINOF WITHOUT OBLIGATION OF DIONEX CORPORATION TO NOTIFY ANY PERSON OR ORGANIZATION OF SUCH REVISION OR CHANGES TRADEMARKS Auto Trace is a registered trademark of Dionex Corporation Microsoft Windows 20
3. 61 Syringes Adjust Air Syringe 61 Syringes Adjust Liquid Syringe 61 Valves Check 12 Port Valve 61 Valves Purge Solvents 61 Dionex Technical Support Contacting 3 Downloading Diagnostic Methods 115 Downloading Utility Methods 66 Dry with Gas Diagram 51 Dry with Gas Flow Chart 50 E EO DUON ARE BAK Oe OE GG 78 Doc 065296 01 1 09 Index 168 Electrical Specifications 160 Elute to Collect Air Push Diagram b57 Air Push Flow Chart 56 Liquid Handling and Air Syringes Fill BELA PAR AA 63 Liquid Handling and Air Syringes Fill Flow Chart 0 52 Liquid Handling Syringe Dispenses Solvent Diagram 55 Liquid Handling Syringe Dispenses Solvent Flow Chart 54 Elution Rack 31 Elution Station 28 31 Elution Station Not in Correct Position 124 Elution Volumes Maximum 75 Environmental Specifications 12 EMO 000065 a pa KAPA seed DIANNA 125 ERROR Light 29 Error Light On During Method 118 Error Light Response 106 Error Messages 113 Example of a Method 91 Exhaust Fan On 74 Exhaust Hose Connection 19 Exhaust Port 32 F File Menu ESE SEE EES se 59 Database 59 DIE UA een es 59 Language 59
4. Regulator P Gas Nitrogen Manifold 12 Port Valve Air Ven Solvent 1 Solvent 2 Solvent 3 Solvent 4 Solvent 5 Handling meee Syringe Figure 35 Dry with Gas Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Doc 065296 01 1 09 Overview 52 Liquid handling syringe fills with elution solvent See Figure 37 Figure 36 Elute to Collect Liquid Handling and Air Syringes Fill Flow Chart AutoTrace SPE Workstation User s Manual Overview 53 ma Solvent Cg Ai Gas Q N 1 Switching O 1 Incoming Sample L 1 Aqueous J Waste Solvent Collect Waste Regulator I Nitrogen Manifold 12 Port J Air Valve 4 N Ven ar Volume according pd h to internal setting Volume according to solvent volume for elution step Solvent 1 nn Paget Solvent 2 x mm Sovent 4 Air Ee Liquid Solvent 5 Handling Waste Syringe Figure 37 Elute to Collect Liquid Handling and Air Syringes Fill Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 54 Elution solvent is dispensed See Figure 39 Figure 38 Elute to Collect Liquid Handling Syringe Dispenses Solvent Flow Chart Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 55 ME Solvent Air a ee v A y A CA y A SPE Hehi Column 1 E i Switching i Valve 1 Incoming AAN Sample IN N AI A L 1 A Collect A A Regulator i Nitrogen Manifold F A 12 Port
5. Valve 1 Incoming E Sample ys 1 Aqueous Waste Regulator Gas Nitrogen Manifold 12 Port Valve Air Vent Solvent 1 Solvent 2 Solvent 3 Air Sclvent 5 Handling Waste Syringe Figure 27 Load Sample Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 44 Liquid handling syringe fills with rinse solvent See Figure 29 Figure 28 Column Rinse Liquid Handling and Air Syringes Fill Flow Chart Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 45 ME Solvent EE Ai Sample Pum Gas SPE Col 1 aa Switching CO id Incoming Sample 1 Aqueous oo ace Solvent Collect Waste Regulator Gas S Nitrogen Manifold 12 Port Air o Vent K a A A Volume according M LI to internal setting Volume according E to solvent volume 1 for rinse step siere SEE AA Air Syringe Liquid Solvent 3 Handling Waste Syringe Figure 29 Column Rinse Liquid Handling and Air Syringes Fill Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 46 Continued 12 port valve switches to the switching valve Liquid handling syringe dispenses rinse solvent See Figure 31 Figure 30 Column Rinse Liquid Handling Syringe Dispenses Solvent Flow Chart Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 47 ME Solvent EE Air Gas SPE A varie i Switching
6. Overlap Horizontal Stack and overlap the windows horizontally Overlap Vertical Stack and overlap the windows vertically Arrange Icons lf any windows are minimized use Arrange Icons to arrange the icons neatly at the bottom of the main window The Help menu contains the options shown in Figure 53 Contents About Figure 53 Help Menu Contents Shows the Help contents and the index While working with the program open the Help window by pressing the F1 key About Opens the About window which contains additional information about the AutoTrace system Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 66 Running AutoTrace Utility Methods A number of utility methods are provided by the AutoTrace software These utilities are used for e Purging the AutoTrace solvent lines e Setting the AutoTrace date and time e Testing general AutoTrace operation e Calibrating the AutoTrace sample pumps To run a utility method 1 From the AutoTrace main menu choose Serial OP Download Utility Procedure 2 Click one of the four buttons see Figure 54 to select an Auto Trace utility W Download Utility Method iPilurge Solvents _B Jenchmark Test _C alibrate Pump Slet Date and Time Figure 54 Download Utility Method Window 3 The selected utility will be downloaded to the AutoTrace Press the CONT button twice slowly on the AutoTrace to run the utility Allow at least 2 se
7. see ee ee ee RR RE ee ee ea ee ee ee 132 PANS se ESE ES EG Ee Aedes GE EG N ee ee a a EE 132 Center the Syringe Plunger ese ee ee Ee a 132 Remove the Defective Svingeri ee Ee a 133 Mount the New SYriNGe sesse se Ee Re ER Ee Re ee Ee Re Ee Ee Ee ee ee ee ee Ee ee ee ee eke 134 Adjust tie NEW SYHNJE SEE RE He GO GE EE EE De Ge SG GE 134 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Table of Contents 10 Replacing FUSES ED EE AA AN 137 Pars and Tools si T AA AD Ee Eg ed GE Pe EE RS GE 137 Remove the Fuse Block Assembly eis se ee Ee Ee RR ER RE ER EE ER Ee Re ER RE Ee ee ee 137 Replace Me Flusel s maa aaa haaa 138 Calibrating Sample PUMPS iese see see ee ee ER EA ee ee Re ee ee ee ee ee Re ee ee ee Re ee ee ee ee 139 Paris aid Tools ws ER EE EG E DE GE 139 Calibration Method ses EE NES a ee OE ER AE ee e ee RD EE week 139 Sea a AN sd ED Se EG ee GO EE De ae Ge OG ER SE EE AD 141 MA IE EE EE ON OE EE HT DES 141 RUNNING the Benchmark Test ESE VR RS Ee DE Ge de ee 141 Column Holder ConversiON sesse R EER EER KERKE RR ER REK EER KERKE RR EER EER EER KERKE KERR Ee 143 Paka EE N E ER ee AA ANA AALAGA 143 Remove the Plunger Assembly sesse aa 143 Install the New Plunger Assembly 0 107 ER Ee Ee ER Ee ee Ee ER Ee Ee ee ee ee ee 144 Changing Between Column and Disk Version seke RR RE RR E RR EER KERKE RE RR EER Ee 146 Procedure SCOPE is bf AGA ANA ES DR AE EE Pe 146 TOO
8. 2 Release the column or disk holders from the fully down position by squeezing the holder s lever and clipping them together as shown in Figure 66 a Lever Clip Figure 66 Column Holder Side View Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 105 Aborting Continued WARNING A Never leave the column or disk holders in the down position without the columns or disks in place because this can deform the O ring 3 Turn the power on Columns Leaking If liquid is leaking through the O ring of the column holder fix the leak as follows 1 Interrupt operation for that sample by releasing the column holder refer to the Aborting method This will turn off the sample pump 2 Create a seal around the O ring by using an up and down motion to lift up and reseat the holder 3 The workstation will resume operation on that sample when the lever is pushed back into the down position and the holder s LED comes on NOTE A small loss of sample will result when step 3 is performed Observe Operation While the workstation runs the method for the first few times observe operation and make note of any procedural changes that are desired for example changing flow rates or volumes The need for changes may not be evident until the examination of the recovery data for the sample run If necessary refer to Application Tips on page 93 Doc 065296 01 1 09 AutoTrace SPE Workstati
9. Solid Phase Elute Commands Continued Pause To add a pause in workstation operation select either a timed delay step in minutes or a pause and alert step that signals the operator until the CONT button is pressed Examples PAUSE AND ALERT Use this step to alert the operator for sample container introduction when the workstation is done with the column conditioning This is useful when a sample contains volatile compounds TIMED PAUSE After conditioning this step introduces a time delay to increase contact time between solvent and column packing material Clean Sample Path Use this selection at the beginning of the SPE method at the end of the SPE method or in a method of its own to flush and prime the sample lines and pumps between sample batches Specify a volume and an effluent waste position of either aqueous waste or solvent waste NOTES UH e The CLEAN SAMPLE PATH step should be selected at least twice When the first CLEAN SAMPLE PATH step runs the workstation pauses to place the sample lines into a beaker containing the elution volume The workstation then pauses again to place the lines into a beaker of water when the second CLEAN SAMPLE PATH step runs e Itis advisable to use CLEAN SAMPLE PATH steps in a separate method that is run between sample batches and at the end of a day See Creating a Method to Clean the Sample Lines with Solvent and DI Water on page 68 If you prefer use the
10. dy CONT Button anaana 29 101 Contacting Dionex 3 Continuing Operation 104 Creating a Method Application Tips 93 Manual Steps 90 Method Example 91 Method Step Considerations 95 Method Steps 95 Sample Recovery Optimization 93 AutoTrace SPE Workstation User s Manual Setup Methods Window 76 77 Setup Parameters 94 Solid Phase Elute Commands 85 Solid Phase Extract Commands 80 Cross Contamination Troubleshooting 123 D Daily Cleanup 110 Daily Operation Checklist 112 Data Menu SEE 63 Name Solvents 63 Setup Commands 63 Setup Parameters 63 Setup User Data 64 Date and Time Settings 67 Default Parameter and Solvent Entries 69 Default Setup Parameter Entries 70 Default Solvent Names 70 Delete Button 78 Detecting Errors 106 Diagnosing Problems AutoTrace Diagnostics 114 Diagnostic List 114 Error Messages 113 Front Panel Error Messages 113 Initialization 115 Replacing Parts 116 Syringes 114 Troubleshooting 116 VAIVES 24s Ghee KAMAG E 114 Diagnostic List 114 Diagnostics Menu 61 Initialization
11. 76 77 Setup Parameters 94 Solid Phase Elute Commands 85 Solid Phase Extract Commands 80 Wrong Liquid Volumes Delivered 120 Wrong Solvent Dispensed 119 Wrong Volume from Sample Container 121 123 Doc 065296 01 1 09 Index 172 AutoTrace SPE Workstation User s Manual
12. ES SS Se 68 Cleaning the AutoTrace Workstation 126 Clicking Sound from Syringe 119 Close Button 78 Collection Container Racks Specifications 161 Doc 065296 01 1 09 Index 167 Column Holder Conversion New Plunger Assembly Installation 144 Plunger Assembly Removal 143 Column Holder LED NotLit 122 Column Holders 28 Column Rinse Air Push Diagram 49 Air Push Flow Chart 48 Liquid Handling and Air Syringes Fill Diagram 444 4686 HAAR AE hi ods 45 Liquid Handling and Air Syringes Fill Flow Chart 0 44 Liquid Handling Syringe Dispenses Solvent Diagram 47 Column Rinse Liquid Handling Syringe Dispenses Solvent Flow Chart 46 Columns Leaking 105 Communications Port 32 Compression Screws Check 22 Computer 008 118 Computer Access 23 Computer Specifications 23 Condition Column Air Push Flow Chart 39 Air Push with Air Factor of 0 5 Diagram 0 00 eee 41 Air Push with Air Factor of 1 0 Diagram 40 Liquid Handling amp Air Syringes Fill Diagram 36 Liquid Handling amp Air Syringes Fill Flow Chart 0 35 Liquid Syringe Dispenses Solvent Diagram 38 Liquid Syringe Dispenses Solvent Flow Chart
13. Plunger Assembly Figure 77 Tubing Clamp Movement 2 Grasp the bottom of the Teflon tubing and carefully pull it upward until it slides off the top end of the stainless tubing 3 Unscrew the plunger assembly see Figure 77 and pull it down to remove it from the column holder Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Column Holder Conversion 144 Remove the Plunger Assembly Continued 4 Set the plunger assembly aside 5 Repeat steps 1 through 4 for each column holder you need to convert Install the New Plunger Assembly Follow these steps to install the new plunger assembly for each column holder to be converted 1 Screw the new plunger assembly into position on the column holder 2 Carefully without developing kinks in the tubing push the Teflon tubing end downward over the top of the stainless tubing as shown in Figure 78 L Teflon Tubing Push tubing down Stainless Tubing Figure 78 Teflon Tubing Installation 3 Now push the tubing clamp down until it is positioned as shown in Figure 79 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Column Holder Conversion 145 Install the New Plunger Assembly Continued Push clamp down Figure 79 Tubing Clamp Positioning Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Changing Between Column and Disk Versions 146 Changing Between Column and Disk Versions Procedure Scope This procedure describ
14. Refer to Ordering Supplies on page 163 for ordering information 1d Fluid path blocked at 1d Inspect the fluid path and valve SPE column or correct the problem tubing 2 Incorrect solvent 2 Solvent lines placed in 2 Reinsert solvent lines into dispensed wrong reservoirs appropriate reservoirs and purge lines 3 Syringe stalls 3a Flow rate is too high 3a Adjust the flow rate 3b Bad SPE column 3b Replace the SPE column 3c 12 port valve problem 3c Run the CHECK 12 PORT VALVE diagnostic Refer to Diagnostics Menu on page 61 and the online Help Do not run the diagnostic until all solvent lines have been purged If the problem continues contact Dionex Technical Support 4 Valves leak 4a Flow rate is too high 4a Adjust the flow rate 4b Valve fitting loose 4b Tighten the valve fitting Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Diagnose Problems 120 Table 16 Liduid Handling Continued 5 Liquid volumes delivered are incorrect 5a Flow rates are too high Causing gas bubbles to form 5b Restricted or leaking solvent inlet tubing 5c Solvent outgassing 5f Syringe leaking 5g 12 port valve is partially blocked or out of alignment 5h Steps using immiscible solvents 5a Reduce the flow rates 5b Inspect for kinks or cracks in the tubing If necessary replace the tubing Refer to Ordering Supplies on page 163 for ord
15. Remove the two top screws from the static strap The static strap is on the back side of the column holder Remove the two Phillips screws from the front of the workstation and remove the holder AutoTrace SPE Workstation User s Manual Changing Between Column and Disk Versions 148 Install the New Column or Disk Holder 1 Insert the column or disk holder into the workstation and secure it in place with the two Phillips screws previously removed Carefully without developing kinks in the tubing push the Teflon tubing end downward over the top of the stainless tubing until there is a 1 8 inch gap between the bottom of the tubing and the top of the slider Now push the tubing clamp down until it is positioned as shown Connect the tubing to the lower end of the holder by finger tightening the compression screw in place Replace the two screws on the static strap Plug the two new holders connectors into the appropriate receptacles on the AutoTrace Column Interface board Secure the wires to the back of the workstation using the supplied cable attachments Changing the Sample Pump Prior to removing the pump follow the steps below to create and run a procedure that will dry the line that runs from the pump to the switching valve This prevents leaking during the replacement 1 2 N OO no A oO Co Doc 065296 01 1 09 Open the AutoTrace software Log in to the AutoTrace software Click the Methods button
16. Valve 1 A Incoming ma YE Sample a aS 1 Aqueous i Waste or Solvent Waste A A Regulator N 15 Nitrogen Manifold i 12 Port i Solvent 1 Solvent 2 Solvent 3 Solvent 4 BAN PO Air Syringe Liquid Handling Syringe Solvent 5 Waste Figure 31 Column Rinse Liquid Handling Syringe Dispenses Solvent Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Doc 065296 01 1 09 Overview 48 Air Push rinses flow path and column See Figure 33 Figure 32 Column Rinse Air Push Flow Chart AutoTrace SPE Workstation User s Manual Overview 49 CO A r l Gas SPE Column 1 Switching Valve 1 ak Incoming Sample s EER i 1 Aqueous Waste or Solvent Waste f J Regulator Nitrogen Manifold N 12 Port Valve o BEBE Solvent 1 sigang maan Solvent 2 eet SESE Wen Air Syringe Liquid Solvent 5 Handling Waste Syringe Figure 33 Column Rinse Air Push Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Overview 50 Switching valve selects gas port Gas flows through column to dry See Figure 35 Continued Ui Figure 34 Dry with Gas Flow Chart Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 51 Gas lt lt lt BD co SPE i A olumn 1 7 A i i Switching Valve 1 7 A ad Incoming Sample S j 1 Aqueous Waste or Solvent A Waste _____Ih
17. and specify the name of the solvents used in your method Up to 15 characters are allowed for each solvent name NOTE Type Not Used for any unused solvent port Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 76 Change Solvent Names Continued 3 Click the Save button 4 To delete a complete solvent set click the Delete button Writing a Method Choose Methods from the main menu to manage the methods The Setup Methods window opens as shown in Figure 58 1 Setup Methods NE EE EE Params Print Help Close PESM new AT 500 ml Solid phase extract Samples 6 Condition column Load sample Wash syringe Pause and Alert Min Timed Pause Column rinse Wash syringe Dry with gas Clean sample path Solid phase elute Elute to soak Elute to collect Elute to soak nd tube Elute to collect nd tube Pause and Alert Autotrace method steps Name Solvent Set Standard Volume Solvent 1 f Solvent 2 f Solvent 3 f Solvent 4 C Solvent 5 Estimated time 1h 21min bethodoo TOO Timed Pause Clean sample path Rinse sample container Concentrate sample Wash syringe End step Mo User logged on Doc 065296 End No 6 Dip Column with gas for 300 mintes DD NB Soek and Colect 20m Fraction usngAceton 9 Colect 2 0 mi Fraction into sample tube using Aceton E OB led Ek Figure 58 Setup Methods Window The last method opened displays in the Setup Metho
18. on page 68 This utility checks the operation of the workstation front panel elution station syringes pumps and valves and is described in detail at the end of this section Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 128 Replacing and Adjusting the Liquid Handling Syringe This section explains how to replace and adjust the 10 mL liquid handling syringe Parts The following item is required to complete this method e 10 mL replacement syringe Purge the Solvent Lines Follow these steps to purge the liquid handling syringe and its tubing 1 Download a Purge Solvents procedure as described in Purging the Solvent Lines Utility on page 66 2 Remove the solvent lines from their reservoirs 3 Run the purge method to air purge the liquid handling syringe and its tubing Center the Syringe Plunger Follow these steps to center the syringe plunger and prepare the syringe for removal in the next method 1 Run the Diagnostics menu option and download an Adjust Liquid Syringe diagnostic as described in AutoTrace Diagnostics on page 114 2 Press the CONT button twice slowly Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 129 Remove the Defective Syringe To remove the defective syringe 1 Remove the two screws from the mounting bracket that secure the syringe to the housing as shown in Figure 69 Stainless Steel Tubing Black Mounting Bra
19. set of 6 071082 Sample Pump Replacement Kit cartridge model 071083 Sample Pump Replacement Kit disk model 071084 Switching Valve Replacement Kit 071087 Teflon Tubing Kit all tubing other than sample and 071088 waste Waste Tubing Kit 071089 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Glossary 165 Glossary Table 22 lists the glossary terms and definitions Table 22 Glossary Terms Air Factor The adjustable factor that determines the distance liquid is pushed beyond the 12 port valve and switching valves The air push factor is used in solvent conditioning and elute to soak steps and pushes the liquid partially through the column path so that the column bed is not dried out The number from 0 3 to 5 increases or decreases the standard 1 2 mL amount of air that follows the liquid being sent through the solid phase extraction column by a factor of 0 3 to 5 times If volumes of greater than 5 mL are required the dry with gas step in Creating a Method to Clean the Sample Lines with Solvent and DI Water is recommended Air Push A flow of air generated by the air syringe that clears liquid from the liquid handling syringe and tubing lines after conditioning rinsing eluting and syringe washing steps AT A program that runs the AutoTrace menu software in the computer allowing the download setup and writing of AutoTrace methods This program also runs the diagnostic software that supplies
20. 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 20 Connect the Gas Supply To connect the gas supply to the workstation s gas inlet 1 Locate the 10 ft 3 m length of 1 8 inch ID x 3 16 inch OD tubing pieces and the 1 8 inch Quick disconnect fitting in the Startup Kit Push the barbed end of the fitting into one end of the tubing as shown in Figure 10 ty Figure 10 Barbed Fitting on Tubing 2 Connect the open end of the Quick disconnect fitting see Figure 11 to the gas inlet on the lower left side of the workstation see Figure 12 e Ja Figure 11 uick Disconnect Fitting Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 21 Connect the Gas Supply Continued Gas Inlet Figure 12 Gas Inlet 3 Using the supplied 14 inch NPT x 1 8 inch barb fitting connect the other end of the tubing to the gas supply 4 Turn on the gas supply The gas supply must be clean and filtered with an incoming pressure of no more than 100 psi 6 9 bars 5 Before operating the AutoTrace Workstation you need to set the workstation pressure to 10 psi 0 7 bars Refer to Operation on page 97 for instructions Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 22 Check the Compression Screws To check the tightness of the workstation s compression screws 1 Open the worksta
21. 8 Air ek RE LT Vent M N i Solvent 1 pins Solvent 2 a Solvent 4 Air Syringe Liquid Solvent 5 Handling Waste Syringe Figure 39 Elute to Collect Liquid Handling Syringe Dispenses Solvent Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Doc 065296 01 1 09 Overview 56 Air push rinses flow path and eluent goes to collection container See Figure 41 Figure 40 Elute to Collect Air Push Flow Chart AutoTrace SPE Workstation User s Manual Doc 065296 01 1 09 Overview 57 a Air Gas y N V A SPE Y j Oo Column 1 Vy A Switching 7 i Valve 1 Incoming bo La Sample s on 1 Collect Regulator C Nitrogen Manifold Air Solvent 1 is Solvent 2 Magi HERE Solvent 3 l ma olven Air Syringe Liquid Handling Syringe Figure 41 Elute to Collect Air Push Diagram Solvent 5 Waste AutoTrace SPE Workstation User s Manual Software 58 Software This section of the manual describes how to use the software supplied with the AutoTrace SPE workstation provides a method example and lists some application tips Once you install the AutoTrace software follow these general steps to automate a method 1 Open the AutoTrace AT software Specify the parameter and solvent information Write a method Save the method Download the method to the AutoTrace unit oOo a A Q N Print the method Us
22. Button Used to stop the workstation after it completes the step it is performing CONT Button By pressing CONT twice slowly downloads a method from the PC Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 30 Workstation Diagram Left Side View 00 EO Figure 15 Left Side View Parts and Functions Left Side View i Ports Behind door not shown Input ports for Ko solvents Waste Port Behind door not shown Output port for system waste from purging solvent lines and or washing the liquid handling syringe Gas Inlet Input for the clean gas supply Air Syringe Draws in and delivers air that follows sample or solvent transfer to assure transfer is complete Liquid Handling Draws in and dispenses solvent through Syringe the workstation Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 31 Gas Regulator Regulates gas pressure in the workstation Knob that is used for the drying column and sample concentration 7 Gas Pressure Indicates the gas pressure set by the Gauge knob Elution Rack Holds tubes or vials for collection of eluent Elution Station Collects effluent to one of two waste positions or collects eluent into collection container by moving into the appropriate position 10 12 Port Valve Controls the flow of air solvent and waste whatever is specified by the method step ia Valves Directs the flow of gas solvent or sample to the colum
23. Cleanup If the solvent used in step 3 is immiscible in water When the workstation pauses the second time remove the sample lines and insert them into a clean container filled with an intermediate solvent Press the CONT button when ready Otherwise skip to step 5 When the workstation pauses the last time remove the sample lines and insert them into a clean container filled with deionized water Press the CONT button when ready When done using the workstation for the day Empty the waste reservoirs Flush the solvent lines Flush the sample lines Flushing the Solvent Lines When using samples that tend to crystallize or corrosive solvents that could attack valves or other AutoTrace parts over time flush the solvent and sample lines with water or an inert soluble solution whenever the workstation will not be processing samples To flush the solvent lines 1 Doc 065296 01 1 09 Fill the solvent reservoirs with the solvent of choice for flushing and fully submerge the tubing Swirl the solvent in the containers to rinse the outside surface of the tubing and weights Download the method created in either Purging the Solvent Lines Utility on page 66 or Customizing a Method to Purge Less than Five Solvent Lines on page 67 and press the CONT button twice slowly When the workstation pauses press the CONT button AutoTrace SPE Workstation User s Manual Operation 111 Flushing the Sample Lines To flus
24. Dionex Auto Trace SPE Workstation you must modify the following entries Database_Data C lt D IREC TORY_NAME gt ATDATA MDB Data_Dir C lt DIREC TORY_NAME gt where DIRECTORY NAME identifies the directory where the files reside Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 26 Overview This section provides a general description of the workstation capabilities parts and functions and liquid flow Description The Auto Trace SPE Workstation performs large volume solid phase extraction using a variety of manufacturers 1 mL 3 mL 6 mL or glass 6 or 8 mL syringe type SPE columns or 47 mm disks Automate the method by using the workstation to e Condition the column or disk e Load sample onto the column or disk e Rinse the column or disk e Dry the column or disk e Elute the sample Menu Software Easy to use software is provided with the workstation for setting the operational parameters and writing the specific method steps that automate the method Descriptions of the parts of the software are provided in Software on page 58 The software includes diagnostic methods run on the workstation to assist in maintaining optimal performance More details on diagnostics are provided in Diagnose Problems on page 113 Solvent Selection When writing an AutoTrace method using the menu software up to five solvents may be designated for the liquid sequences used in column preconditio
25. Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 131 Adjust the New Syringe Continued 2 Doc 065296 01 1 09 Turn the thumbscrew to the left until the knurled thumbscrew moves to its upper limit of travel Loosen the white compression screw at the top of the syringe one to two turns Press the CONT button twice quickly to rerun the ADJUST LIQUID SYRINGE diagnostic As the plunger moves up you should hear a clicking sound Turn the thumbwheel to the right until the clicking just stops Then turn it one more partial turn as shown in Figure 71 Top View Turn thumbwheel one more partial turn to the Thumbwheel right by the amount shown Figure 71 Thumbwheel Rotation Tighten the knurled thumbscrew to secure the position Slide the stainless tubing down into the syringe as far as it will go Press the CONT button twice to rerun the diagnostic Check that as the plunger moves to the top it moves the stainless tubing to the correct height After the plunger has pushed the stainless tubing to the correct height tighten the white compression screw AutoTrace SPE Workstation User s Manual Maintenance 132 Replacing and Adjusting the Air Syringe This section explains how to replace and adjust the 10 mL air syringe Parts The following item is required to complete this method e 10 mL replacement syringe Center the Syringe Plunger Follow these steps to center
26. File Download Terminated Repeat the download and let all the download windows close automatically 4096 INI File Not Found Close the software and verify that the AT INI file exists in the directory 4100 COM port not set in INI file Close the software and verify that the COM port is set in the AT INI file 16385 Port Control Error Check COM port communications 16896 No Response time out Check the connection with the AutoTrace and verify that the correct COM port is set in the AT INI file Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 126 Maintenance This section of the manual describes how to maintain adjust and replace components in the AutoTrace SPE Workstation including e Routine Maintenance e Replacing and Adjusting the Liquid Handling Syringe e Replacing and Adjusting the Air Syringe e Replacing Fuses e Calibrating Sample Pumps e Running the Benchmark Test Establish an appropriate schedule for performing routine maintenance according to how often the workstation is run Perform any of the other methods indicated by the solution steps in Troubleshooting on page 116 In order to test adjust or replace components other than what is covered in this section run the diagnostics Information on running the diagnostics can be found in Diagnose Problems on page 113 Also refer to the detailed instructions that come with the AutoTrace Replacement Kits Refer to Ordering
27. Flashing 117 Ready Light NotLit 117 Recalling Default Entries 70 Removing Cover Fuse Block 156 Removing Defective Air Syringe 133 Removing Defective Liquid Handling SYFINGE ssc cee ee enw ee wees 129 Removing the Fuse Block Assembly 137 Removing Used Columns 108 Replacing Air Syringes 132 Doc 065296 01 1 09 Index 170 Replacing Fuses 137 138 Replacing Liquid Handling Syringes 128 Replacing Parts 116 Required Installation Tools 12 Right Side View Ji Routine Maintenance 126 RUN Light 0 29 Run Light Not Lit after Loading 117 Running an SPE method 101 Running the AT Program 58 Running the Benchmark Utility 141 S Sample Input Lines 32 Sample Pump Calibration 139 Sample Pump Fails to Start 123 Sample Pump Specifications 161 Sample Pumps 28 Sample Recovery Optimization 93 Sample Run Completion 106 Save Button 0 78 Serial Number 11 Setting Date and Time 67 Setup Methods Window 76 77 Close Button 78 Delete Button 78 Edit Button 78 Help Button 78 Load Button 77 New Button 77 Params Button 78 Print
28. Ve EE sd 12 Prepare the Work AGAS ED AE aa ee ee se ee ke eo 12 Connect the Solvent Reservoirs se se ee aaa 13 Install the Waste Drain and Tubing 1 11 71 2 Ee ER ER Ee ee Ee ee Ee ER ee Ee ee ee ee ee ee ee 16 Gone the Exhaust OSC oe EN ED Do a DoE ee 19 Connect Ie Gas SUDD V ass ED EE ER ER DE GE ee GE ee 20 Check the Gompression SCheWwS EER Be EDE GR RR EER ee Ge DES Gee ea ee 22 POWER Up TMG WorkstallOm ses DEE EA EE ee ie ee N 23 O ACCESS AA 23 s0fWware instalati Orgran Ge EE AG N DE Ee a 24 INEE le EE GE ED EE E DE E GE DE EE ie 25 OVS EO ie ERGER AA AA DO GE oa We Be DE ASe eel 26 LE GUID NOM aaa aa aaa Er AA 26 MENU ON NAE ka ANG EE GE GE AN De GR DE N ER EG De kAkAt 26 DOVER AIN ses RE ER ER EE ER GE DA N EE EE DR SEE Ee 26 Flow hate COMMON ROES EDE GE EE EG ED ED ans SD GE EP Dee 26 standard OOS AOMS Es ER EE ED ee SR ee EE GE se DE eo EE 27 pional Operations EE a bas N ccs AA ea ice 27 Workstation Diagram Front VIEW sesse sesse se ee Ee Ee Re Ee Re Ee ee ER Ee ee Ee Re Ee ee ER Ee ee ee Ee 28 Parts and Functions Front VIEW ese sesse ee ee se Ee Ee Ee Ee Ee ER Ee Ee ER Re Ee Ee Ee ee ee ee Ee ee 28 Workstation Diagram Left Side VIEW iese ee ee aa 30 Parts and Functions Left Side VIEW ee ee Ee Ee ER ER Ee ER ER ee ee ee Ee ee ee 30 Workstation Diagram Right Side VieW ee ee ee Ee ER ER ER aa 32 Parts and Functions Right Side VieW ee ee ee Ee Ee Ee Ee Ee ER ER ee ee ee ee ee 3
29. Workstation User s Manual Software 73 Changing Setup Continued Table 3 Flow Rate Definitions Cond Flow Flow rate at which the syringe will 0 6 to 40 0 mL min push conditioning solvent through the column Load Flow Flow rate at which the pump will 1 0 to 30 0 mL min push sample through the column Cartridge version 2 0 to 60 0 mL min version Rinse Flow Flow rate at which the syringe will 0 6 to 40 0 mL min push rinse solvent through the column Elute Flow Flow rate at which the syringe will 0 6 to 40 0 mL min push elution solvent through the column 2 Cond Air Push Flow rate when the air syringe clears 0 6 to 40 0 mL min liquid from the syringe and tubing after a conditioning step Rinse Air Push Flow rate when the air syringe clears 0 6 to 40 0 mL min liquid from the syringe and tubing after a column rinse step Elute Air Push Flow rate when the air syringe clears 0 6 to 40 0 mL min liquid from the syringe and tubing after an elution step Push Delay Time delay after liquid is pushed into 0 to 999 seconds the column path before the next operation begins It allows time for pressure in the column to dissipate a If any flow rate is set too high excessive pressure will result and the syringe may stall b Most applications show higher recoveries at slower flow rates c Air Pushes are used to evacuate the lines and ensure solvent delivery d Air Push rates should initially be se
30. be changed For details refer to the New function description Save Save data being changed after the New or Edit functions Undo Recall the last entries before starting edit mode Delete Delete a method Before deleting you are asked if you want to delete the method After deleting the method the method is obsolete and cannot be recalled Params Change the setup parameters of the method Each method has its own set of parameters Parameters are initially set at default values For more details refer to Changing Setup on page 72 Print Print the method The printout includes e The AutoTrace SPE software version and the method title e A listing of the method steps e A record of the setup parameters Help Press the F1 key to open the Help window Close Close the Setup Methods window Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 79 Writing a Method Continued Adding a Method Step To add a new method step 1 Inthe AutoTrace commands list on the left side of the Setup Methods window double click a step under either the Solid Phase Extract or Solid Phase Elute heading The step will be inserted in the line below the arrow 2 Specify the volume or time in the box above the method steps 3 If applicable choose a waste position 4 If applicable choose a solvent Deleting a Method Step Double click the method step to be deleted in the list of method steps on the right side
31. diagnostic method Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Voltage Conversion 155 Voltage Conversion This section of the manual describes how to set up the AutoTrace Workstation s power entry port to correspond with the AC power source The Auto Trace Workstation comes factory configured for 120V AC NOTE Follow these steps only to convert the workstation s voltage selection to a new voltage Power Entry Port The power entry port contains a fuse holder compatible with dual 220 240V fuses or a single 100 120V fuse A voltage selector is also present that allows the voltage to be set to one of four configurations 100 120 230 or 240 volts Parts and Tools The following parts and tools are required to complete this procedure e Small flat blade screwdriver e Small Phillips screwdriver e Needle nose pliers e Two 1 6A 220 240V fuses or one 3A 100 120V fuse Refer to Figure 87 as required Power Entry we Housing Voltage Selector lt Card Fuse Block Assembly Figure 87 Fuse Block Assembly Removal Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Voltage Conversion 156 Remove the Fuse Block Assembly Follow these steps to remove the fuse block assembly NOTE Turn off the Auto Trace power and unplug the AC power cord before beginning this procedure 1 Turn the workstation s power off and unplug the AC power cord 2 Using the small screwdriver place the screwdr
32. example specify 1050 mL instead of 1000 mL 7b Sample pump is out of 7b Perform CLEAN calibration SAMPLE PATH with deionized water and then run the CALIBRATE PUMP utility as described in Calibrating Sample Pumps on page 139 7c Fittings are loose atthe 7c Tighten the fittings sample pump 8 Uneven volumesin 8 Loose fitting at 12 port 8 Check the tightness of the elution containers For valve or switching valve fittings example 10 mL is expected and one container has 8 mL while the other has 12 mL Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Diagnose Problems 122 Solid Phase Extraction Troubleshooting Table 17 Solid Phase Extraction Symptom Probable Cause Solution 1 LED on column or 1a Column or disk deformed 1a Discard and replace the Or size incorrect column or disk disk holder fails to light 1b Defective column or disk 1b Contact Dionex Technical holder Support 1c The column or disk is 1c Install the column or disk missing 2 Leakage around the 2a Packing material debris 2a Clean out the columns or O ring of the column may exist on the inside walls disks before use Refer to or disk holder of the column or disk Cleaning the SPE Columns causing a poor seal in Preparing the AutoTrace SPE Workstation on page 97 2b Dirty O ring 2b Clean the O ring with a wipe and solvent 2c Cracked O ring 2c Replace th
33. local Setup Parameters window Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Changing Setup Software 72 A brief description of each setup parameter is included in e Table 3 Flow Rate Definitions on page 73 e Table 4 SPE Parameters on page 74 e Table 5 Workstation Parameters on page 74 e Table 6 Maximum Elution Volumes on page 75 To change the setup parameters 1 From the AutoTrace main menu choose Data Setup Parameters 2 Click the Edit button The Setup Parameters window opens as shown in Figure 56 Use the arrow keys to move to the field that requires changing and specify the new value The window displays the minimum and maximum values allowed Setup Parameters g Edit Default Print Last Change 2 16 2001 9 05 35 AM Flow Hates Cond Flow 15 0 ml min Load Flow 10 0 mlmin Rinse Flow 90 0 ml min Elute Flow BO ml min Cond Air Push 15 0 ml min Rinze Air Push 20 0 ml min Elute Air Push 3 0 ml min User Dionex logged on re aL Help Close SPE Parameters Push Delay Aur Factor Autowash Wol Workstation Parameters Mas Elution val 12 0 ml Exhaust Fan On i Beeper On lw Figure 56 Setup Parameters Window 3 Click the Save button To recall the default entries click the Default button Values shown in Table 3 are for both the Column and Disk versions of the AutoTrace Workstation unless otherwise specified Doc 065296 01 1 09 AutoTrace SPE
34. needle nose pliers If any of the tubing lengths need to be cut you need wire cutters or scissors Review Specifications Review Specifications on page 160 before you begin the installation Converting Voltages If you need to convert your AutoTrace Workstation s voltage to a voltage other than the factory configured 120 VAC refer to Voltage Conversion on page 155 Prepare the Work Area WARNING A The appliance inlet is the disconnecting device Place the device or equipment in a manner so that the disconnecting device is accessible at all times To prepare the work area for AutoTrace installation 1 Provide a level stable and flat surface with enough room to accommodate the workstation s 23 in 57 cm width 27 in 69 cm height and 25 in 63 5 cm depth 2 Make sure there is enough room for the 12 x 14 in 30 x 36 cm sample rack on the right side of the workstation 3 Provide an additional 2 to 3 sq ft 1 sq meter of space on the left side of the workstation for the solvent reservoirs 4 Provide an environment with the following Operating 50 to 104 F 10 to 40 C Temperature Relative Humidity 20 80 Operating Altitude 200 to 10 000 ft 61 to 3048 meters Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Installation 13 Prepare the Work Area Continued 5 Using at least two people carefully place the workstation on the work area If necessary refer to the unpacking sl
35. of e Solvent for the first step e Intermediate solvent for the second step if necessary e Water for the last step 8 Choose Dry With Gas and specify a time of 0 5 minutes to remove the water from the solvent path This step is very important because it removes the water between the switching valve and the column WARNING AA Only inert gases such as nitrogen argon or compressed air free from oil should be used 9 Click the Save button 10 From the AutoTrace main menu choose Serial OP 5Download Method Specifying Parameter and Solvent Information Specify the parameter and solvent information using the two choices available from the DATA program option Default Entries The two choices from the DATA program option are SETUP PARAMETERS and NAME SOLVENTS beginning with default entries Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 70 Default Setup Parameter Entries If the method does not specify flow rates begin with the default setup parameters Observe workstation operation and examine the recovery data to determine if any modifications need to be made Additional Parameter Information For tips on parameter settings refer to the Help screens by pressing the F1 key Also review the Application Tips on page 93 Default Solvent Names You can choose to keep the default solvent names SOLVENT 1 SOLVENT 2 etc or specify the actual names of the solvents to be used Specif
36. of 0 5 Figure 23 Condition Column Air Push Flow Chart AutoTrace SPE Workstation User s Manual Overview 40 Solvent L Air Pum Gas N Solvent stops here A with 1 0 Air Factor SPE Column 1 A Switching A Valve 1 l a Incoming r ie Sample 1 A A a or Solvent N sole Waste A A Regulator N Nitrogen Manifold 12 Port i Air Valve Vent O ET VV A mad Solvent 1 Solvent 2 ninn er Solvent 3 Air Syringe Liquid Solvent Handling Waste Syringe Figure 24 Condition Column Air Push with Air Factor of 1 0 Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual SPE Overview 41 ME Solvent 711 Air fm ras A Column 1 A Switching N Valve 1 Incoming Sample i 1 Aqueous Waste or Solvent i Waste A Solvent stops here Regulator A Gas Nitrogen Manifold N 12 Port 5 Air Valve f Ventr pasara A oe Solvent 1 Hiss Solvent 2 sens Sinn Solvent 3 Air Syringe Liquid Solvent Handling Waste Syringe Figure 25 Condition Column Air Push with Air Factor of 0 5 Doc 065296 01 1 09 Diagram AutoTrace SPE Workstation User s Manual Doc 065296 01 1 09 Overview 42 Pump turns on and pumps sample through switching valve and onto column See Figure 27 Figure 26 Load Sample Flow Chart AutoTrace SPE Workstation User s Manual Overview 43 WJ Sample Gas SPE Column 1 Switching
37. of the Setup Methods window NOTE The first step Process x samples using and the last step End can t be deleted Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 80 Writing a Method Continued Solid Phase Extract Commands The Solid Phase Extract commands found on the leit side of the Setup Methods window specify the steps prior to sample elution The solid phase extract menu is shown in Figure 60 An example method is provided in Method Example on page 90 NOTE Figure 60 shows commands for the Column version of the Auto Trace Workstation The Disk version of the Auto Trace Workstation will display the word Disk instead of Column Solid phase extract Condition column Load sample Pause and Alert Timed Pause Column rinse Wash syringe Dry with gas Clean sample path Figure 60 Solid Phase Extract Menu Condition Column or Condition Disk To activate the SPE column or disk specify a volume and solvent to be passed through the column or disk with the effluent directed to a solvent or aqueous waste position For more than one solvent repeat this selection as many times as necessary NOTE L After this step is performed a small volume of air affected by the Air Factor parameter setting is used to push solvent past the 12 port and switching valves The air push clears the lines between the switching valve and column or disk of any remaining solvent
38. risk of danger Refer to the user documentation Mm NOTE A cautionary statement an operating tip or maintenance suggestion may result in instrument damage if not followed Hazardous voltage risk of shock injury Crush hazard Risk of body parts hair jewelry or clothing getting caught in a moving part a a Apa A me PO P oa a AE A Lifting hazard May result in injury Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Preface 6 Table 1 Important Symbols Continued Symbol Protective ground symbol Ground symbol Ela od pi Alternating current Off GIE EN CE compliance mark Signifies that the unit has passed safety tests for grounding power line transience and current leakage GE Bl OP Equipment Yellow Caution risk of danger labels are Red Stop color coded Blue Mandatory action Green Safe condition or information Helpful hints additional information Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Table of Contents 7 Table of Contents ed KAC 0 iS N AA ER de De ae DE a De OD ED E OE ie 3 KAHEL AA Eia 11 Paris ESUN ER RS ie ANG ANAN O 11 dale sie las ER OE EE ER ET EE EE EN 11 Record ihe Serial Numbers ER ED SE RR De DE Ee Se ee ER ON Ge Ne ge 11 stallat OVerVle We ER AUN N Ge AA LAG 11 Tools Feduired si ME IE GER ER RE Ee N NR BE RE GE PAGA 12 Review Speeifi ations ED SS ES SE ek a 12 GE onveriind Vollades EES N SG a Ee ie Ep Re ee Oe Ge
39. steps from the method disk as the last steps in the method instead 1 an intermediate solvent is required between the elution solvent and water insert a third CLEAN SAMPLE PATH step using this solvent between these two steps Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 88 Solid Phase Elute Commands Continued WARNING A Do not use acetone as a solvent to clean the sample path because it is harmful to sample pumps Rinse Sample Container To rinse the sample container and elute to one of the three elution stations specify the solvent volume that you will add to the sample container for rinsing and designate the elution station position This step causes the workstation to pause for you to add the solvent and swirl the sample container before it pumps the container s solvent through the column and into the solvent waste aqueous waste or collection containers Concentrate Sample To concentrate the final eluent specify the time in minutes for gas to flow into the collection containers This step causes the workstation to pause for you to replace the SPE columns with empty columns before gas flows into the collection containers Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Software 89 Solid Phase Elute Commands Continued Wash Syringe Whenever the next step requires a solvent different from the previous step perform this operation Specify a solvent and volume to w
40. sure the waste tubing never drops below the level of the waste container cap If you route the water waste tubing to a drain make sure you follow the same tubing guidelines If necessary cut the tubing to the desired length with wire cutters or scissors 7 Locate the tubing port labelled WASTE found directly below the five solvent tubing lines on the left side of the workstation as shown in Figure 8 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 18 Install the Waste Drain and Tubing Continued Waste Port Figure 8 Waste Tubing Port 8 Insert the waste tubing from this port into one of the bottles supplied with the workstation keeping the following in mind a Make sure the end of the tubing extends Just below the top of the container b Avoid sharp turns and uphill pieces of tubing from the workstation to the container Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 19 Connect the Exhaust Hose If the eluted solvents need to be vented use the workstation s internal fan to safely vent solvent vapors To connect the workstation s exhaust hose 1 Connect the exhaust hose to the workstation s exhaust port by sliding and rotating the hose onto the port as shown in Figure 9 4 Exhaust Port Figure 9 Exhaust Port 2 Route the hose to a suitable vent location If necessary use wire cutters or scissors to cut any excess hose as required Doc
41. the Date and Time Utility The AutoTrace clock is factory set at USA Eastern time If your time zone differs save and run this method to reset the real time clock in the workstation as follows 1 Doc 065296 01 1 09 From the AutoTrace main menu choose Serial OP 5Download Utility Procedure Click the Set Date and Time button The system date and time 2 minutes of your computer is written to the AutoTrace Workstation After about one minute a beep signals that the workstation is ready to update its date and time using the values from the method AutoTrace SPE Workstation User s Manual Software 68 Setting the Date and Time Utility Continued 4 Press the CONT button on the workstation s front panel display The workstation s date and time are immediately updated Once set the time is maintained even when power to the workstation is turned off Testing General Operation Benchmark Test Utility 1 From the AutoTrace main menu choose Serial OP Download Utility Procedure 2 Click the Benchmark Test button NOTE Refer to Benchmark Test Utility on page 141 for instructions on how to run this utility Calibrating the Sample Pumps Utility 1 From the AutoTrace main menu choose Serial OP Download Utility Procedure 2 Click the Calibrate Pump button NOTE Ul Refer to Calibrating Sample Pumps on page 139 for instructions on how to run this utility Creating a Method to Clean the Sample L
42. 00 and Windows XP are either registered trademarks or trademarks of Microsoft Corporation in the United States and or other countries Teflon is a registered trademark of E I duPont de Nemours amp Company All other trademarks and registered trademarks are the property of their respective holders PRINTING HISTORY Revision 01 January 2009 Preface 3 Preface Contents The information in this manual may contain typographical errors or technical inaccuracies and is subject to change without notice Modifications may also be made to the product described in this manual at any time Statement of Proper Use The AutoTrace SPE Workstation automates cartridge conditioning rinsing sample addition and the cartridge elution steps of solid phase extraction SPE The workstation processes up to six samples through its unique fluid management system It can be used for all solid phase extraction water methods WARNINGS AA e To reduce the risk of electric shock do not remove the cover No user serviceable parts are inside Refer to qualified service personnel e Use this product only in the manner described in this manual When used in a manner other than specified the safety precautions may be impaired Contact Us lf you have a question about this product that is not answered in this manual or if you need assistance regarding this product please contact Dionex Technical Support In the U S call 1 800 346 6390 Outsi
43. 04 ADORNO n N N ee iS RE AP 104 SOUS ECA NG es ES hala ED DE NG 105 Ae AA 105 Deleng ETOS aa AA AA AA a 106 ENOr LIGNE RESPONS G ie EE NANANA ANG ERA NAAN N bl Di ie DE ee es Ge 106 Flashing Ready Light Response a NAA Ee ed kaaa 106 Sample Bun EO O CALAUAN 106 After Running the Method seip Hah AA AA ee 107 Determine Required ChangeS iese se aka e Ea ANRE ee ee EED 107 Make the Necessary Changes si ss EE RE Ee RR Ee Ee Ee ee Ee ee ee Ee ee ee ee eke 107 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Table of Contents 9 Test lie Changes ER Gavotte EE Ee na 107 Removing Used Columns ESE SEE AA aea DEE OG Ge N 108 Removing sed DISKS ses EE N N Ge Ee ee ee ee ee EE 108 Next Sample Batch Preparation ies ee ee se Ee Ee Ee Ee Ee Ee ER ee ee ee ee ee ee 109 Daly CICANUD EE aa oat a ioe ae oad AA N EE De 110 Flushing he Selventlines is De ahi Naa 110 Flushing the Sample LINES 11111 EE EE EE RE SEKER EE RE ER ER Ne GENE EN Ke Dee GE RE ER GR GE Ne si 111 Method Development Checklist see se Ee R ER ee ee ee ee ee ee ee 111 Speeily YOUN Melhod ss RE ERA RE EA EE ESE EE SI ee Ee Ee 111 Prepare the Works ON ee Ee ANA AA 111 Kuning MEMO ses SE ee SR DE GE de Re OD EO n Ee ma 111 After Running the Methods is EE N N GE Re EG ke ED 111 Daily Operation Checklist iese se Ee ER RR ER Ee ER Ee Ee EER Ee Ee ee ee ee Re Ee Ee ee ee ee ee ee 112 Prepare the Works ON ss EE ie EA ANA NANANA ASA AA 112 RUN COUR Melo
44. 09 AutoTrace SPE Workstation User s Manual Overview 34 Workstation Interconnection Diagram Figure 18 shows a simplified view of the main AutoTrace components and their connections NOTE The dashed box shows the pump switching valve column and sample container for position 1 only Refer to the flow charts and diagrams that follow for details on the SPE process Column SPE jor Disk 1 Switching Valve 1 Incoming Sample HY 1 Aqueous Solvent Collect Waste Waste cv ma EE EE BT To Valves Regulator 2 6 N Nitrogen Manifold 12 Port Air Valve NG nG ki Vent O Solvent 1 Solvent 2 Solvent 3 Solvent 4 Solvent 5 Waste Air Syringe Liquid Handling Syringe Figure 18 Interconnection Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Overview 35 SPE Process The flow charts and associated diagrams that follow show how the Auto Trace Workstation processes a typical SPE method Start SPE method 12 port valve selects one of five solvents Liquid handling and air syringes fill with conditioning solvent See Figure 20 Figure 19 Condition Column Liquid Handling and Air Syringes Fill Flow Chart Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Doc 065296 01 1 09 Overview 36 ME Solvent Ar Pung Gas SPE Column 1 Switching CO a Bra 1 Aqueous Solvent Collect Waste Waste Regula
45. 2 SOWAS Diaan EE EE OS GR Oe es EE ei 33 Software Files and FUNCTIONS ese see ee ee aa 33 Workstation Interconnection Diagram ee see ee ee ER Ee ER ER ER ee Ee ee Ee ee Ee ee ee Ee 34 OPE PI OCOS S ER EA Na ana OG DS EE GE RA GE Ee EE ee na 35 ole HEER AE EE EE aane Ori 58 Using the AutoTrace AT Program esse se see Ee ee a 58 FIS MENU ts cece oie aha AA AA a Aa aka hha EE ee ei 59 IN le SAN AA AA 59 Ciel OO MET ER EE EE EO N EE RE OE ONE 60 DIAGHOSIICS Men ASA SE Ie ANAN ics WE DE Ge 61 LOGIN Logout Men GR ee Navn de be N GED Dk 61 bata Men eo ie Se ie Ee Ee N Ge DE N EG 63 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Table of Contents 8 Windows MENU EES IE ee ed EG ED ee 65 FICID MENU kua GE SE EE ANA AA GE Ee EE Pana ei fe 65 Running AutoTrace Utility Methods a 66 Purging the Solvent Lines Utility aaa 66 Setting the Date and Time UI see a 67 Testing General Operation Benchmark Test Utility 2 QXXX 68 Calibrating the Sample Pumps Utility ee ee ER ER Ee EE ee ee ee ee ee Ee ee 68 Specifying Parameter and Solvent Information eise ese see ee ee Ee Ee ee ee ee ee ee 69 Peiatil EiHIES EER AS AA 69 Default Setup Parameter ENIES urissaan ds kes se ge secede ee ee se Ke Ee AGE GE eke WEE ee 70 Additional Parameter Information ss EER EER ES SE AASA 70 Default Solvent Names ANNA GE ie ee ee ge 70 Recalling Def
46. 5 ABDOU spe ae dws ee KORE Re 65 Contents EES Ese 65 Initialization Problems 115 Installation Compression Screws Check 22 Environmental Specifications 12 Exhaust Hose Connection 19 Gas Supply Connection 20 Overview 2 2 2 2 0000 ee eee 11 Power Up a aes eee ee bw 23 Software 00000 ee 24 Solvent Reservoir Connections 13 Doc 065296 01 1 09 Index 169 HATID Kilns seen SERE aw een eed 20 Tools Required 12 Waste Drain and Tubing 16 Work Area Preparation 12 Interconnection Diagram 34 L Leak Checks 127 Leak on Column Holder O ring 122 Leaking Columns 105 Left Side View 4 30 Liquid Buildup in 10 mL Air Syringe 121 Liquid Handling Syringe 30 Liquid Management Specifications 160 LOAD Button 29 101 Load Button if Load Sample Diagram 43 Load Sample Flow Chart 42 Login Logout Menu 61 Change Password 62 LOGIN g 5 etserkunewavanewna 61 Beelde OE NE eee 09444 62 Low Recovery of Volatile Compounds 122 M Making Changes 107 Maximum Elution Volumes 75 Menu Software 26 Method Changes 107 Method Development Checklist 111 Method Does Not Run 117 Method Example 91 Method Manua
47. 96 01 1 09 AutoTrace SPE Workstation User s Manual Software 92 AutoTrace Method Example continued FLOW RATES Cond Flow Load Flow Rinse Flow Elute Flow Cond Air Push Rinse Air Push Elute Air Push SETUP PARAMETERS AutoTrace Extraction Workstation 10 0 mL 10 0 mL 10 0 mL 2 0 mL 10 0 mL 10 0 mL 10 0 mL SPE PARAMETERS Push Delay 5 sec Air Factor 1 0 Autowash Vol 0 00 mL WORKSTATION PARAMETERS Max Elution Vol 12 0 mL Exhaust Fan on Y Y Yes N No Beeper On Y Y Yes N No a Specifying 2 mL for the Autowash Volume allows the elimination of steps 2 5 10 and 12 in the method Solvent 1 MeOH Solvent 2 WATER Solvent 3 EtO Ac Solvent 4 MeC12 Solvent 5 not used NAME SOLVENTS a The corresponding solvent names are specified Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 93 Application Tips Once the method is written it may require some fine tuning to optimize sample recovery and or sample throughput The need for changes may be evident when first running the method or when examining the recovery data from the sample run If the recovery data looks good test higher flow rates shorter times etc to achieve a higher sample throughput Optimizing When making changes to optimize the method make them one at a time to evaluate the effect of the change The next few pages provide recovery data setup parameter and method step c
48. Button 78 Save Button 78 Undo Button 78 Setup Parameters 94 Shipping Container 11 Software Diagram 33 Software Files and Functions 33 Software Installation 24 Solid Phase Elute Commands 85 Solid Phase Elute Selections Clean Sample Path 87 103 Concentrate Sample 103 Elute to Collect 86 Elute to Collect Second Tube 86 Elute to Collect 2nd Tube 103 Elute to Soak 24 aa 244200565008 85 AutoTrace SPE Workstation User s Manual ST MA AERODEN 87 Pause and Alert 104 Rinse Sample Container 88 103 Wash Syringe 89 Solid Phase Extract Commands 80 Solid Phase Extract Selection PauSe 0 0 0 cee eee 27 Solid Phase Extract Selections Clean Sample Path 27 Column Rinse 27 82 Concentrate Sample 27 Condition Column 27 80 Dry with Gas 27 83 Elute to Collect 27 Elute to Soak 27 Load Sample 27 81 Optional Operations 27 Pause 0 AA 81 Rinse Sample Container 27 Standard Operations 27 Wash Syringe 27 83 Solid Phase Extraction Specifications 160 Solvent Parts 30 Solvent Reservoir Connections 13 Solvent Selection 26 Solvent Waste Tubing
49. CONT button twice rapidly Stop continuous Press the PAUSE button routines a To run a subsequent method or diagnostic select another diagnostic from the drop down menu and then press CONT twice slowly Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Diagnose Problems 116 Troubleshooting This section provides troubleshooting information for the AutoTrace SPE Workstation The section is divided into the following topics e General Operation Troubleshooting on page 117 e ERROR Light Troubleshooting on page 118 e Computer Troubleshooting on page 118 e Liquid Handling Troubleshooting on page 119 e Solid Phase Extraction Troubleshooting on page 122 Refer to the appropriate section and locate the symptom in the left hand column that describes the problem Then refer to the probable cause and solution listed to the right of the symptom Symptoms experienced may not indicate a problem with the workstation they may be related to a parameter setting or method step selection Refer to Application Tips on page 93 Replace Parts If the solution is to replace a part refer to Ordering Supplies on page 163 The AutoTrace Replacement Kits include detailed instructions on part replacement WARNING AA Unplug the AC power from the workstation before servicing the unit Additional Assistance If after following this manual you need additional help contact Dionex Techn
50. E T 167 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 11 Installation Parts Listing The Dionex AutoTrace SPE Workstation is available in two versions Cartridge and Disk The workstation comes with the following parts Unpacking Workstation Cartridge or Disk Sample Rack 6 position Waste Containers 2 Startup Kit Unpack the shipping container and verify that all items listed above are present If anything is damaged or missing contact Dionex Technical Support see Contact Us on page 3 Record the Serial Number Record the workstation s serial number The serial number is on the back of the workstation This information is required when you call Dionex Technical Support Installation Overview Installing the AutoTrace Workstation involves the following steps 1 O OA N O CF FP Q N Review the specifications If necessary convert the workstation voltage Prepare the work area and position the workstation Make solvent connections Install the waste drain and tubing Connect the exhaust hose and gas supply Check compression screws for tightness Power up the workstation Provide access to a computer 10 Install the AutoTrace software Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 12 Tools Reduired If you need to convert the workstation from 120 VAC have available a small flat blade screwdriver a small Phillips screwdriver and
51. Figure 1 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 14 Connect the Solvent Reservoirs Continued Small Hole Tubing Weight Figure 1 Tubing in Tubing Weight 6 Push a barbed fitting into the end of the tubing as shown in Figure 2 Barbed Fitting p Figure 2 Barbed Fitting NOTE UH To hold the tubing in your fingers while installing the barbed fitting grasp the tubing using a flat rubber band or piece of emery cloth 7 Gently pull the tubing upward until the barbed fitting seats itself within the recess of the tubing weight as shown in Figure 3 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 15 Connect the Solvent Reservoirs Continued f upward 1 Recessed Area Figure 3 Pulling Tubing Upward 8 Cap the bottle and adjust the length of tubing until the weight touches the bottom surface of the reservoir as shown in Figure 4 Tubing Weight Figure 4 Tubing Weight in Reservoir 9 Repeat steps 4 through 8 for each reservoir to be used Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 16 Install the Waste Drain and Tubing To install and orient the waste drain and connect the solvent and waste tubing 1 Locate and remove the waste drain from its bubble pack bag in the Startup Kit as shown in Figure 5 Hose Fittings Waste Drain Figure 5 Waste Drain 2 Determine whether you want the waste t
52. I file AT INI to reflect the disk or column version Download the proper files and dictionary to the AutoTrace unit Erasing AutoTrace Dictionary 4 2 3 4 5 6 Close the AutoTrace software on the PC Open the HyperTerminal communication software Establish communication with the AutoTrace Workstation Type Erase When the software asks if you are sure answer NIE Type Dir to make sure that the dictionary is empty Close the HyperTerminal software Changing the AutoTrace INI file 1 A 5 Locate the AT INI file The default path is C Program Files Dionex AutoTrace SPE Workstation Open the AT INI file using Windows Notepad Find the following line Version x Where x 1 column or 2 disk Change the version number to reflect your new configuration Save the AT INI file and close it Downloading the New Dictionary to AutoTrace 1 Doc 065296 01 1 09 Open the AutoTrace software The title bar should display the proper version Cartridge or Disk AutoTrace SPE Workstation User s Manual Changing Between Column and Disk Versions 152 2 From the main menu select Diagnostics lnitialization A DOS window opens The window should state that the proper ZYOS file and then the proper dictionary file are downloading e BMAT133 BMD for column e BMATD103 BMD for disk This download will take several minutes to complete because the entire dictionary files and method are being downl
53. LS REGU Ta GA ED GE EG N NANANA 146 Pars REGUN OO nananana EE EERS ES NE EE ee ei eng DER se Eie EE ee sl Ge 146 Pro edure OVerVie Wise ed ite De ea ee ee eld ued ds 146 Remove the Existing Column or Disk Holder iese see see see see see see ee ee ee ee ee 147 Install the New Column or Disk Holder iese see see ee ee ee a 148 Changing the Sample PUMP ses SE SE SE es SE Ee NAMANA ANA 148 Removing the Defective PUMD iese sesse aaa 149 jastalling die Ne MPRDA EO EG DR Ee EG OE GE 150 Reconfigure the AutoTrace Software see see ee ee Ee ee ee RE ee ee ee ee ee ee ee 151 Erasing Auto race Dina se RS EISE Ee AARD Ee AAJ 151 Changing the AutoTrace INI file sesse se Ee ER Re Ee EA ee ee Ee EE ee ee ee 151 Downloading the New Dictionary to AUtOTrace sesse se ee ee RR ee AE 151 Configuring HyperTerminal to Communicate with AutoTrace 152 Vollage CONVErSIO0N su NANANA 155 POWT ERNI FON bansasa a NAG AA MAAN PAN ANAL NG AAO GAAN ana Bugan O nG Ge 155 a OK AA 155 Remove the Fuse Block Assembly aa 156 Select the New Voltage a ee ER ee a ee ee ee ee 156 Converting from 100 120V to 220 240V ee ee ee Ee ee ee AA Re ee ee 157 Converting from 220 240V to 100 120V ee ee eee ee ee ee RE AA ee ee ee 158 LENIN Opera io RE AN Na OE OE EE be EO NG OG ED 159 jellie jies died ri EE RE RE EE 160 Ordering Supplies 163 GOS AE NAA E 165 BING AA AA PAA N OE RE
54. Print Setup 59 Flashing Ready Light Response 106 Flow Rates Cond Air Push 73 Cond Flow 73 Control 02 26 Elute Air Push 73 Elute Flow 13 Load Flow 7a Rinse Air Push 73 Rinse FlOW SS SS 73 Flushing Sample Lines 111 126 Flushing Solvent Lines 110 126 Front PANG xa one Ka KARL en 29 AutoTrace SPE Workstation User s Manual Front Panel Controls CONT Button 29 101 ERROR Light 29 LOAD Button 29 101 PAUSE Button 29 101 RUN CIGN si way god GA DE ee REG 29 Front Panel Display Error Messages 113 Front Panel Display During Operation 102 Front Panel Display Messages 103 Front Panel Error Messages 113 Front Panel Messages Clean Sample Path 103 Concentrate Sample 103 Displaying 103 Elute to Collect 2nd Tube 103 Pause and Alert 104 Rinse Sample Container 103 Front VIEW ES SES SE ss eee 28 Fuse Replacement 137 G GaS Nlet sies eae ER ER ER ob anes 30 Gas Pressure Gauge 31 Gas Regulator Knob 31 Gas Regulator Specifications 161 Gas Supply Connection 20 GIOSSANY piss ma ka NA wed Gos 65 HA 165 H Help Button 78 Help Menu 200005 6
55. Supplies on page 163 to order Replacement Kits Contact Dionex Technical Support see Contact Us on page 3 with any questions about maintaining the workstation Routine Maintenance This section reviews the routine maintenance to be performed on the AutoTrace Workstation Regularly observing AutoTrace operation and following the limited number of methods in Table 18 will ensure optimum workstation performance Table 18 Routine Maintenance Description Periodically clean column holders racks and other workstation surfaces with warm soapy water Flush Lines Flush the workstation s solvent and sample lines if not using the workstation for an extended period Refer to Operation on page 97 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 127 Table 18 Routine Maintenance Continued Description Check for Leaks Routinely check for tubing and syringe leaks If a tubing leak is found replace the tubing as necessary If liquid is below the plunger tip level inside any syringe replace the syringe Check for Fitting Make sure all syringe and valve fittings are Tightness finger tight Check for O ring Check the O rings at the bottom of the Wear column holder for cracking or wear and replace any O rings as required Check Overall Check the overall workstation performance Performance by running the utility method see Testing General Operation Benchmark Test Utility
56. a series of special diagnostic and service programs AutoTrace Created when the method is entered into the Method AutoTrace menu software This method is then used by the AutoTrace operating software to run the samples Earlier versions of software referred to Procedure instead of Method but the terms have the same meaning AutoTrace Software that provides menu software for setting up Software the method in the computer and operating software for running the method in the AutoTrace SPE Workstation Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Glossary 166 Table 22 Glossary Terms Continued Flow Rates The speed in mL min at which to run the AutoTrace syringes Flow rates for solid phase conditioning loading rinsing and eluting operations are designated on the Setup Parameters screen Maximum The maximum volume that can be eluted into the Elution collection container based on the container size Volume Menu The portion of the AutoTrace software on the Software computer that is used to set up write and review Auto Trace methods Method The list of steps used for implementing a laboratory application Earlier versions of software referred to Procedure instead of Method but the terms have the same meaning Operating The portion of AutoTrace software that runs a Software method in the AutoTrace Workstation See AutoTrace Method Push Delay The time in seconds to pause
57. according to the air factor parameter a higher air factor will position the end of the solvent closer to the column Any subsequent elution steps can have smaller volumes e If the automated method doesn t require soaking or multiple elution steps use the following ELUTE TO COLLECT step e An ELUTE TO SOAK step must be followed by an ELUTE TO COLLECT step ELUTE TO COLLECT is ended by a larger air push that will push any remaining eluent into the collection container Elute to Collect To perform a sample elution specify a solvent and a volume to be passed through the column or disk with the eluent directed to the collection container NOTES e In contrast to CONDITION COLUMN or CONDITION DISK and ELUTE TO SOAK when ELUTE TO COLLECT is performed a larger volume of air is used to push the sample through the entire path of liquid lines e Performing multiple ELUTE TO COLLECT steps is allowed as long as the maximum elution volume for the collection container is not exceeded and the larger air push between each step is not a concern Elute to Collect Second Tube To elute up to double the volume allowed for the collection container specify a solvent and volume to be passed through the same column or disk with the eluent directed to a second sample container This step causes the workstation to pause for the operator to change collection containers Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 87
58. after liquid has been sent through the column allowing the pressure to equilibrate Setup The screen display of all changeable AutoTrace Parameters parameters Every parameter listed begins with a default value SETUP The program used to install the Auto Trace software Program on the computer hard drive Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Index Numerics 12 Port Valve SS SS ee 31 6 Position Sample Rack 11 A Aborting Operation 104 Additional Parameter and Solvent Information EE 70 Adjusting Air Syringes 132 Adjusting Liquid Handling Syringes 128 Adjusting New Air Syringes 134 Adjusting New Liquid Handling Syringes 130 After Method Run 107 Air Syringe 30 Air Valve anaa 0 eee 31 Application Tips 93 Aqueous Waste Tubing 31 AutoTrace Main Window 58 B Beeper ON ee 74 C Calibrating Sample Pumps 139 Cannot Download Method 118 Centering Air Syringe Plunger 132 Centering Liquid Handling Syringe Plunger ee ee 128 Changing Setup Parameters 72 Changing Solvent Names 75 Checking Compression Screws 22 Checking Fitting Tightness 127 Checking Leaks 127 Checking O ring Wear 127 Checking Overall Performance 127 Cleaning Sample Lines with Solvent and DI Water 0
59. an the Sample Lines with Solvent and DI Water on page 68 between each batch of samples 7a Increase the sample volume specified in the LOAD SAMPLE step refer to Solid Phase Extract Commands on page 80 by 5 to 7 For example specify 1050 mL instead of 1000 mL 7b Perform CLEAN SAMPLE PATH with deionized water refer to Creating a Method to Clean the Sample Lines with Solvent and DI Water on page 68 and then run the CALIBRATE PUMP utility as described in Calibrating Sample Pumps on page 139 8 Contact Dionex Technical Support to determine the faulty part and replace See Ordering Supplies on page 163 AutoTrace SPE Workstation User s Manual Diagnose Problems 124 Table 17 Solid Phase Extraction Continued 9 Nothing comes out 9 Clogged nozzle 9 Clean the nozzle with a of an elution manifold fine piece of wire If the nozzle problem persists replace the manifold See Ordering Supplies on page 163 10 Elution station 10 Bad stepper motor or 10 Run the Benchmark Test does not move into loose connection on control Utility on page 141 and the correct position board contact Dionex Technical Support Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Error Codes 125 Error Codes This section describes the error codes that may appear when downloading either methods or utility procedures Error Code Description Action 1073741510
60. ash the liquid handling syringe NOTES e Atleast 2 mL of solvent is a recommended starting point e Alternative Use the Autowash feature instead For details see the description in Setup Parameters on page 94 e You must insert a WASH SYRINGE step with an intermediate solvent when going between steps that use immiscible solvents even if Autowash is being used For example Rinse column with 10 mL of water into aqueous waste Added Wash Syringe Step gt Wash syringe with 2 mL of isopropyl alcohol Wash syringe with 2 mL of MeCl or by Autowash Collect 5 mL fraction into sample tube using MeCl End Method This selection completes the entry of your method steps This step is required for all methods Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 90 Method Example To give you a better idea of how to transfer a method into an AutoTrace method a method example follows Manual Steps The steps summarized below have been taken from a nitrogenous herbicide method as a demonstration of how to transfer a method to the AutoTrace Workstation 1 Doc 065296 01 1 09 Condition the SPE cartridge with two 10 mL aliquots of methanol Add 10 mL of reagent water to the SPE cartridge Pass 1 liter of prepared water sample through the SPE cartridge Wash the sample reservoir with 10 mL of reagent water and pass through the SPE cartridge to waste Dry the SPE cartridge under vacuu
61. ault EMGS ER SE SERE Se ME ge be RO nala 70 Changing Sep sa EE EE inet ate E nA aee 72 Ghande Solvent Names SE EE RE EED N SE N GE EE Ee GE e ia a 75 WHUN a Methods ER N AA MA de Ee td ee Ee ie 76 Adding a Method Sle ESE ER N DE EE etd ale Ee ee EE AD END GE 79 Deleting a Method Step aa EE NE N EK ER ERROR GER SEER EER SE RE DE GR ede sw SR We 79 Solid Phase Extract COM Mana NA Ee oe es le 80 Solid Pnase lute COMM MAS EE EE EG ER Se DE GE 85 MeMO fal AMPIE aste ie N te EE AE ae DE ER DE SE eae 90 Manual Steps EE ee ER RS EE ee EE EG DE edd 90 Auto Trace Method Example aa Ee ee N oe 91 ADDIICALON DS SEE DE ES ER N SE N SE dd ee RE Ee ee 93 OQDUMIZINO EE SR N OE DR Do Ee Ee ie eee eee 93 Sample REGOVErY su SEER ER ER GEE GER Ee De De OG EE DR SE EE DE Ge EE 93 Selup Paramelelfs ES ee EE n GE a ke TE sees 94 Method Steps EE ada NAGLABAN AGA ee Ge ED AA 95 Operation RE AA KA EE 97 Preparing the AutoTrace SPE Workstation ees ee see see ee a 97 Running an AutoTrace SPE Method esse sesse see ee ee ee ee ee ee ee ee ee Ee ee ee ee ee 101 LOAD Button Operalion EE weet DE ie NANA na EA Gare EG De eee 101 CONT Button Operali s ES RE Re ee ei nee ee 102 Front Panel Display During Operation ee ese ee ee ee ee ee ee Ee ee ee ee ee 102 Front Panel Display MessageS ss sesse se see ee Ee ke Ee ee ee ee ee ee Ee ee ee ee ee ee 103 Pausing Opera OM sis SS EE GE EE E E Ge ei ee 104 GONTAUING OperatiOmM sk sb EE a De DE DE SE 1
62. cket Fitting Screw Housing Black Thumbscrew Plunger Driving Arm Thumbscrew Figure 69 Syringe Screws and Mounting Bracket 2 Remove the black thumbscrew from the bottom of the syringe plunger 3 Gently slide the syringe assembly out of the housing 4 Loosen the small black thumbscrew on the mounting bracket 5 Holding the black mounting bracket in your left hand and the syringe in your right hand turn the syringe counterclockwise until it disengages from the fitting 6 Separate the syringe from the fitting Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 130 Mount the New Syringe To mount the new syringe 1 Slide the new syringe into the fitting When aligned turn the syringe clockwise to secure it in the fitting 2 Tighten the small black thumbscrew on the mounting bracket 3 Slide the syringe assembly into the housing and secure the mounting bracket using the two screws previously removed 4 Gently pull the syringe plunger down until it contacts the top of the driving arm 5 Secure the plunger to the arm with the black thumbscrew previously removed Adjust the New Syringe To adjust the new syringe 1 Loosen the knurled thumbscrew approximately two turns as shown in Figure 70 GE a i r n a e f j n r F 4 ess Steel Tubing Compression Screw Plunger Driving Arm Knurled Thumbscrew bumata Thumbwheel Figure 70 Syringe Knurled Thumbscrew
63. conds between presses Purging the Solvent Lines Utility Purge the entire length of the solvent lines any time they are dry For example when the workstation is being used for the first time each day or whenever the solvent supply runs out To purge the solvent lines download the Purge Solvent utility method provided or write your own purge method Purging the sample lines is described in Customizing a Method to Purge Less than Five Solvent Lines on page 6 7 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 67 Customizing a Method to Purge Less than Five Solvent Lines To save a method to purge the solvent lines when you will not be using all five solvent ports do the following For more details refer to Writing a Method on page 76 1 2 3 A From the AutoTrace main menu choose Methods Click the New button Name the method Purge Solvent Path Custom Specify the maximum number of samples that can be run a Select WASH SYRINGE once for each solvent port being used Specify a volume of 5 mL b For example when using three solvent ports the purge method would consist of these steps e Process 3 samples using the following method Step 1 WASH SYRINGE with 5 mL of SOLVENT 1 e Step 2 WASH SYRINGE with 5 mL of SOLVENT 2 e Step 3 WASH SYRINGE with 5 mL of SOLVENT 3 Click the Save button From the AutoTrace main menu choose Serial OP 5Download Method Setting
64. ctor and separate the two connector halves Locking Tab Pump Mounting Bracket Screw 1 of 2 Figure 83 Pump Rear View 5 Remove the two screws that secure the pump to the pump mounting bracket Set the screws aside 6 Carefully pull the pump through the hole in the mounting bracket angling the back of the pump downward to allow the tab on the front of the pump to clear the hole Installing the New Pump 1 Install the new pump by carefully placing it through the hole in the mounting bracket angling the back of the pump downward to allow the tab on the front of the pump to clear the hole 2 Replace the two screws that secure the pump to the pump mounting bracket 3 Reconnect the two connector halves and check the wiring 4 Replace the screws that secure the rear cover of the workstation 5 Reconnect the pump s compression screws and tubing 6 Reconnect the power cord and turn on power to the AutoTrace 7 From the main menu choose Serial Op Download Utility Procedure and choose Calibrate Pump 8 Follow the instructions in the Help screens to run the calibration utility Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Changing Between Column and Disk Versions 151 Reconfigure the AutoTrace Software To reconfigure the AutoTrace software after converting the unit from Column to Disk or Disk to Column you need to perform three steps Erase the Auto Trace Dictionary Edit the AutoTrace IN
65. de the U S call the nearest Dionex office Before you call you should have the following information available for the Technical Support Representative e Product serial number e Software version found by choosing About from the main Help menu e If applicable the error code reference number shown on the product s LCD display or from the database event log Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Preface 4 FCC This device complies with part 15 of the FCC United States Federal Communications Commission Rules Operation is subject to the following two conditions e This device may not cause harmful interference e This device must accept any interference received including interference that may cause undesired operation CE This device complies with all CE rules and requirements NOTE Changes or modifications to this equipment not expressly approved by the party responsible for compliance could void the user s authority to operate the equipment Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Preface 5 Table of Symbols Table 1 contains symbols that identify particularly important information and alert you to the presence of hazards Some of these symbols may not appear in this manual or on the product it describes Table 1 Important Symbols Symbol D DANGER An imminently hazardous situation which if not avoided will result in death or serious injury WARNING Caution
66. dge the reminders and continue e The RUN light to come on e The valves to click The sample processing to begin CONT Button Operation To start processing a new batch of samples after all samples from the prior run have been processed press the CONT button twice slowly This begins running the method without loading the operating system first NOTE Use caution when using the CONT button to start a method If all steps haven t been run the PAUSE button has been pressed pressing the CONT button continues operation where it was before processing was interrupted not at step 1 Front Panel Display During Operation While the method runs the front panel reports each step as it is performed and the time left for the operation if applicable For example while a sample is being loaded pumped onto the column the front panel displays LOADING SAMPLES ONTO COLUMNS 10 MLS MIN 5 MINUTES LEFT Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 103 Front Panel Display During Operation Continued NOTE The Disk version of the Auto Trace Workstation will display Disk instead of Column on the front panel The display also reports when manual intervention is required and when the sample run is finished Front Panel Display Messages Some method steps cause the workstation to pause operation and wait for manual intervention When this happens the workstation beeps if the Beeper On pa
67. die SE EG GA DE SG DE GP artes Alen 112 After Running the Method sies ES Se Ee ee AA 112 DIAGNOSE Problehis ia Es RR iN EE AA EE a ES GE Ee EE 113 EIOF ME SSAOES RE ee NA AA AA AA 113 FrontPanel Emor Messade aat Ee en Me ie bee N ke AR bien as 113 Auto Trace Diadnos Us sms EEN SN EE NE AN GE OND N DEE ER DE 114 DIAOMOSUG IS see EE ER ad ie De ee oe EE 114 Downloading and Running an AutoTrace Diagnostic Method 115 TFOUIDIESMOOUING ss ES na na Nadaanan kanaba atah Ge Ee EE les a 116 Aeplace Pak AA ANA ANA NA init Malet 116 Adallonal ASSISTANCE AA AA Aa a 116 General Operation Troubleshooting a 117 ERROR Light Troubleshooting 1 1 aa 118 Computer TIrouble 8s N00 NG Kaman ANA AA NA aa TALA 118 Liquid Handling Troubleshooting 2 a 119 Solid Phase Extraction Troubleshooting a 122 ERROR CODES AA AA AA 125 MAINTENANCE EE AA AN 126 ROUTINE Malril nanEe ESE SS Oe A RE EE GR EE Ek DE ee bo 126 Replacing and Adjusting the Liquid Handling Syringe ees see se sees ee see ee ee ee 128 a EE EA EE TEE EO ORE OT EA EE 128 Puide Ihe SOIWENE Lines ER ORE AA RE 128 Centerthe Syringe PUNGE is EERS SR ED Re EE taste EE AE ba De ee 128 Remove the Defective Syringe ee ee Ee Ee Ee Ee ER ER ER ER ER ee ee ee Ee Ee Ee ee 129 Mont the NEW SYN Gama kA a a a RE de 130 Adjust the NEW Syringe ES BERE ES Ge aa ANAN 130 Replacing and Adjusting the Air SYriINge
68. ds window To choose a different method click the Load button to open the Find Method window see Figure 59 and double click the method that you want to open The selected method is loaded in the Setup Methods window 01 1 09 AutoTrace SPE Workstation User s Manual Software 77 Writing a Method Continued 3 Find Method Help Close Las Change Method Name DJ 08 06 2004 PESM new 2T 500 mi Figure 59 Find Method Window Buttons in Setup Methods Window See Figure 58 on page 76 Load Button Loads an archived method from the database New Button Allows you to write a new method The Method window prompts for the method name the number of samples to be run and the selections for defining the method steps Method Name Type a name for the method up to a maximum of 38 characters Spaces and any characters can be used Samples Type the number of samples to process when the method runs This information is used for time estimating purposes only Specifying the number of samples causes the first line of the method to change Example for only two samples Step 1 Process 2 samples using the following method steps Default value 6 Solvent set Select a solvent set with up to five solvents by clicking the button next to the solvent in the solvent box Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Software 78 Writing a Method Continued Edit Edit mode for the method Any data can
69. e following specifications Doc 065296 01 1 09 Compatible with Microsoft Windows 2000 SP4 and Windows XP SP1 Professional operating systems including the latest released service packs Follow Microsoft s recommendation for the computer specification with the following minimum hardware specifications Windows 2000 CPU 400MHz RAM 128M Windows XP CPU 650MHz RAM 192M AutoTrace SPE Workstation User s Manual Installation 24 Computer Access Continued You can also install the AutoTrace software on a local area network LAN Software Installation NOTES n e To install this software you must be assigned to the Windows Administrator group e An operator must be assigned to the Windows Power User group in order to use the software To install the Auto Trace software on your computer 1 Start Windows and insert the CD in the CD drive 2 From the Microsoft Windows operating system Start menu select Run and click the Browse button 3 Navigate to the CD drive 4 Select the setup exe file and click the Open button 5 Click the OK button Follow the on screen instructions The software is installed in the default directory of C Program Files Dionex Auto Trace SPE Workstation NOTE Ul If the software is installed in a directory other than C Program Files Dionex Auto Trace SPE Workstation the INI file has to be modified as described in INI File on page 25 6 Op
70. e O ring When replacing the O ring for glass column units replace the whole plunger assembly Refer to Ordering Supplies on page 163 3 Low recovery of 3a Sample evaporates 3a Use a PAUSE AND volatile compounds while column or disk ALERT step to introduce conditioning occurs sample when needed by the method 3b The gas pressure is set 3b Decrease the gas too high pressure 4 Low recovery 4 Varies 4 Refer to the list in Sample Recovery Optimization on page 93 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Diagnose Problems 123 Table 17 Solid Phase Extraction Continued 5 Water coming off with eluent 6 Cross contamination 7 Incorrect volume removed from the sample container 8 Sample pump fails to start Doc 065296 01 1 09 to clear the lines 5a Method is missing a step 5a Add a COLUMN RINSE or DISK RINSE or DRY WITH GAS step before elution ob The gas pressure is too 5b Increase the gas low pressure 5c The drying time is too short 5d None of the above 6 The sample path was not cleaned between sample passes 7a Samples with large amounts of suspended solids 7b Sample pump is out of calibration 8 Bad electronics board or pump 5c Increase the dry time specified in the DRY WITH GAS step 5d Run eluent through a drying column or disk before analysis 6 Use Creating a Method to Cle
71. en the AutoTrace software by choosing from the Windows Start menu Programs Dionex AutoTrace SPE Workstation 7 Close the AutoTrace software Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual INI File Installation 25 The AutoTrace software program uses a file named AT INI which is loaded by starting the program AT INI must always be in the working directory the default is C Program Files Dionex Auto Trace SPE Workstation Modifications can be made using an ASCII editor such as Windows Notepad NOTE u Blank spaces are not allowed in the AT INI file to the left of an equal sign and before the first letter to the right of an equal sign The AT INI file contains specifications concerning path name of the necessary data bases DATABASES and the language adjustment AUTOTRACE An example of an AT INI file follows DATABASES Database Data ATDATA MDB Data Dir C 1Program Files Dionex AutoTrace SPE Workstation data AUTOTRACE AT Drive A Language 1 Version 1 See Note below Comm Port 1 NOTE The Version option identifies whether you are running a Cartridge Version 1 or Disk Version 2 AutoTrace Workstation If you have both types of units you can run the AT software for either unit by e Changing the Version option to the correct value in the INI file e Saving the INI fil and e Starting the AutoTrace software If the program is installed in a directory other than C Program Files
72. ering information 5c Degas or sparge reagents with helium before use 5d Loose valve fittings or od Make sure all fittings are loose coaxial fitting finger tight oe Defective valve fittings 5e Contact Dionex Technical Support 5f Run the Syringe Diagnostic Refer to Diagnostics Menu on page 61 and the online Help If necessary replace the syringe Refer to Ordering Supplies on page 163 for ordering information 5g Run the CHECK 12 PORT VALVE diagnostic Refer to Diagnostics Menu on page 61 and the online Help Do not run the diagnostic until all solvent lines have been purged If the problem continues contact Dionex Technical Support oh Wash the syringe with intermediate solvent between steps Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Diagnose Problems 121 Table 16 Liduid Handling Continued 6 Liquid buildup in 6a Excessive pressure built 6a Inspect and correct the 10 mL air syringe up in unit due to blocked problem line or excessive solids in column 6b Syringe speed too fast 6b Adjust the flow rates 6c Air valve leaking 6c The valve needs replacement Contact Dionex Technical Support 7 Incorrect volume 7a Samples with large 7a Increase the sample removed from the amounts of suspended volume specified in the sample container solids LOAD SAMPLE step refer to Solid Phase Extract Commands on page 80 by 5 to 7 For
73. es how to change the AutoTrace configuration from either Column to Disk or Disk to Column Tools Required e Phillips screwdriver e Slotted screwdriver Parts Required e Replacement SPE column holder e Replacement SPE disk holder Procedure Overview mk Remove the existing column or disk holder Install the new column or disk holder Change the sample pump Ph QW N Reconfigure the AutoTrace software Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Changing Between Column and Disk Versions 147 Remove the Existing Column or Disk Holder 1 2 10 Doc 065296 01 1 09 Turn the AutoTrace power off and unplug the power cord Slide the tubing clamp up so that it is no longer over the stainless steel tubing G La lt a Tubing Clamp p Figure 80 Disk or Column Holder Grasp the bottom of the Teflon tubing and carefully pull it upward until it slides off the top end of the stainless tubing Disconnect the Teflon tubing from the lower end of the column or disk holder by unscrewing the compression screw Remove the screws that secure the rear cover Set the cover and screws aside Locate the back of the holder you are replacing Follow the two sets of wires that lead from the back of the holder to the AutoTrace Column Interface board Unplug the holder s two connectors from the board Carefully undo the cable attachments that secure the holder wires to the back of the workstation
74. ess the new fuse s into place Make sure the new fuse s are identical to the old fuse s 3 Slide the fuse block assembly into the power entry port housing and snap it into place 4 Close the power entry port door 5 Plug the AG power cord into an AG power outlet WARNING A Only plug the AC power cord into a properly grounded outlet Only use a standard IEC 320 style power cord appropriate for your country 6 Turn the workstation on 7 Verify that the READY light comes on and the workstation operates normally Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Maintenance 139 Calibrating Sample Pumps This section explains how to run the CALIBRATE PUMP utility method This method should be run only if the volume removed from the sample container does not match the sample volume requested in the method s LOAD SAMPLE step Parts and Tools The following parts and tools are required to complete this method Allen wrench 3 32 inch Sample container with approximately 120 mL of water pump being calibrated Balance 1 16 inch ID tubing provided in Startup Kit Calibration Method Perform the following steps on each sample pump that requires calibration 1 Doc 065296 01 1 09 Perform a single step CLEAN SAMPLE PATH method as discussed in Creating a Method to Clean the Sample Lines with Solvent and DI Water on page 68 using DI water Download a Calibrate Sample Pumps procedure a From t
75. h the sample lines refer to Next Sample Batch Preparation on page 109 Method Development Checklist Specify Your Method LJ Run the AutoTrace software LI Specify the parameter and solvent information LJ Write the method LJ Print and save the method Prepare the Workstation Turn on the workstation Turn on and check the gas supply and set gauge if applicable Check the solvent reservoirs Check empty the waste containers Purge the solvent lines Load the elution rack Optional Clean the columns or disks Load the SPE columns or disks DDLLDULDLDLLDLDLD Load the sample container rack Run the Method LJ Load the method LI Observe operation L Press the CONT or PAUSE button to silence alarm for end of run After Running the Method LI Based on recovery data and observations during operation make any necessary procedural changes using the METHODS program option LJ Remove the used columns or disks Q Prepare to run the next batch of samples by cleaning the sample lines Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual E Operation 112 If done for the day clean up by emptying the waste reservoirs and flushing the solvent and sample lines Daily Operation Checklist Prepare the Workstation DDLLLDLDULDULDULD Turn on the workstation Turn on and check the gas supply and set gauge if applicable Check the solvent reservoirs Check empty the waste containers P
76. h the syringe into place Position the syringe clamp across the chrome end piece and secure it in place by tightening the knurled knob Gently pull the syringe plunger down until it contacts the top of the driving arm Secure the plunger to the arm with the black thumbscrew previously removed Adjust the New Syringe To adjust the new syringe 1 Doc 065296 01 1 09 Loosen the knurled thumbscrew approximately two turns as shown in Figure 73 on page 135 AutoTrace SPE Workstation User s Manual Maintenance 135 Adjust the New Syringe Continued Plunger v Knurled Thumbscrew ad lt t humbwheel Figure 73 Syringe Knurled Thumbscrew 2 Turn the thumbscrew to the left until the knurled thumbscrew moves to its upper limit of travel 3 Press the CONT button twice quickly to rerun the ADJUST AIR SYRINGE diagnostic As the plunger moves up you should hear a clicking sound 4 Turn the thumbwheel to the right just until the clicking stops Then turn it one more partial turn as shown in Figure 74 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance Adjust the New Syringe Continued Top View Turn thumbwheel one more partial turn to the Thumbwheel right by the amount shown Figure 74 Thumbwheel Rotation 5 Tighten the knurled thumbscrew to secure the position 6 Press the CONT button twice quickly again to rerun the diagnostic Confirm that the s
77. he AutoTrace main menu choose Serial OP 5Download Utility Procedure b Click the Calibrate Pump button c Read the online Help for this utility before continuing Press the CONT button twice slowly and follow the prompts on the front panel display As instructed weigh the collection vessel before and after pumping Determine the percentage difference between the expected volume of 100 mL and the delivered volume Example If the volume of water that the utility pumps is 103 mL rather than the expected 100 mL the volume is off by 3 Locate the pump s calibration screw in the hole on the right side of the pump as shown in Figure 76 AutoTrace SPE Workstation User s Manual Maintenance 140 Calibration Method Continued Calibration Screw Figure 76 Pump Calibration Screw 6 Use the Allen wrench to adjust the screw as follows a aturn clockwise to decrease the volume 2 5 b 4 turn counterclockwise to increase the volume 2 5 Example For the example above you would turn the adjustment screw clockwise approximately 4 of a turn 7 Rerun the calibration utility to test the change and make any further adjustments that are needed 8 Repeat steps 3 through 7 for each sample pump to be calibrated Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 141 Benchmark Test Utility This section explains how to run the Benchmark Test Utility method Run this utility if there is any indication
78. ical Support see Contact Us on page 3 When calling please have the information recorded in the front of the manual ready for the Technical Support Representative Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual General Operation Troubleshooting Symptom 1 READY light not ON 2 READY light flashing 3 When AC power is turned on syringe motors make a chattering sound with syringes fully emptied 4 RUN light fails to turn on after the LOAD button is pressed or the method does not run Doc 065296 01 1 09 Diagnose Problems 117 Table 13 General Operation Probable Probable Cause 1c Fuse is blown 1d No voltage at power outlet 2a Internal CPU error condition system error 2b CPU is bad 3 Limit switch on the syringe drive needs adjustment 4a Files missing from download 4b Loose connection on the control board 4c Column or disk holder not fully down holder s green LED is Off Solution 1a Power switch is ET 1a Turn power switch on left side of workstation ON 1b AC power cord is 1b Connect the AC power unplugged cord 1c Replace the fuse Refer to Replacing Fuses on page 137 1d Check the outlet voltage with another component such as a desk lamp 2a Turn AC power OFF Wait 15 seconds Press the LOAD button while turning AC power on and then release the LOAD button 2b Replace the CPU Refer o Ordering Suppl
79. ies on page 163 3 Adjust the syringe s according to the program s syringe diagnostics or as described in Maintenance on page 126 4a Run the program s Initialization diagnostic referring to the Help screens If the problem continues contact Dionex Technical Support 4b Run the Benchmark Test Utility on page 141 and contact Dionex Technical Support 4c Push down on the holder lever until it clicks and the holder s green LED comes On Press the LOAD button AutoTrace SPE Workstation User s Manual Diagnose Problems 118 ERROR Light Troubleshooting Table 14 Error Light Symptom Probable Cause Solution The ERROR light Hardware error Error message displays comes on during or at Contact Dionex Technical the end of a method Support Computer Troubleshooting Table 15 Computer Unable to download a Communication error Check the communication method cable and the COM port setting Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Diagnose Problems 119 Liquid Handling Troubleshooting Table 16 Liquid Handling Symptom Probable Cause Solution la Syringe speed is too 1a Adjust the flow rates fast 1 Syringe makes a clicking sound while moving 1b Syringe not securely 1b Check the syringe mounted mounting 1c Defective syringe 1c Replace the syringe according to Replacing and Adjusting the Liquid Handling Syringe on page 128
80. igure 49 Data setup Parameters Name Solvents Figure 49 Data Menu Setup Parameters Set parameters to meet method specifications For more information refer to Specifying Parameter and Solvent Information on page 69 Name Solvents Specify solvent information For more information refer to Specifying Parameter and Solvent Information on page 69 Setup AutoTrace Commands Change standard options for method steps Only the values in the Std column can be changed The Setup AutoTrace Commands window is shown in Figure 50 This menu option is available only if the user type selected in the Setup User Data window see Figure 51 corresponds to Service Ted Setup Autotrace Commands AWA Print Help Autotrace Commands ml Ha min Pos Type Autotrace Command i Condition disk 0 1 5 0 Load sample 10 0 100 0 Pause and Alert Timed Pause Disk rinse Wash syringe Dry with gas Clean sample path Elute to soak Elute to collect Elute to soak 2nd tube Elute to collect 2nd tube Pause and Alert Timed Pause Clean sample path Rinse sample container Concentrate sample 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 No User logged on Figure 50 Setup AutoTrace Commands Window Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 64 Data Menu Continued Setup User Data The Setup User Data window see Figure 51 allows you to edit user data such a
81. ines with Solvent and DI Water Before beginning routine operation with the AutoTrace SPE Workstation a method is needed for cleaning the sample lines If the method does not end with CLEAN SAMPLE PATH steps see Clean Sample Path on page 87 run this method between sample runs to clean the lines Also whenever the workstation is idle for a period of time run this method to clean the lines and leave the lines filled with DI water To create the method perform the following steps For more details refer to Writing a Method on page 76 1 From the AutoTrace main menu choose Methods 2 Click the New button 3 Name the method Clean Sample Path Solvent amp Water Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 69 Creating a Method to Clean the Sample Lines with Solvent and DI Water Continued 4 Specify the maximum number of samples that can be run 5 Choose Clean Sample Path Specify a volume of 25 0 mL and select Solvent Waste as the Waste Position 6 If the solvent used for the first Clean Sample Path step is immiscible in water repeat the Clean Sample Path selection Specify a volume of 25 0 mL and choose Solvent Waste as the Waste Position Otherwise skip to step 7 7 Repeat the Clean Sample Path selection Specify a volume of 25 0 mL and choose Aqueous Waste as the Waste Position For each CLEAN SAMPLE PATH step the workstation pauses for the sample lines to be placed in a beaker
82. ing the AutoTrace AT Program To start the menu software click the Windows Start button and then choose Programs Dionex AutoTrace SPE Workstation If available you can click the AUTOTRACE icon on the desktop instead The copyright window now appears Close the window or wait 5 seconds for the window to close The AutoTrace main window is shown in Figure 42 The main menu and its options are discussed in this section t4 AutoTrace SPE Workstation Copyright 2008 by Dionex Version 2 11 File Methods Serial Op Diagnostics Login Logout Data Windows Help kg ad P Methods Serial Op H Diagnostics ed Logout Data pd Help Exit od P r rd ph paaa D l P ape a e e g P Figure 42 AutoTrace Main Window Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Software 59 File Menu The File menu contains the options shown in Figure 43 English Print Setup ek German Language F z h renc Database PF T Exit N Compact Repair Figure 43 File Menu Print Setup Change printer settings such as the standard printer page size and format Language Change the language between English German and French Database Compact As data changes in the database the database file can become fragmented and use more disk space than necessary Periodically compact the database to defragment the database file The compacted database is usually smaller Repair This method attempts to repair a database that was mar
83. ing the method is being downloaded The download takes a few minutes to complete depending on the size of the method and if other files are needed during the download process After the method is downloaded either press the CONT button or power cycle the AutoTrace and follow the on screen instructions on the AutoTrace to run the method Download Utility Procedure Downloads one of four utility methods to the AutoTrace Workstation e Purge Solvents purges the AutoTrace solvent lines e Benchmark Test tests general AutoTrace operation e Calibrate Pump calibrates the AutoTrace sample pumps Set Date and Time sets the AutoTrace date and time Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 61 Diagnostics Menu The Diagnostics menu contains the options shown in Figure 45 Use this menu to copy a diagnostic file onto the AutoTrace Workstation For more details refer to Diagnose Problems on page 113 Diagnostics Initialization Syringes Adjust Liquid Syringe Syringes Adjust Air Syringe Valves Check 12 Port Valve Figure 45 Diagnostics Menu Initialization Diagnose the reason for an AutoTrace failing to initialize properly Syringes Adjust Liquid Syringe Check the integrity of the liquid handling syringe drive mechanism Syringes Adjust Air Syringe Check the integrity of the air syringe drive mechanism Valves Check 12 Port Valve Confirm the positioning integrity of the 12 port
84. inge Motors Chattering Sound 117 Syringe Stalls 119 Uneven Volumes in Elution Containers 121 Valves Leaking 119 Water Coming Off with Eluent 123 Wrong Liquid Volumes Delivered 120 Wrong Solvent Dispensed 119 Wrong Volume from Sample Container 121 123 U Undo Button 78 Uneven Volumes in Elution Containers 121 Unpacking Procedure 11 Use with Columns 98 V Valve Problems 114 Valves Leaking 119 AutoTrace SPE Workstation User s Manual Voltage Conversion 100 120V to 220 240V Conversion 157 220 240V to 100 120V Conversion 158 Power Entry Port 155 Set New Voltage 156 Verify Operation 159 W Waste Containers 11 Waste Drain and Tubing Installation 16 Waste Ports EES anaa 30 Water Coming Off with Eluent 123 Weight Specifications 160 Windows Menu 65 Arrange Icons 65 Cascade 65 OwverlaD AR 65 Tile paaa on ER PBA AN Park AHA 65 Work Area Preparation 12 Workstation Parameters 74 Writing a Method Application Tips 93 Manual Steps 90 Method Example 91 Method Step Considerations 95 Method Steps 95 Sample Recovery Optimization 93 Setup Methods Window
85. ip for instructions on how to correctly lift the workstation WARNING AA At least two people are required to lift the Auto Trace Workstation onto the work area Connect the Solvent Reservoirs To connect the solvent reservoir bottles to the solvent tubing lines on the left side of the workstation 1 Position the reservoir bottles to the left side of the AutoTrace Workstation keeping the following in mind e You must position the reservoirs within reach of the tubing that extends from the left side of the workstation e The most precise liquid transfer occurs with the solvent reservoirs positioned slightly higher than the workstation s 12 port valve Dionex recommends that you do not place the solvent reservoirs on the top of the workstation NOTE L You must provide up to five suitable containers for your solvents The supplied plastic bottle should only be used for water Do not use the bottle for solvents or plastic may appear in your chromatogram 2 Uncap the solvent reservoirs and fill them with the required solvents 3 Remove the tubing weights and barbed fittings from the Startup Kit 4 Insert the end of the tubing from solvent port 1 through the hole in one of the reservoir caps Cut the tubing length if necessary to avoid slack or kinks in the solvent lines 5 Push the tubing end through the small hole in the top of one of the tubing weights until the tubing extends through the opposite end as shown in
86. iver blade in the right side of the AC power socket Now push the screwdriver blade to the right to pry the door open 3 Lift and swing the power entry port door outward toward you 4 Hold the fuse block assembly and pull it out from the power entry port housing Select the New Voltage Follow these steps to select a new voltage 1 Using the needle nose pliers grasp the voltage selector card located on the far right of the power entry housing and pull it straight out 2 Orient the voltage selector card so that the numbers indicating the desired voltage are positioned at the bottom of the card as shown in Figure 88 Indicator Pin Q Q aa Q o Q O D O O z z INWNOOHOO R Desired Voltage Figure 88 Voltage Selector Card Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Voltage Conversion 157 Select the New Voltage Continued 3 Move the indicator pin so that it is positioned up when the card is held in the above position NOTE When the Indicator pin is fixed each successive voltage is selected by rotating the card clockwise 4 Reinstall the card in the housing with the printed side of the card facing toward the center of the housing and the pin facing out The arrow on the pin will face the small arrows on the divider to the fuse housing Converting from 100 120V to 220 240V Follow these steps to convert from a single 100 120 volt 3A fuse to dual 220 240 volt 1 6A f
87. ked as possibly corrupt by an incomplete write operation This can occur if an application is closed unexpectedly because of a power outage or computer hardware problem The database won t be marked as possibly corrupt if the application is closed in the usual way Exit Quit the AT program Click the Yes button to close the software If there is any window open in editing mode make sure that you first save the data Methods Menu Selecting Methods from the main menu opens the Setup Methods window This allows you to write a new method and edit values as well as print the method steps and the parameter or solvent settings For more details refer to Writing a Method on page 76 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 60 Serial Op Menu The Serial Op menu contains the options shown in Figure 44 Download Method Download Utility Procedure Figure 44 Serial Op Menu Use the Serial Op menu to download AutoTrace methods and utility methods NOTE u Code 8192 means that the method or utility file downloaded successfully Refer to page 125 for a list of other codes Download Method Downloads an AutoTrace method to the AutoTrace Workstation e If the editing window for methods is open the current method is downloaded to the AutoTrace e If the method window is not open the Find Method window opens Choose the method to download by double clicking it A DOS window opens indicat
88. l Steps 90 Method Setup Parameters 94 Method Step Considerations 95 Mounting New Air Syringes 134 Mounting New Liquid Handling Syringes 130 New Button 77 Next Sample Batch Preparation 109 Nothing Out of Elution Manifold Nozzle 124 AutoTrace SPE Workstation User s Manual O Observing Operation 105 Operation Testing 68 O ring Wear Checks 127 Overview of Installation 11 P Parameter and Solvent Information Additional Information 70 Changing Setup Parameters 72 Changing Solvent Names 75 Default Parameter and Solvent EISE o a AA GG ER NA 69 Default Setup Parameter Entries 70 Default Solvent Names TAO Flow Rates 73 Maximum Elution Volumes 75 Recalling Default Entries 70 SPE Parameters 74 Workstation Parameters 74 Params Button 78 Parts Replacement 116 PAUSE Button 29 101 Pausing Operation 104 Power Entry Port 32 Power Switch 32 Power up 2 ES SS ee 23 Preparing the AutoTrace for Operation 97 Print BUOM 63 2448 os bebe de ema 4 78 Purging Less than Five Solvent Lines 67 Purging Liquid Handling Syringe Solvent LINCS 46 4 45 EE EE TEI 128 Purging Solvent Lines 66 R READY light ii ou ou KA ae iresi 29 Ready Light
89. m GC 17 x 60 mm 4 mL screw cap em ER piston and Liner and Liner Ceramic eee i AA for use with acetic acid and acetone Gas Regulator Output O to 20 psi O to 1 4 bars WARNINGS A e Do not use acetone as a solvent to clean the sample path or rinse the sample container because it is harmful to the sample pumps e Do not run pumps dry Always leave DI water in the sample lines when the workstation is not in use Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Specifications 162 Table 20 lists lengths and volumes for tubing in the AutoTrace Workstation Table 20 Tubing Lengths and Volumes 20 in 51 cm 0 8 mL 20 in 51 cm 0 8 mL Switching valve 34 in 86 cm 1 36 mL SPE cartridge 38 in 97 cm 1 52 mL SPE cartridge Elution station or 24 in 61 cm 0 96 mL elution manifold Sample containers 54 in 137 cm 2 16 mL Switching valve 3 20 in 51 cm 0 8 mL Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Ordering Supplies 163 Ordering Supplies To order more supplies for your workstation use the part numbers listed in Table 21 Table 21 Supplies List mm eng 3 mL O ring Kit 6 071057 3 way Valve Replacement Kit 071058 Glass O ring Kit 6 071074 Liquid Handling Syringe Bag of 5 071075 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Ordering Supplies 164 Table 21 Supplies List Continued Sample input lines column model
90. m for 10 minutes Elute the SPE cartridge with 5 mL of ethyl acetate to collect Elute the SPE cartridge with 5 mL of methylene chloride to collect AutoTrace SPE Workstation User s Manual AutoTrace Method Example Software 91 The following AutoTrace method printout example shows how to automate the manual steps listed on the previous page Dionex AutoTrace Extraction Workstation 2 11 2 Auto Trace Extraction Method Nitrogenous Herbicide Method Step 1 Step 2 Step 3 Step 4 Step 5 2 Step 6 Step 7 Step 8 Step 9 Step 10 8 Step 11 Step 1 Step 13 Step 14 Process six samples using the following method Wash syringe with 2 mL MeOH Condition column with 10 mL of MeOH into SOLVENT WASTE Condition column with 10 mL of MeOH into SOLVENT WASTE Wash syringe with 2 mL of WATER Condition column with 10 mL of WATER into AQUEOUS WASTE Load 1000 mL of sample onto column Rinse column with 10 mL of WATER into AOUEOUS WASTE Dry column with gas for 10 minutes Wash syringe with 2 mL of EtOAc Collect 5 mL fraction into sample tube using EtOAc Wash syringe with 2 mL of MeCl Collect 5 mL fraction into sample tube using MeCl END 1st part of manual step 1 2nd part of manual step 1 manual step 2 manual step 3 manual step 4 manual step 5 manual step 6 manual step 7 a To eliminate all traces of the previous solvent before using the next solvent Doc 0652
91. me delay to increase contact time between solvent and column or disk packing material Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 82 Solid Phase Extract Commands Continued Column Rinse or Disk Rinse To clear the lines before eluting specify a volume and solvent usually DI water to be passed through the column or disk and specify whether the effluent is directed to the solvent or aqueous waste position For more than one solvent repeat this selection as many times as necessary NOTES Doc 065296 01 1 09 Ul In contrast to a CONDITION COLUMN or CONDITION DISK step when a COLUMN RINSE or DISK RINSE step is performed a larger volume of air is used to push solvent through the entire solvent path Therefore it is advisable to use this step to rinse the column or disk with solvent after loading the sample onto the column or disk If the manual method requires a rinse with water without allowing the water to leave the column or disk use a CONDITION COLUMN or CONDITION DISK step rather than a COLUMN RINSE or DISK RINSE step so that a smaller air push is used Always rinse the column or disk aiter sample loading to clear the lines of conditioning solvent before eluting especially if the Air Factor is less than 1 AutoTrace SPE Workstation User s Manual Software 83 Solid Phase Extract Commands Continued Wash Syringe Whenever the next step requires a solvent differen
92. mulation Telnet terminal ID ANSI Backscroll buffer lines C Play sound when connecting or disconnecting Input Translation ASCII Setup Figure 85 Properties Window Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Changing Between Column and Disk Versions 154 6 Click the ASCII Setup button 7 Select the parameters shown in Figure 86 ASCII Setup ASCII Sending DL Send line ends with line feeds Echo typed characters locally Line delay milliseconds Character delay milliseconds ASCI Receiving Append line feeds to incoming line ends Force incoming data to 7 bit ASCII Wrap lines that exceed terminal width Figure 86 ASCII Setup Window 8 Click the OK button 9 At the prompt type DIR 10 The following files should be listed e Zy0s Z0s e BMAT133 BMD for Cartridge version or BMATD103 BMD for Disk version e Method BMD lf ERROR comes up on the screen type DIR again It may take several attempts to communicate If communication still fails check the parameter settings and COM port and try again 11 Close HyperTerminal and reopen the AutoTrace software NOTE UH Only one dictionary file should be listed either BMAT133 BMD or BMATD103 BMD If both files are on the Auto Trace type ERASE to delete all the files Close HyperTerminal and open AutoTrace software Make sure the correct version is listed on the AutoTrace software title bar and download either a utility or
93. n sample loading column rinsing and elution Flow Rate Control Through setup parameters the workstation controls the flow rates of solvent and sample in each solid phase extraction step of the written method Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 27 Standard Operations The standard solid phase extraction operation steps used in a method are described briefly below Conditioning the Column or Use CONDITION COLUMN or CONDITION DISK to Disk pass the solvent through the column or disk and direct the effluent to waste Loading the Sample Use LOAD SAMPLE to pump sample from the sample container to the column or disk for extraction Rinsing the Column or Disk Use COLUMN RINSE or DISK RINSE after loading the sample path and column or disk and direct the effluent to waste Washing the Syringe Use WASH SYRINGE to prewash the liquid handling Solvent syringe with the next solvent of choice to waste Eluting the Sample Use ELUTE TO COLLECT to pass solvent through the column or disk and direct eluent into the collection container Optional Operations These optional operation steps can be used in a method Rinsing the Sample Use RINSE SAMPLE CONTAINER to manually add Container solvent and swirl the sample container before continuing Drying with Gas Use DRY WITH GAS to flow gas through the column clearing the path of residual water Pausing Operation Use PAUSE to delay operation
94. n holders kila Valve 3 Way Draws in air for the air syringe Valve Aqueous Waste Routes aqueous effluent to waste Tubing not shown Solvent Waste Routes sample and solvent effluent to Tubing not waste shown Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 32 Workstation Diagram Right Side View Figure 16 Right Side View Parts and Functions Right Side View 1 Sample Input Lines Connects the workstation to sample containers Power Switch Turns the workstation On and Off Power Entry Port Provides a power connection and holds fuses WARNING A The appliance inlet is the disconnecting device Place the device or equipment in a manner so that the disconnecting device is accessible at all times Exhaust Port Outlet for routing solvent vapors to a suitable vent location Communications Connects the communication cable Port from the AutoTrace Workstation to the PC Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Overview 33 Software Diagram The AutoTrace software diagram is shown in Figure 17 Communication Cable AutoTrace Figure 17 AutoTrace Software Diagram Software Files and Functions Software files and functions are listed in Table 2 Table 2 Software Files and Functions Software CD Files Installs the AutoTrace software on the computer Doc Folder Contains the user s guide Doc 065296 01 1
95. n sample loading and one elution the elution solvent is immiscible in eliminate channeling by performing a DRY WITH GAS step to remove all water from the column you are not drying the column or you must perform a COLUMN RINSE or DISK disk after loading sample RINSE step before elution there is water in your extract increase the pressure and or time of the DRY WITH GAS step the elution solvent is not reaching use a volume of 3 mL or greater in the elution the packing material in the first ELUTE TO SOAK step you need to increase the contact use an ELUTE TO SOAK step before ELUTE time between solvent and packing TO COLLECT material for extraction of analytes Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 96 Table 9 Method Step Considerations Continued you need to keep the amount of use an ELUTE TO SOAK step before ELUTE air introduced between multiple TO COLLECT elution steps to a minimum you need to collect more than the use an ELUTE TO COLLECT 2nd TUBE step to maximum elution volume of your double the collection volume collection container you need to improve throughput decrease times wherever possible you need to improve recovery refer to the Sample Recovery table you need to run a solvent through use a CLEAN SAMPLE PATH step to designate the sample path from sinkers either of the waste positions through the sample lines sample pumps switching valves and Or colum
96. n the screen and the ERROR light comes on at the end of the sample run Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 107 After Running the Method After running your method e Make any necessary procedural changes during method development e Test the changes e Remove the used columns or disks e Prepare to run the next batch of samples e Clean up if done for the day Determine Required Changes Based on the recovery data and operation observations during method development changes may be needed in the AutoTrace SPE method The Elute Flow and Load Flow parameters are usually the most critical settings Refer to the method development guide published by the manufacturer of your SPE columns or disks for additional assistance Also use the AutoTrace online Help and refer to Application Tips on page 93 NOTE u When making changes to optimize the method make them one ata time to evaluate the effect of the change Make the Necessary Changes To make changes 1 Start the AutoTrace software 2 From the AutoTrace main menu choose Methods 3 Press the LOAD button 4 Double click the desired method from the list 5 Close the Find Method window 6 Edit the method 7 After making changes to the method choose Save Method Test the Changes To test the changes run the method to evaluate the outcome of the changes Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Ope
97. nning an AutoTrace SPE Method The front panel controls are displayed in Figure 65 and their functions are described in Table 10 Figure 65 Front Panel Controls Table 10 Front Panel Controls 1 LOAD button Downloads software and a method when held down during power up 2 PAUSE button Stops the workstation after it completes the step it is performing 3 CONT button Continues operation after using the PAUSE button responding to the ERROR light or after manual intervention Also used to start a method or download a method There are two ways in which you can run an AutoTrace method e Pressing the LOAD button when the unit is turned on e Pressing the CONT button for subsequent runs of a previously loaded method LOAD Button Operation To refresh all files on the units CPU board and load a method at power up press the LOAD button This initiates an automatic startup sequence that loads the operating software initializes the workstation and begins running the method Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 102 LOAD Button Operation Continued The workstation s automatic startup sequence that is initiated after pressing the LOAD button causes e The operating files and method to be loaded e The workstation to beep and the front panel display to remind you to check for columns and tubes to check the waste container and prompt you to press CONT to acknowle
98. ns to a designated collection position use a RINSE SAMPLE CONTAINER step to designate either of the waste positions or the For example in a conditioning collection container position step requiring 40 mL of water rather than using four CONDITION COLUMN or CONDITION DISK steps of 10 mL you can save time by using a single 40 mL CLEAN SAMPLE PATH step to aqueous waste Follow with a PAUSE AND ALERT step for moving the lines from the water container to the sample containers Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 97 Operation This section describes the steps involved in operating the AutoTrace SPE Workstation The information is divided into three major topics e Preparing the AutoTrace SPE Workstation for operation e Running the AutoTrace SPE method e What to do after running the method Also see the Method Development Checklist on page 111 and the Daily Operation Checklist on page 112 Preparing the AutoTrace SPE Workstation To prepare the AutoTrace SPE Workstation for operation 1 Turn on the workstation using the power switch located on the right of the unit toward the middle After power up the work station goes through a brief initialization NOTE We recommend that you leave the workstation running unless it will not be used for an extended period of time 2 To perform a DRY WITH GAS or CONCENTRATE SAMPLE method step turn on the gas supply Set
99. oaded Configuring HyperTerminal to Communicate with AutoTrace Parameters In some cases it may be necessary to communicate with the AutoTrace Workstation directly HyperTerminal can be used to reconfigure the software when changing from Column to Disk versions of the Auto Trace If there are conflicting dictionaries that have been downloaded onto the unit HyperTerminal will need to be used to remove the extra files from the AutoTrace HyperTerminal is a Microsoft Windows software accessory typically installed with Windows The user should be familiar with this software to perform the following steps Refer to Microsoft s documentation for information on HyperTerminal 1 Follow the steps in HyperTerminal to set up a new connection by selecting a name and an icon 2 Inthe connect to screen select COM1 The COM1 Properties window opens as shown in Figure 84 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Changing Between Column and Disk Versions 153 3 Inthe COM1 Settings screen select the parameters shown in Figure 84 COM1 Properties Port Settings Restore Defaults o Figure 84 COM1 Properties Window 4 Click the OK button 5 From the main menu select File Properties The Properties window opens as shown in Figure 85 test Properties Connect To Settings Function amow and ctrl keys act as Terminal keys Windows keys Backspace key sends GH Del Cin H Space Ctr H E
100. of trouble with the workstation or if any of the following workstation components have been replaced PC boards tubing valves syringes keypad or column holder Parts The following parts are required to complete this method e Six 16 x 100 mm test tubes and elution rack for optional wet test Sample container with at least 100 mL of water for optional wet test e Solvent containers filled with colored water for optional wet test Running the Benchmark Test Perform the following steps to verify workstation operation 1 Download a Benchmark Test procedure a b C From the AutoTrace main menu choose Serial OP Download Utility Procedure Click the Benchmark Test button Read the online Help for this utility before continuing 2 Press the CONT button twice slowly and follow the prompts on the front panel display to verify that the a b C Doc 065296 01 1 09 Front panel RUN light turns on Front panel ERROR light turns on Elution shuttle moves to its three different positions Exhaust fan turns on Holder s LEDs are lit AutoTrace SPE Workstation Users Manual Maintenance 142 Running the Benchmark Test continued 3 Perform the following wet test whenever tubing valves or syringes have been replaced Follow the display s prompts and do the following Doc 065296 01 1 09 a b e f Place empty tubes in the 16 x 100 mm elution rack Place the workstation s five s
101. olvent lines in containers holding water solutions of different colors Observe that the tubes are filled with water as follows Tube 1 fills with 10 mL from solvent container 1 Tube 2 fills with 10 mL from solvent container 2 Tube 3 fills with 10 mL from solvent container 3 Tube 4 fills with 10 mL from solvent container 4 Tube 5 fills with 10 mL from solvent container 5 Tube 6 fills with 10 mL from solvent container 1 With the gas turned on verify gas valve operation by placing a finger under the elution manifold s nozzles and sensing the gas flow Place all sample lines in a container of water Verify that all pumps direct sample to aqueous waste If you need to repeat the Benchmark Test press the CONT button twice quickly AutoTrace SPE Workstation User s Manual Column Holder Conversion 143 Column Holder Conversion This section describes how to convert a column holder on an AutoTrace Cartridge version unit to work with a different size column Parts To convert your column holder obtain the appropriate plunger assembly for the column size to be converted See Ordering Supplies on page 163 Remove the Plunger Assembly Follow these steps to remove the existing plunger assembly for all column holders to be converted 1 Slide the tubing clamp up so that it is no longer over the stainless steel tubing as shown in Figure 77 fa Teflon Tubing LED Tubing Clamp Stainless Tubing
102. on Users Manual Operation 106 Detecting Errors The AutoTrace operating software detects hardware and system errors Hardware errors pause operation write a message to the display and light the ERROR light System errors pause operation and cause the READY light to flash Error Light Response lf the ERROR light comes on check the front panel display for a message describing the error Correct the error and resume operation by pressing the CONT button Flashing Ready Light Response In the uncommon event of a system error flashing READY light follow the steps below 1 Turn the power off and wait 15 seconds 2 Press and hold the LOAD button while turning the power back on and then release the LOAD button 3 If the condition persists the file may be bad Download the method again 4 lf the condition still persists contact Dionex Technical Support see Contact Us on page 3 Sample Run Completion If the Beeper On parameter is set to YES the workstation beeps every 60 seconds to alert you to the end of the sample run Silence the alarm Press the CONT or PAUSE button Run the same method on Press the CONT button after another batch of samples performing the necessary preparatory steps 1 Exception If a column or disk gets clogged and the sample pump stalls the workstation stops processing that sample but continues processing all others An error message THESE DISK ARE BAD X X X X X X is displayed o
103. on the toolbar to open the Setup Methods window Click the New button In the Name text box type Dry Lines Double click the AutoTrace Method Steps line in the left pane Expand the Solid Phase Extract option double click Load Sample and set the volume to 10 0 mL Double click Dry with Gas and set the time to 0 5 mins Save the method AutoTrace SPE Workstation User s Manual Changing Between Column and Disk Versions 149 10 From the main menu choose Serial Op Download Method choose the Dry Lines method and click Yes when asked to download the method to the Auto Trace 11 Place the sample lines in an empty clean container 12 Run the Dry Lines method 13 When finished turn off the AutoTrace s power and unplug the power cord Removing the Defective Pump 1 One piece at a time unscrew the pump s compression screws and secure the tubing to the front of the workstation with a piece of tape Compression Screws Tubing Figure 81 Pump Front View 2 Remove the screws that secure the rear cover of the workstation Set the rear cover and screws aside 3 Locate the back of the defective pump and follow the pump s wires to the white connector that connects the pump to the wiring harness ii Wiring Harness Connector Figure 82 Pump Back View Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Changing Between Column and Disk Versions 150 4 Squeeze the locking tab on the conne
104. onsiderations for optimizing the automated method Sample Recovery Table 7 describes three areas that can cause unacceptable recovery and should be investigated when optimizing sample recovery Table 7 Sample Recovery Optimization Breakthrough Elution O Internal Loss Conditioning steps Solvent type Sample path Conditioning flow and Solvent miscibility Sample container air push rates Solvent type Solvent volume Solvent volume Elution flow and air push rates a Can be determined by collecting aqueous waste EE manually analyzing it for target compounds b Sample retention still on column or disk c Sample adsorption NOTE L Sometimes sample recovery is optimized at the expense of sample throughput e g slower flow rates and longer times Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Software 94 Setup Parameters Table 8 lists some considerations for setting the parameters in the automated method Table 8 Setup Parameters He IThen you a to improve Sa the flow rate s recovery you need to improve increase the flow rate s throughput the liquid handling syringe decrease the flow rate s Stalls you are using viscous liquids adjust the Push Delay you need to decrease the reduce the Air Factor amount of air between multiple conditioning steps you need syringe washing to disable Autowash and use the appear in your method WASH SYRINGE method steps printout for a
105. or stop operation and signal manual intervention Increasing Absorption Time Use ELUTE TO SOAK before an ELUTE TO COLLECT step to allow sample to soak the column Performing Multiple Elution Use ELUTE TO COLLECT 2nd TUBE or multiple ELUTE TO SOAK or ELUTE TO COLLECT steps as required by the method Cleaning the Sample Path Use CLEAN SAMPLE PATH method steps between sample batches to prevent cross contamination Concentrating the Sample Use CONCENTRATE SAMPLE for automated concentration of the eluent Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 28 Workstation Diagram Front View Figure 14 Front View Parts and Functions Front View Column Disk Holds the SPE columns or disks Holders depending on the workstation s type for the extraction process Elution Station Collects aqueous effluent solvent effluent or sample effluent on the elution station These components are shown in detail in the next view Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 29 4 Front Panel Communicates workstation status to the operator READY Light A steady light indicates power is ON to the unit a flashing light indicates a system error 6 RUN RUN Light Indicates a method is running a method is Indicates a method is running 2 a Light Indicates that operation has stopped due to an error condition 8 LOAD Button Used to download a method from the PC GR ed
106. prior to the next conditioning column or disk rinsing or sample loading step Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 81 Solid Phase Extract Commands Continued Load Sample To load sample onto the SPE column or disk specify a volume of sample to be transferred from the sample container to the SPE column or disk Sample is passed through the column or disk and the effluent directed to agueous waste NOTES e To get the entire sample and or compensate for the pump s 12 596 accuracy adjust the column or disk entry e With samples containing large amounts of solids it is advisable to over pump sample onto the column or disk by 596 to 796 For example if the desired sample volume for the LOAD SAMPLE step is 1000 mL specify 1050 mL e If the sample contains volatile compounds avoid sample evaporation during the conditioning steps by placing a PAUSE AND ALERT step before the LOAD SAMPLE step See a description of the steps below Pause To add a pause in workstation operation select either a timed delay step in minutes or a pause and alert step that signals the operator until the CONT button is pressed Examples PAUSE AND ALERT Use this step to alert the operator for sample container introduction when the workstation is done with the column or disk conditioning This is useful when a sample contains volatile compounds TIMED PAUSE After conditioning this step introduces a ti
107. ps appear on the front panel display during operation but do not appear in the method printout Therefore for auditing purposes we suggest that you turn off Autowash set to zero and use WASH SYRINGE steps where needed Table 5 Workstation Parameters Max Elution Maximum volume that can be eluted onto the collection container for safe handling as Table 6 listed in Table 6 Exhaust Fan On Enable or disable the exhaust fan for solvent Y or N vapor removal during operation Enable or disable the workstation s beeper Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 75 Changing Setup Continued Table 6 Maximum Elution Volumes 17 x 60 mm vial 7 mL IT mm GC val Change Solvent Names To change the solvent names 1 From the AutoTrace main menu choose Data Name Solvents The Edit Solvent Sets window opens as shown in Figure 57 Edit Solvent Sets E od TY RR Save Undo Delete Print Help Close Set name Standard Solvent No Nomenclature Solvent 1 Solvent 2 Solvent 3 Solvent 4 Solvent 5 Figure 57 Edit Solvent Sets Window 2 Select one item in the list of the available solvent sets on the left side and then click the Edit button or click the Add button to create a new solvent set Each solvent set can be named Set name and has five solvents Up to 25 characters are allowed for the Set name Use the arrow keys to move to the field that requires changing
108. rameter is set to YES and the front panel displays a message prompting that an action is required Table 11 lists the front panel messages NOTE Ul The Disk version of the Auto Trace Workstation will display Disk instead of Column in the messages Table 11 Front Panel Messages Method Step Front Panel Display Rinse Sample RINSE SAMPLE Container CONTAINER WITH xx ML PRESS CONT TO RESUME Elute to Collect SECOND ELUTION STEP 2nd Tube REPLACE TUBES WITH NEW TUBES PRESS CONT TO RESUME Concentrate CONCENTRATION STEP Sample PLACE EMPTY COLUMNS IN THE HOLDERS PRESS CONT TO RESUME Clean Sample TO CLEAN SAMPLE PATH Path PLACE SAMPLE INPUT LINES INTO A BREAKER PRESS CONT TO RESUME Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 104 Table 11 Front Panel Messages Continued Method Step Front Panel Display Pause and Alert SYSTEM PAUSED PRESS CONT TO RESUME When you complete the manual steps press the CONT button so the workstation can proceed running the method Pausing Operation To pause the method at any time press the PAUSE button The workstation stops and pauses after it completes the operation it was performing when the PAUSE button was pressed Continuing Operation To resume the method from where it paused press the CONT button Aborting If you do not wish to continue workstation operation abort the operation as follows 1 Turn the power off
109. ration 108 Removing Used Columns Remove the used columns see Figure 67 by sdueezing the holder s lever and clip together to release the column from the holder N Figure 67 Column Holder Side View WARNING A Never leave the column holders in the down position without the columns in place because this can deform the O ring Removing Used Disks Remove the used disks by unscrewing the locking collar see Figure 68 squeezing the clip and moving it up toward the lever and sliding the holder up Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Operation 109 Removing Used Disks Continued lever pp Clip Locking Collar gt gt Figure 68 Disk Holder Side View Next Sample Batch Preparation Unless the last steps of the method were CLEAN SAMPLE PATH steps you need to clean the sample lines between batches of samples 1 Place an empty column or disk in each holder and make sure each holder is in the fully down position with the holder LED on 2 Download the Clean Sample Path method that was saved to the database 3 When the workstation pauses the first time insert the sample lines into a clean container filled with a solvent Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 110 Next Sample Batch Preparation Continued WARNING A Do not use acetone as a solvent to clean the sample path because it is harmful to the sample pumps 4 Daily
110. rsion 159 Verify Operation Follow these steps to verify a successful voltage conversion 1 Plug the AC power cord into an AC power outlet WARNING A Only plug the AC power cord into a properly grounded outlet Only use a standard IEC 320 style power cord appropriate for your country 2 Turn the workstation on 3 Verify that the READY light on the workstation s front panel is on Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Specifications 160 Specifications Table 19 lists the specifications for the AutoTrace Workstation Table 19 Workstation Specifications 23 in 57 cm wide x 25 in 63 5 cm deep x 27 in 69 cm high 12 in x 14 in 30 x 36 cm 150 Ibs 68 1 kg 100 120 220 or 240 V 10 150 VA maximum Liquid Management Air Syringe One 10 mL air syringe Liquid Handling One 10 mL liquid handling syringe Syringe Solvent Reservoir 1 liter 2 total supplied 10 liter 2 total supplied Solid Phase Extraction SPE Columns 1 mL syringe compatible columns 3 mL syringe compatible columns 6 mL syringe compatible columns 6 mL glass syringe compatible columns 8 mL glass syringe compatible columns Column Plunger Adapters available for four column types Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Specifications 161 Table 19 Workstation Specifications Continued Collection Container Tube Racks 16 x 100 mm stainless steel Racks Vial Racks 11 m
111. s user name User ID Password user type and access rights This menu option is available only if your user type corresponds to Administrator _ Setup User Data D g X Add Edit Delete Help Close Hame Diones Service Administrator User ID ADMIN Password f Readonly Access CU User Print allowed CU Service O Write allowed fe Administrator fe White Delete allowed lt User Diones logged on Figure 51 Setup User Data Window To change the user type choose the user type in the User Type box on the left After choosing the user type the corresponding tab on the right switches to User Service or Administrator User Manage methods parameter and solvent settings serial operations and diagnostics Service Manage additional command seitings in the Setup Commands menu option Administrator Manage additional user data The access rights for the user type are displayed on the right of the Setup User Data window e Read only mode e Print mode e Write mode e Delete mode Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 65 Windows Menu Help Menu The Windows menu contains the options shown in Figure 52 Cascade Overlap Horizontal Overlap Vertical Arrange Icons Figure 52 Windows Menu Cascade Stack and overlap the windows diagonally Cascade allows the entire top window to be visible but only the title bars of the remaining windows are visible
112. t equal to their corresponding flow rate For example if the Rinse Flow rate is set to 18 set Rinse Air Push to the same Then if either can be increased for better throughput without negative effects your final Air Push rate may differ from its corresponding flow rate e This parameter is useful when transferring viscous liquids Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 74 Changing Setup Continued Values shown in Table 4 are for both the Column and Disk versions of the AutoTrace Workstation unless otherwise specified Table 4 SPE Parameters Air Factor Sets the distance that liquid is pushed 0 3 to 5 0 Cartridge beyond the 12 port valve in version CONDITION COLUMN or 0 0 to 5 0 Disk version CONDITION DISK and ELUTE TO SOAK method steps 2 Autowash Vol Allows the workstation to automatically O to 10 zero turns prewash the liquid handling syringe Autowash Off with the next solvent during operations such as CONDITION COLUMN or CONDITION DISK RINSE COLUMN or RINSE DISK and ELUTE f a Reduce this factor to decrease the amount of air between multiple conditioning steps b Increase this factor to advance solvent and avoid soaking of the column c Alternative Place a WASH SYRINGE step in the method where needed d When going between immiscible solvents in your method use the WASH SYRINGE method step with an intermediate solvent e Occurrence of Autowash ste
113. t from the previous step perform this operation Specify a solvent and volume to be used to wash the liquid handling syringe NOTES e Atleast 2 mL of solvent is a recommended starting point e Alternative Use the Autowash feature instead For details see the description in Setup Parameters on page 94 e You must insert a WASH SYRINGE step with an intermediate solvent when going between steps that use immiscible solvents even if Autowash is being used For example Rinse column with 10 mL of water into aqueous waste Added Wash Syringe Step 5 Wash syringe with 2 mL of isopropyl alcohol Wash syringe with 2 mL of MeCl or by Autowash Collect 5 mL fraction into sample tube using MeCl Dry With Gas To eliminate residual water specify a time period in minutes during which gas passes from an external source through the SPE column This is important when the elution solvent is not miscible in water NOTES e Arecommended time is 15 minutes at 10 psi 0 7 bars using Zero grade nitrogen with an in line scrubber Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 84 Solid Phase Extract Commands Continued e This step is also used in Creating a Method to Clean the Sample Lines with Solvent and DI Water on page 68 to clean the sample path between batches of samples The DRY WITH GAS step removes the liquid from the lines between the switching valve and column leaving only water in
114. the CONT button Descriptions follow of the error messages displayed on the AutoTrace Workstation s front panel display Front Panel Error Message An example error message displayed on the front panel is shown below Messages that appear for method steps and require manual intervention are described in Front Panel Display Messages on page 103 Message METHOD FILE DID Download the method from the PC NOT APPEND CORRECT THE PROBLEM PRESS CONT TO RESUME THESE DISK ARE BAD Inspect the columns or disks for XXXXXX plugging Inspect sample pumps for correct operation Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Diagnose Problems 114 AutoTrace Diagnostics The Diagnostics menu option in the AutoTrace software contains diagnostic routines that can be downloaded and run on the workstation If there is a need to test adjust or replace AutoTrace components and an AutoTrace diagnostic method needs to be run refer to the Downloading and Running an AutoTrace Diagnostic Method on page 115 Diagnostic List The tables below list when various diagnostics are useful Consult the Diagnostics online Help windows for the current selections and most up to date information and recommendations on how to save run repeat and advance when using the diagnostic facility NOTE H You must read all online Help information before running any Auto Trace diagnostic Table 12 Diagnostic List ma When
115. the AutoTrace Cartridge version Place columns in each holder to be used by sliding a column upward onto the bottom of the column holder s plunger Push down on the lever until the assembly clicks into place and the holder s LED comes on See Figure 62 For the AutoTrace Disk version Place disks in each holder to be used by opening the disk holder by unscrewing the locking collar squeezing the clip and moving it up toward the lever and sliding the holder up Push down on the lever until the assembly clicks into place and the holder s LED comes on See Figure 63 AutoTrace SPE Workstation Users Manual Operation 99 Preparing the AutoTrace SPE Workstation Continued O LED Lever Plunger Column Figure 62 Column Holder Front View LED MT 7 oy a Locking Collar Figure 63 Disk Holder Front View Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 100 Preparing the AutoTrace SPE Workstation Continued 10 Place a sample container in each rack position to be used and insert the sample line with tubing weight into the appropriate container Each sample line and each rack position is numbered to correspond to the numbered positions on the right side of the AutoTrace Workstation as shown in Figure 64 Sample Rack Figure 64 AutoTrace Workstation Right Side and Sample Rack Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 101 Ru
116. the pressure no greater than 100 psi 6 9 bars The gas supply should have sufficient reserve for the sample run 3 Adjust the workstation s output gas pressure to the proper setting for running the method A recommended operating setting is 10 psi 0 7 bars Adjust the gas pressure using the regulator knob provided on the left side of the unit 4 Check that the solvent reservoirs are full and the tubing is fully submerged in reservoirs use the tubing weights provided 5 Check that all waste containers side port elution station solvent and elution station aqueous waste are empty 6 Download the Purge Solvent method or run your customized purge method see Customizing a Method to Purge Less than Five Solvent Lines on page 67 The method draws a sufficient amount of solvent from each port to prime the liquid lines Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Operation 98 Preparing the AutoTrace SPE Workstation Continued 7 Place a collection container in each elution rack position Install the elution rack onto the two pins on the front of the elution station NOTE n The rack is symmetrical and can be positioned either way 8 Optional Step When using the AutoTrace Cartridge version Doc 065296 01 1 09 manually rinse the columns with MeCl or water This prevents leakage around the column holder O ring due to the presence of packing debris on the inside walls of the SPE column For
117. the sample lines before the switching valve Clean Sample Path Use this selection at the beginning of the SPE method at the end of the SPE method or in a method of its own to flush and prime the sample lines and pumps between sample batches Specify a volume and an effluent waste position of either aqueous waste or solvent waste NOTES e The CLEAN SAMPLE PATH step should be selected at least twice When the first CLEAN SAMPLE PATH step runs the workstation pauses to place the sample lines into a beaker containing the elution volume The workstation then pauses again to place the lines into a beaker of water when the second CLEAN SAMPLE PATH step runs e Itis advisable to use CLEAN SAMPLE PATH steps in a separate method that is run between sample batches and at the end of a day See Creating a Method to Clean the Sample Lines with Solvent and DI Water on page 68 If you prefer use the steps from the method disk as the last steps in the method instead WARNING A Do not use acetone as a solvent to clean the sample path because it is harmful to the sample pumps 1 Ifan intermediate solvent is required between the elution solvent and water insert a third CLEAN SAMPLE PATH step using this solvent between these two steps Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Software 85 Solid Phase Elute Commands The Solid Phase Elute commands found on the left side of the Setup Methods window specif
118. the syringe plunger and prepare the syringe for removal in the next method 1 From the AutoTrace main menu choose Diagnostics 5Syringes Adjust Air Syringe and download the Adjust Air Syringe diagnostic as described in AutoTrace Diagnostics on page 114 2 Press the CONT button twice slowly Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 133 Remove the Defective Syringe To remove the defective syringe 1 Loosen the knurled knobs on both sides of the syringe clamp Pivot the open end of the syringe clamp out of the way as shown in Figure 72 Knurled Knob Luer Lock Fitting snrome AA T End Piece Housing Tab aq Syringe Clamp Syringe Plunger Driving Arm gs Thumbscrew gt gt Figure 72 Syringe Clamp Knurled Knobs 2 Remove the black thumbscrew from the bottom of the syringe plunger 3 Gently slide the syringe assembly out of the housing 4 Loosen the Luer Lock fitting between the tubing and the syringe by turning the lower fitting counterclockwise approximately 1 2 turn Now turn the syringe and remove it from the fitting Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 134 Mount the New Syringe To mount the new syringe 1 Insert the Luer Lock fitting into the chrome end piece of the new syringe and turn the fitting clockwise until secure Align the grooves in the chrome end piece with the tabs in the housing Gently pus
119. tion s side door and locate the white compression screws on the 3 way valve 12 port valve switching valves and syringes as shown in Figure 13 Switching Valves Compression Screw pi i By Bs Bu Bu Li 12 Port Valve ma 3 Way Valve Figure 13 AutoTrace Left Side View 2 Make sure each screw is finger tight 3 Perform the same check for the compression screws on the pumps and column holders on the front of the workstation Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 23 Power Up the Workstation To power up the workstation 1 Plug the AC power cord securely into the receptacle on the right side of the workstation Plug the 3 pronged end of the power cord into an appropriate AG power source WARNING AA 3 Only plug the AC power cord into a properly grounded outlet Only use a standard IEC 320 style power cord appropriate for your country The AutoTrace Workstation does not require a dedicated AC line However you should provide a clean AC source similar to one used for computers and other equipment A UPS is recommended where power outages or brownouts frequently occur see ordering information in Ordering Supplies on page 163 Turn on the Auto Trace Workstation Computer Access While a computer is not required for AutoTrace control you must have access to a computer to write AutoTrace methods and download AutoTrace methods The computer must have th
120. tor Gas Nitrogen Manifold 12 Port Air Valvef Verslag aa A j M Volume according to Air Factor setting f 8 default of O for disks De Volume according to solvent volume for condition step EEEE Solvent 1 sakin Solvent 2 q as olven Air ide Sain Solvent 5 Handling Waste Syringe Figure 20 Condition Column Liquid Handling and Air Syringes Fill Diagram AutoTrace SPE Workstation Users Manual Continued 12 port valve switches to the switching valve Liguid handling syringe dispenses conditioning solvent See Figure 22 Continued Overview 37 Figure 21 Condition Column Liquid Syringe Dispenses Solvent Flow Chart Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Overview 38 Solvent EE Air Par Gas SPE Column 1 A Switching i Valve 1 l pr Incoming Ss f Sample Sia 1 NN Aqueous or Solvent A Waste Waste A Regulator N I Nitrogen Manifold A 12 Port Valve lee TE Solvent 1 sa Solvent 2 saa a Solvent 3 Air Syringe Li Sp Handling Waste Syringe Figure 22 Condition Column Liquid Syringe Dispenses Solvent Diagram Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Doc 065296 01 1 09 Overview 39 Air syringe pushes conditioning solvent through switching valve and into column See Figure 24 for air push with Air Factor of 1 0 See Figure 25 for air push with Air Factor
121. ubing to extend from the workstation s left or right side and then orient the waste drain s hose fittings to the appropriate side Install the waste drain onto the elution station s two ball studs making sure the waste drain snaps into place and sits flush on the base plate as shown in Figure 6 Ball Stud a Base Plate Figure 6 Ball Stud and Base Plate 3 Push the waste drain toward the back of the workstation It only moves about 1 8 in 3 mm This correctly positions the drain under the manifold Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Installation 17 Install the Waste Drain and Tubing Continued 4 Locate and remove the two 3 ft 0 9 m pieces of waste tubing with caps provided in the Startup Kit One is used for water waste the other for solvent waste 5 With one hand supporting the waste drain install the water and solvent waste tubing onto the drain s hose fittings as shown in Figure 7 Water Waste Tube rear drain Solvent Waste Tube front drain Figure 7 Waste Tubing Connections 6 Route the two waste lines as follows a Connect the cap of the solvent waste tubing the tubing connected to the front drain trough to one of the supplied waste containers making sure the waste container tubing never drops below the level of the waste container cap b Connect the cap of the water waste tubing the tubing connected to the rear drain trough to the remaining waste container making
122. uditing purposes where needed a When using an Air Factor less than 1 always perform a COLUMN RINSE or DISK RINSE after loading the sample Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 95 Method Steps Table 9 lists some considerations for designating the steps in the automated method Table 9 Method Step Considerations Wes ooo the sample contains volatile introduce samples to the workstation only when compounds ready for them by placing a PAUSE AND ALERT step between conditioning and loading steps the manual method requires a use a CONDITION COLUMN or CONDITION rinse with water step without DISK step rather than a COLUMN RINSE or allowing the water to leave the DISK RINSE step so that a smaller air push is column or disk used you need an extended contact introduce a TIMED PAUSE step time between solvent and packing material the sample contains a large add 5 to 7 to your volume entry for the amount of solids LOAD SAMPLE step you are going between immiscible perform a WASH SYRINGE step with an solvents in the method intermediate solvent before performing the next step even if Autowash is being used you need syringe washing to disable Autowash and use WASH SYRINGE appear in your method printout for method steps where needed auditing purposes you are running with the Air you must perform a COLUMN RINSE or DISK Factor parameter set to less than RINSE step betwee
123. urge the solvent lines Load the elution rack Optional Clean the columns or disks Load the SPE columns or disks Load the sample container rack Run Your Method Q m m Load the method or press the CONT button to rerun a method on a different batch of samples Intervene as required Press the CONT or PAUSE button to silence alarm for end of run After Running the Method m m E Doc 065296 01 1 09 Remove the used columns or disks Prepare to run the next batch of samples by cleaning the sample lines If done for the day clean up by emptying the waste reservoirs and flushing the solvent and sample lines AutoTrace SPE Workstation Users Manual Diagnose Problems 113 Diagnose Problems This section of the manual describes how to diagnose AutoTrace Workstation problems This information is divided into e Error Messages e AutoTrace Diagnostics e Troubleshooting Guide If you have any additional duestions about diagnosing workstation problems contact Dionex Technical Support see Contact Us on page 3 When calling please have the information recorded in the front of the manual ready for the Technical Support Representative Error Messages Hardware errors pause operation write a message to the front panel display and light the ERROR LED If the ERROR LED comes on look at the front panel display for a message describing the error After correcting the error resume operation by pressing
124. uses 1 Remove the single 100 120V fuse as shown in Figure 89 100 120V Fuse Fuse Block Figure 89 100 120V Fuse Removal 2 Invert the fuse block and install the two 220 240V fuses into place as shown in Figure 90 220 240V Fuse 220 240V Fuse Fuse Block P Figure 90 220 240V Fuse Installation Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Voltage Conversion 158 Converting from 100 120V to 220 240V Continued 3 Slide the fuse block assembly into the power entry port housing and snap it into place 4 Change the voltage on the voltage selector card 5 Close the power entry port door and verify that the indicator pin shows the desired voltage Converting from 220 240V to 100 120V To convert from dual 220 240 volt 1 6A fuses to a single 100 120 volt 3A fuse do the following 1 Remove the dual 220 240V fuses as shown in Figure 91 220 240V Fuse 220 240V Fuse Fuse Block d Figure 91 220 240V Fuse Removal 2 Invert the fuse block and install the single 100 120V fuse into place as shown in Figure 92 100 120V Fuse Fuse Block Figure 92 100 120V Fuse Installation 3 Slide the fuse block assembly into the power entry port housing and snap it into place 4 Change the voltage on the voltage selector card 5 Close the power entry port door and verify that the indicator pin shows the desired voltage Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Voltage Conve
125. valve Valves Purge Solvents Prime or drain the liquid lines Login Logout Menu The Login Logout menu contains the options shown in Figure 46 Login Logout Figure 46 Login Logout Menu Login Register as a user with access rights given by the system supervisor Selecting Login from the menu opens the User Identification window see Figure 47 Type a User ID and Password and then click the OK button The default User ID is ADMIN and the default password is ADMIN Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 62 Login Logout Menu Continued User Identification User ID Password Change Figure 47 User Identification Window If the registration is successful your User ID displays in the status bar at the bottom of the window Change Password To change a password open the User Identification window and click the Change button The Change Password window opens as shown in Figure 48 Type the old password the new password repeat the new password and click the OK button Change Password Old Password New Password Repetition EE Figure 48 Change Password Window Logout Log out of the software by selecting Logout from the menu Your access rights are changed to READ ONLY mode The status bar shows No user logged in Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 63 Data Menu The Data menu contains the options shown in F
126. y Not Used for any solvent ports that do not have solvents connected These names appear in a selection list whenever you write a method step requiring solvent The name of the selection appears in the method step display and printout Recalling Default Entries You can recall global default entries at any time by pressing the Default button on the Setup Parameters window that is accessed from the Data menu Global default parameters include flow rates SPE parameters and workstation parameters See Figure 55 1 Contact the column or disk manufacturer for their recommended flow rates Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Software 71 Recalling Default Entries Continued Setup Parameters g a Edit Default Print Help Last Change 271672001 9 05 35 AM SPE Parameters Flow Rates Push Delay Ai Factor Cond Flow 15 0 ml min Aubomash Vol Load Flow 10 0 ml min Rinse Flow 20 0 miEmin Elute Flow 5 0 ml min Cond Air Push 15 0 ml min Rinse Air Push 20 0 ml min Mas Elution Wol 12 0 ml Elute Air Push AA mlAmin Exhaust Fan On Workstation Parameters r 7 Beeper On User Dionex logged on Figure 55 Global Setup Parameters Window NOTE n This window is not the same as the local Setup Parameters window which contains parameters that are local to the specific method that can be opened from within the Setup Methods window The Default button does not appear on the
127. y the steps that perform and follow sample elution The solid phase elute menu is shown in Figure 61 An example method is provided in Method Example on page 90 Solid phase elute Elute to soak Elute to collect Elute to soak nd tube Elute to collect nd tube Pause and Alert Timed Pause Clean sample path Finse sample container Concentrate sample Wash springe Figure 61 Solid Phase Elute Menu NOTE u Before eluting perform a COLUMN RINSE or DISK RINSE or DRY WITH GAS step to clear the lines Elute to Soak Soak the column or disk with elution solvent or perform multiple elution steps with a minimal air push between them Specify the solvent and volume to be introduced onto the column or disk with any eluent directed to the collection container NOTES e Soaking the column or disk sometimes helps in the extraction of analytes by increasing the contact time between solvent and packing material therefore maximizing elution efficiency e Using a minimum amount of air when performing multiple elution steps prevents column or disk drying Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Software 86 Solid Phase Elute Commands Continued e Fora single ELUTE TO SOAK step or for the first of multiple ELUTE TO SOAK steps use a solvent volume of at least 3 mL to ensure that the elution solvent reaches the column or disk packing material The tail end of the elution solvent is positioned in the flow path
128. you want to Run the diagnostic Syringes Check the integrity of Adjust Liquid Syringe the liquid handling syringe drive mechanism Check the integrity of Adjust Air Syringe the air syringe drive mechanism Valves Confirm the positioning Check 12 port valve integrity of the 12 port valve WARNING A Do not run the valves diagnostic if the solvent lines have not yet been purged Prime or drain the liquid Purge Solvents lines Doc 065296 01 1 09 AutoTrace SPE Workstation Users Manual Diagnose Problems 115 Table 12 Diagnostic List Continued MEN When you want to Run the diagnostic Initialization Diagnose the reason for Initialization an AutoTrace failing to initialize property a In most cases writing your own purge method does a better job of purging the lines A customized purge routine can save time and conserve solvent Downloading and Running an AutoTrace Diagnostic Method To download a diagnostic and run it on your workstation 1 From the AutoTrace main menu choose Diagnostics 2 Select the appropriate diagnostic from the listing NOTE Press the F1 key to access online Help and get detailed information about the diagnostic selected 3 The diagnostic is automatically downloaded to the AutoTrace workstation When you want to Perform this action Run the diagnostic Press the CONT button twice slowly 2 seconds between presses Repeat the diagnostic Press the
129. yringe drive mechanism is operating correctly 136 Doc 065296 01 1 09 AutoTrace SPE Workstation User s Manual Maintenance 137 Replacing Fuses This section explains how to replace the fuse s in the workstation s power entry port The port is located on the right side of the unit The method applies to single North American or single dual international fuse configurations Parts and Tools The following parts and tools are required to complete this method Two 1 6A 220 240V fuses or one 3A 100 120V fuse Small flat blade screwdriver Refer to Figure 75 as required Power Entry Port Housing pi Fuse Fuse Block Assembly Figure 75 Fuse Replacement Details Remove the Fuse Block Assembly Follow these steps to remove the fuse block assembly NOTE u Power off the Auto Trace and unplug the AC power cord before beginning this method 1 2 Doc 065296 01 1 09 Turn the workstation s power off and unplug the AG power cord Using the small screwdriver place the screwdriver blade in the right side of the AC power socket Now push the screwdriver blade to the right to pry the door open Swing the power entry port door outward toward you Hold the fuse block assembly and pull it out from the power entry port housing AutoTrace SPE Workstation User s Manual Maintenance 138 Replace the Fuse s Follow these steps to replace the fuses 1 Remove the fuse s from the fuse block assembly 2 Pr

AutoTrace SPE Workstation User`s Manual

Contents

Download Pdf Manuals

Related Search

Related Contents