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SD-1 User Guide - Chemical Instrumentation Facility

1. D v 5 oZ 2 2 ka ejg lo S o amp lc lo r Ed D S a O oj SjS o 2 elols lt C on o SJE e x Oo oO ols clGlSlEl2 Jolsls lt olev S e le ISBlElsifSleisla fsisis siz ciales g l fe DIEISI2 Zlfol S 2 Blo Ele Sle ls 5 5 3 5 S F o B 8 2 o s o o S ZI2 S o o ClElSlelSlSlelalslSlelelelSlelSlelflelflelclelFis Zlelsl lo CIDISIPI SIL fo lolLlLislslalMl_ IS ISIS ZSIS IBIS lL lICiSiSlolelalc SISISINSI S 5 fSlS e lL lals S GIZIZIS S L Llslslolela CIZEILSC ONSIS ElEIS ZIZ19 exa IRIE lee IS 5 S Jo jale 8 8 8 o 5 ls E ISSIS Sl ElE ISIE IE to 15 2 2 Ols lolz S lS ole SS lt lt lt A la lO lo SA l i a T T2 ZZ A 2 Aa Ee EEEE Figure 30 Solvent miscibility of some common solvents 142 SD 1 Purification Solution System Manual Appendix 6 The Waste Electrical and Electronic Equipment Directive Abstract The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC adopted by EU Commission on 13 February 2003 is introducing producer responsibility on all electric and electronic appliances starting with 13 August 2005 This product complies with the WEEE Directive 2002 96 EC marking requirements The affixed label indicates that you must not discard this electrical electronic product in domestic household waste Product Category With reference to the equipment types in the WEEE Directive Annex I this product is classed as a Monitoring
2. OO0OO0O000000000 OOOOQOQ00Q000000 OOO0O000000000 OO0OO0000000000 OOOO0O00000000 Front of the fraction collector Figure 21 Tube positions on the fraction collector SD 1 Purification Solution System Manual 91 3 Installation Connecting the Power to the Fraction Collector Connecting the Power to the Fraction Collector The connection panel of the Agilent 440 Fraction Collector G9340A is located on the pillar also called a control column The panel contains an I O port indicators DIP switches the power socket and switch and a RS 232 port for communication between the Agilent 440 Fraction Collector G9340A and the system or computer that is running instrument control software Error indicators eset button 1 0 port Relay status dicators showin i GS statu of relays Which are AB ana aun hardwired P circuit oard Console software configuration ov m Status indicators A Auxilliary a communication port S 77 not supporte Instrument ure communication port Power Supp ply inlet switch and fuses Figure 22 Connection panel Prerequisites Three power cables are supplied with the module Select the correct one for your location 92 SD 1 Purification Solution System Manual Installation 3 WARNING Electrical shock Electrical power for the module must be provided through a three wire outlet with ground connection The outlet must be rated for at least 75 VA
3. SD 1 Purification Solution System Manual Installation Installing the Fraction Collector Installing the Fraction Collector Overview of the Module i a 2 10 mo Eo i Eert l Back 3 11 SH 7 all 9 y Figure 18 Fraction collector components 3 1 Theta axis 2 Z axis slide 3 Top knurled mount nut on the probe assembly 4 Probe mounting block 5 Lower knurled mount nut on the probe assembly SD 1 Purification Solution System Manual 83 3 Installation 6 Nut holding the metal probe 7 Probe 8 Rack 9 Rack location mat 10 Split retaining ring 11 Fraction collector pillar control column Installation Overview Basic installation involves e Assembling the fraction collector Connecting the fraction collector to the HPLC system Installing Agilent OpenLAB CDS ChemStation PrepLC Drivers e Determining the delay volume and probe depth All external DIP switches should always be in the OFF position Assembling the Fraction Collector Carefully follow the instructions provided below to assemble your instrument Assembling the Agilent 440 Fraction Collector includes installing the 1 Spill tray 2 Rack location mat 3 Probe and tubing 4 Sample racks Position the fraction collector on the side of the HPLC system closest to the detector output to help decrease the delay volume 84 SD 1 Purification Solution System Manual Installation 3 Installing the F
4. gt Ensure that power receptacles are earth grounded at the grounding pin Ensure that the probe arm s movement is not interfered with during operation initialization Ensure that the power switch is turned off 0 Plug one end of the power cable into the module both the switch and the power socket are located on the connection panel on the pillar and the other into the mains power outlet In some countries it may be necessary to fit a suitable three pin power plug to the cord A three pin earthed power outlet must be used Ensure the module is always connected to the mains supply protective earth Turn on the module The module will go through initialization tests and set the probe position If the initialization process is not successful refer to chapter Troubleshooting and Diagnostics in Agilent 440 Fraction Collector User Manual G9340 90000 If the fraction collector does not start up check each fuse as described in chapter maintenance in Agilent 440 Fraction Collector User Manual G9340 90000 During the initialization sequence 1 2 The probe rises to the full extreme of the Z axis The probe travels to the full extremes of the X axis and rotates to the full extremes of the Theta axis Then the probe is positioned at the front left of the fraction collector SD 1 Purification Solution System Manual 93 3 Installation Instrument Communication Port The instrument communication port see Figur
5. 10 After the wash solvent tubing and the syringe are filled press WASH to perform a standard wash routine Repeat the wash routine 2 or 3 times All tubing connected to the syringe valve will be rinsed with wash solvent The autosampler will give the best results if all air is removed from the syringe Connecting to the Autosampler To ensure reproducible injections the following connections to your HPLC system should be made 1 Connect the HPLC pump to port 1 of the injection valve 2 Connect the HPLC column to port 6 of the injection valve 3 Check for leakage and let the system equilibate for at least 5 min The instrument is flushed with Isopropanol Make sure that the mobile phase of your HPLC system is miscible with Isopropanol If your mobile phase is not miscible with Isopropanol then start with an intermediate solvent that is a transition to the mobile phase To avoid possible contamination of the column it is good practice to not have the column installed during this operation It is essential that the contents of the sample loop are injected as a back flush onto the column therefore do not exchange column and pump connections at the injection valve 80 SD 1 Purification Solution System Manual Installation 3 Filling and Sealing the Vials 1 Fill the standard vials as well as the conical vials by means of a narrow end pipette to allow air to escape when filling the vial Do not fill vials completely to the top In
6. 2 Make sure to check carefully for all miscellaneous components that might be contained in the inner compartments The detector is a sensitive instrument and should always be handled with the degree of care appropriate for laboratory instrumentation Keep the shipping carton as it provides excellent protection if you have to transport or store the detector in the future SD 1 Purification Solution System Manual 33 3 Installation Unpacking the Autosampler CAUTION Risk of damaging the autosampler gt Do not lift the Agilent 410 Autosampler by the front cover 1 Lift the Agilent 410 Autosampler as shown in Figure 1 on page 34 with both hands under the instrument or with one hand under the front and the other hand grasping the rear top of the Agilent 410 Autosampler Figure 1 Agilent 410 Autosampler lifting instructions 34 SD 1 Purification Solution System Manual Installation 3 Unpacking the Solvent Delivery System WARNING Danger to hands and feet The instrument is heavy gt Always use a fork lift or other suitable lifting device when moving the instrument CAUTION Overheating of the pump Objects interfering with airflow to the pump gt Maintain at least 15 cm 6 inches clear space next to the fan SD 1 Purification Solution System Manual 35 3 Installation Unpacking the Fraction Collector Prerequisites Ensure there is enough room on the bench for the fraction collector WARNI
7. Example IP address 192 168 0 97 SD 1 Purification Solution System Manual Installation 3 Setup the Software F r Detector Configuration Instrument 1 Detector Configuration Instrument 1 IP address 0 0 0 0 IP oddress 192 168 0 97 Activate communicaton ___Aatwvate communication Options Options Dual wavelength option Enabled Dual wavelength option Enabled Cel type so x Cel type s0 Enable ready in Enable ready in ooo i 7 ok Cae Hep j 0K Cano Hep 3 Verify the connection by clicking on Activate communication Information Communication established with COM1 is visible on the screen 4 Click OK Configuration dialog closes Fraction Collector Configuration 1 Doubleclick in Configurable Modules on Fraction Detector Fraction Collector Configuration dialog opens SD 1 Purification Solution System Manual 107 3 108 Installation 2 Select the COM Port as COM 2 Yi Fraction Collector Configuration Instrument 1 comro Activate communication Serial number AY1101M015 Flow settings Volume delay Rack and tube settings Rack type Probe depth Max tube time g Communication established with COM2 ampas eo ee Help 4 3 Fill in the Flow settings and the Rack and tube settings 4 Verify the connection by clicking on Activate communication 5 Verify the connection by click
8. Isocratic Pump Stainless Steel Tubing Kit 1 16 x 0 03 i d Isocratic Pump Stainless Steel Tubing Kit 1 16 x 0 04 i d Isocratic Pump Stainless Steel Tubing Kit 1 8 x 0 08 i d In addition a Technical Note with installation instructions is included Delivery Checklist User Documentation CD Part of a standard delivery is also the Agilent Purification amp Preparative LC User Documentation CD G9300 64500 SD 1 Purification Solution System Manual 31 3 Installation Unpacking and Inspection Unpacking and Inspection 1 Check carefully to make sure you received all the items listed on the packing list 2 Carefully unpack all the containers and inspect the contents for damage as soon as possible 3 Save the packing containers they will be useful if you have to file a claim for damage or in the case of future transit 32 SD 1 Purification Solution System Manual Installation 3 Unpacking the Detector Prerequisites Ensure there is enough room on the bench for the detector Heavy weight The Agilent 325 UV VIS Dual Wavelength Detector weighs in excess of 15 kg 33 Ib gt Carry the instrument at least with 2 people gt Avoid back strain or injury by following all precautions for lifting heavy objects gt Ensure that the load is as close to your body as possible gt Ensure that you can cope with the weight of your load 1 Carefully unpack the unit from the shipping carton and place it on the bench
9. e Assy PWB Sync Interface 325 335 optional Cross over Ethernet cable Power cord Flow cells are required for the detector but are ordered separately See Hydraulic Connections Flowcells on page 64 for suitable flowcells Delivery Checklist Autosampler The autosampler is packed in a single carton The following list shows all items delivered in a standard delivery Your personal list depends on your order therefore countercheck delivery with your order e Agilent 410 Autosampler G9331A G9332A Power cord e Agilent 410 Reservoir Rack e Standard Tray Assy G9332A Agilent and PrepStar Mast kit e Prime purge valve bracket e Prime purge valve stainless steel 30 SD 1 Purification Solution System Manual Installation 3 Delivery Checklist Fraction Collector The following list shows all items delivered in a standard delivery Your personal list depends on your order therefore countercheck delivery with your order Agilent 440 LC Fraction Collector Assy USB RS 232 serial adaptor optional Rack Funnel Rack Kit optional Power cord Delivery Checklist Capillary Kits Your order contains one of the following Capillary Kits Binary Pump Stainless Steel Tubing Kit 1 16 x 0 02 i d Binary Pump Stainless Steel Tubing Kit 1 16 x 0 03 i d Binary Pump Stainless Steel Tubing Kit 1 16 x 0 04 i d Binary Pump Stainless Steel Tubing Kit 1 8 x 0 08 i d Isocratic Pump Stainless Steel Tubing Kit 1 16 x 0 02 i d
10. so that a solvent will not come into direct contact with the skin gt Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor Cuts gt When working with glass or quartz parts take care to prevent breakage 140 Other Precautions Airflow to the cooling fans of the liquid chromatograph must be unobstructed Do not block the ventilation grills on the liquid chromatograph and accessories Consult the manuals supplied with your PC monitor and for their specific ventilation requirements SD 1 Purification Solution System Manual Appendix 6 High Pressure Hazards WARNING High velocity stream of volatile and or toxic liquids If a line ruptures a relief device opens or a valve opens accidentally under pressure potentially hazardous high liquid pressures can be generated by the pump gt Wear personal protective equipment when you inject samples or perform routine maintenance gt Never open a solvent line or valve under pressure Stop the pump first and let the pressure drop to zero gt Always keep the doors and covers closed during operation gt Read and adhere to all Notes Cautions and Warnings in the manual Ultraviolet Radiation WARNING Irritation to the skin eyes and upper respiratory system gt Ensure that protective lamp covers of variable and fixed wavelength detectors are in place during operation gt Do not look directly into
11. 143 service 12 external contacts panel connecting 45 B battery F safety information 144 features 10 bench space 21 flowcell types 64 flowcell C install 66 cables connecting 49 G other 61 general waste tubing power 61 connecting 76 column oven 12 components 83 H condensation 20 hardware connections setup 98 workstation control 125 high pressure outlet tubing installation 51 D pump head 51 defect on arrival 28 high pressure delivery checklist hazard 141 autosampler 30 HPLC system capillary kits 31 auto preparative 41 SD 1 Purification Solution System Manual Index flushing 59 gradient 39 isocratic 38 scale up 42 inlet and outlet tubing installation 54 pump head 54 inspection 32 installation overview 84 probe 86 tubing 86 installing door 70 internet 148 introduction autosampler 11 detector 10 fraction collector 15 preparative autosampler 13 system 8 9 L lithium batteries 144 location detector module 60 low pressure inlet tubing installation 51 pump head 51 M maintenance 149 Index module 122 mat rack location 86 method setup 110 0 overview installation 84 module 73 P packaging damaged 28 parts 122 power cords 19 power connection 92 prep option installing 82 pump head installation 56 priming 58 rack location mat 86 rack orientation 91 radio interference 145 reagente addition 12 relay output 127 remote control connecting 49 removing door
12. 71 front panel 64 150 S safety information lithium batteries 144 safety general information 136 sample rack assembly 89 installation 90 sample tray installation 81 76 scale up processing 43 setup ChemStation control 102 electrical 45 hardware 98 OpenLAB 102 side port needle 11 site requirements power cords 19 specifications 22 spill tray installation 85 stack optimizing 37 synchronization signals 131 syringe waste tubing connecting 76 system components 26 rinsing 79 T terminal block analog 47 digital input 48 relay output 48 troubleshooting 122 U unpacking 32 using 122 V vials filling and sealing 81 W waste electrical and electronic equipment 143 water and leakage drain connecting 77 WEEE directive 143 SD 1 Purification Solution System Manual www agilent com In This Book This manual provides setup information on following modules Agilent SD 1 Solvent Delivery Module G9302A G9303A Agilent 325 UV VIS Dual WL Detector G9309A Agilent 410 Autosampler G9331A G9332A Agilent 218 Solvent Delivery Module G9300A G9301A Agilent 440 Fraction Collector G9340A The manual describes the following Optimizing stack configuration Setup hardware Setup software Setup methods Agilent Technologies 2012 2013 Printed in Germany 03 2013 G9302 90301 EE Agilent Technologies
13. Proper connection of the power cord 2 Power at the wall receptacle 3 Functionality of the main power fuse F1 Connecting the External Contacts Panel The Agilent SD 1 Pump has a number of analog and digital connections on the rear panel These can be used to digitize data from an analog detector start and stop other devices through contact closures and to receive contact closures to start and stop the pump The external contacts are not used with the standard systems offered by Agilent The standard systems using the serial interface connections for communication and is organized by the OpenLAB software The external contacts panel can be removed for convenience when attaching the connections SD 1 Purification Solution System Manual 45 3 Installation Captive screw Figure 5 External contacts panel panel turned 90 for clarity 1 Remove the panel by loosening the three captive screws holding it in place and pulling the handle away from the pump Incorrect voltage to the instrument Damage to your instrumentation can result if the devices are applied to a voltage higher than specified gt Connect the terminal block 2 digital input of your instrument only to a voltage from 0 5 5 5 VDC gt Connect the terminal block 3 relay output of your instrument only to a voltage of 24 VDC and a current of 1 A gt If any module you are switching requires higher voltage or current than the specifi
14. Sample Tray 81 Installing the Agilent 410 Autosampler Prep Option 82 Installing the Fraction Collector 83 Overview of the Module 83 Installation Overview 84 Assembling the Fraction Collector 84 Installing the Spill Tray 85 Installing the Rack Location Mat 86 Installing the Probe and Tubing 86 Assembling the Sample Racks 89 Installing the Sample Racks 90 Rack Orientation 91 Connecting the Power to the Fraction Collector 92 Connecting the Fraction Collector to the HPLC System 94 Determining the Delay Time 94 Determining the Correct Probe Depth 94 Installing the RS 422 485 Communication Kit 95 Installing the Stream Splitter 97 Setup Hardware 98 Setup the Hardware 98 Setup the Pump 98 Setup the Autosampler 99 Setup the Detector 100 Setup the Fraction Collector 100 SD 1 Purification Solution System Manual Installation 3 Setup the Software 101 Install Agilent OpenLAB CDS ChemStation PrepLC Drivers 101 Setup the System with OpenLAB CDS ChemStation Edition Control Panel 102 Setup Method 110 Setup the CIM in the OpenLAB CDS ChemStation PrepLC Drivers 116 This chapter gives information about the installation of your Agilent SD 1 Solvent Delivery Module Agilent 325 UV VIS Dual WL Detector Agilent 410 Autosampler and Agilent 440 Fraction Collector SD 1 Purification Solution System Manual 25 3 Installation Delivery Delivery 26 For detailed information on parts delivered with the modules please ref
15. Solution System Manual Installation 3 window Your chosen flowcell type is packed internally in the detector The four flowcell types are outlined in Table 6 on page 65 Table 6 Compatible flowcells Flowcell type Flowcellp n pathlength Column ID Flow rate Maximum pressure Analytical 210181800 9mmxO0mm 2 8mm 0 0001 69 bar 10 mL min 1000 psi Preparative 210181900 9mmximm 4 76mm 1 69 bar 500 mL min 1000 psi Scale Up2 210224200 4mm x 4 76 mm 10 69 bar 0 25 mm 200 mL min 1000 psi Super Prep 210182000 4mm x 8 152 mm 30 69 bar 0 15 mm 1200 mL min 1000 psi Micro analytical 210182100 4mmxOmm 1 4mm 0 69 bar 20 mL min 1000 psi A pathlength of a mm x b mm means that the sample light path has a pathlength of a mm and the reference light path has a pathlength of b mm A reference light path of zero means there is no fluid in the cell air acts as the reference Extended range cell It is important for the extended range cells to run at least at the minimum flow rate SD 1 Purification Solution System Manual 65 3 Installation Installing a Flowcell The Agilent 325 UV VIS Dual Wavelength Detector is not shipped with a flowcell installed You will need to install the flowcell that you purchased with the detector Each flowcell comes with a set of recommended nuts and ferrules that may be fitted to tubing 1 16 tubing is used on all flowcells However for the 4 mm x 0 15 mm super prep flowcell
16. bench If an autosampler is present it should be placed on top of the detector e Position the master pump as highest pump in the stack This position allows easy access to keypad and display to control the HPLC system via pump instead of software SD 1 Purification Solution System Manual 37 3 Installation Optimizing the Stack Configuration Isocratic System Injector valve Drain valve Agilent SD 1 From solvent reservoir Column Detector Figure 2 Isocratic HPLC system The high pressure outlet from the Agilent SD 1 connects to the system drain valve to the injector valve the column and to the detector flow cell The outlet from the detector can be directed to waste or collected 38 SD 1 Purification Solution System Manual Gradient System Injector valve Drain valve High pressure mixer SD 1 pump A From solvent reservoir A SD 1 pump B From solvent reservoir B l Column Detector Figure 3 Binary gradient HPLC system SD 1 Purification Solution System Manual Optimizi Installation gt onfiguration 3 39 3 Installation The two Agilent SD 1 pumps can be used to pump two solvents in a gradient under front panel control A binary gradient HPLC system can also be controlled by a applicable instrument control software on a computer The software controls the flow rates for both Agilent SD 1 pumps Plumbing is the same for both these systems The high pressure outlets from
17. in four pairs and define how the detector will operate in a HPLC system These signals are important for controlling timing and synchronization of the detector with the other devices in the system Synchronization signals are closely tied to the detector states and transitions P9 and J10 pin designations are shown in Figure 27 on page 131 J10 P9 15 5 Volts 1 Fault Out 8 Ground 14 Lamp Off 2 Fault Out 7 Lamp Off 3 Ready In 6 Auto zero 4 Ready In 5 Fault In 11 Enable Out 5 Start Out 4 Fault In 10 Enable Out 3 Ready Out 9 5 Volts 2 Ready Out 1 Start In Figure 27 Pin designations for J10 and P9 P9 provides connections when the Agilent 325 UV VIS Dual Wavelength Detector acts as a slave and receives control from another module J10 provides connections when the detector acts as a master and sends control to another device An input is activated or said to be present when its two signal wires are connected together This can be done with a relay contact closure If the inputs are driven from another instrument with optical isolators or other polarized devices then attention must be paid to the polarity of the signal wire SD 1 Purification Solution System Manual 131 5 Cables connections The positive output signal must be connected to the positive input signal and the negative output to the negative input The colo
18. installed see OpenLAB CDS Installation Driver Prep LC M8366 64000 Modules are wired as described in Cable Connections on page 125 All modules are setup as described in Setup the Hardware on page 98 All modules are switched on OpenLAB configuration 1 Open the T OpenLAB Control Panel and select Create gt Create Instrument R iti Create Refresh Edit Nosikations Columns Create Instrument s Properties Create Location k Instruments Application Fj Instruments X Administration Your startup license expires in 60 days 2 Define the Name Example PrepLC 102 SD 1 Purification Solution System Manual Installatio 3 he Sof p Retesh wstruments and Locabons Properties Appicaton instrument controler instrument type Contact 0G Wstruments SK Administration Your startup license expires in 60 days 4 Select Configure Instrument IROA EARR Edit Delete Refresh Lock Create Configure Edit Notifications Shortcuts Instrument Instruments and Locations Properties Actions Navigation PrepLc Not Connected EEEE Instruments Start Instrument J Prep a Launch o Launch Offiine Status Ei instruments ra Administration Your startup license expires in 60 days SD 1 Purification Solution System Manual 103 3 Installation 5 Select No to avoid the auto configuration It doesn t work with this version store Agilent LC System Z 20 wec evehat
19. it is recommended to use 1 8 tubing at higher flow rates In this case you can add the Adaptor 1 8 1 16 1610126800 This will require the 1 8 tubing and the 1 8 flowcell fittings Tubing connections are PEEK type except for the Super Prep flowcell which uses ETFE tubing 0 125 mm x 0 062 mm Parts required p n 66 OR OR OR 210181800 210181900 210224200 210182100 9910128300 210182000 1610126900 1610126400 1610126800 ae a ee a ee ee Description Flowcell 9 mm x 0 mm inert analytical Flowcell 9 mm x 1 mm inert prep Flowcell 4 mm x 0 25 mm inert scale up Flowcell 4 mm x 0 mm inert micro analytical Flow cell replacement fittings Flowcell 4 mm x 0 15 mm inert super prep Fitting 1 8 tube nut flat bottom Fitting 1 8 tube ferrule Pack of 10 Adaptor 1 8 1 16 SD 1 Purification Solution System Manual Installation 3 Installing the Detector 1 Fit the nuts and ferrules on the PEEK tubes 2 Screw the two tubes into the inlet and outlet connection of the flowcell Each flowcell has an inlet and outlet connection Ferrule NOTE Be careful not to cross thread the connector into Nut the flowcell body Do not over tighten as this will damage the threads PEEK tube Thumbscrew Outlet connection Inlet connection Tubing NOTE The position of the inlet and outlet connections varies for different flowcells SD 1 Purification Solution System Manua
20. may be left unconnected If applicable plug the AC connector on the serial interface cable into the AC power supply Configure the pump IDs see Agilent SD 1 Isocratic Solvent Delivery Module User Manual G9302 90001 SD 1 Purification Solution System Manual Installation 3 Plumbing Connections 200 to 800 mL Pump Heads Low Pressure Inlet Tubing Tools required Description Wrench open ended inch Remove the solvent inlet assembly from the accessories package 2 Immerse the inlet filter into clean HPLC grade water 3 Remove the plug from the low pressure inlet tee and connect the inlet fitting to the inlet tee a Store the plug in a safe place 4 Thread the fitting into the inlet tee and finger tighten 5 Tighten the fitting in the inlet tee with the inch open ended wrench and tighten 1 4 turn past finger tight High Pressure Outlet Tubing Refer to the following figure to find the outlet connections for your SD 1 pump The appropriate compression fitting for your SD 1 pump is in the accessories package SD 1 Purification Solution System Manual 51 3 Installation Table4 Connections for the outlet check valve Type of pump Ferrule Tubing Ferrule Tubing Ferrule Tubing PFA head tubing Titanium SST Titanium PEEK PVDF FEP 200 mL min 0 159 cm 1 16 inch l Compression fitting Compression fitting PEEK tubing l stas d 1 a 7 Ferrule collar T SST ferrule PEEK ferrule
21. neck of the solvent reservoir As an alternative you can finish connecting the instrument through the drain valve to the rest of the HPLC system and prime the instrument with the drain valve open to waste see Priming the Pump Heads on page 58 SD 1 Purification Solution System Manual 53 3 Installation Plumbing Connections 3 2 L Pump Head Inlet and outlet plumbing use flared tubing compatible with PFA or PVDF fittings CAUTION Damage to the fittings Use of tools such as wrenches or pliers to tighten the fittings may damage the fitting or cause the tubing to fail under pressure gt The fittings with the exception of the check valves should only require hand tightening 1 Remove the white shipping plug from the inlet valve a Store the plug in a safe place 54 SD 1 Purification Solution System Manual Installation 3 2 Attach the inlet and outlet tube assemblies see Figure 8 on page 55 a Keep the inlet tube to the solvent reservoir short A short tube prevents inlet pressure oscillations b Flush the tubing and reservoirs with air or filtered solvent Outlet assembly 1 4 inch 0 635 cm OD FEP tubing Wrench Inlet assembly 1 2 inch 1 27 cm OD FEP tubing eg Figure 8 Connections for 3 2 L pump heads 3 Fill the system with filtered solvent SD 1 Purification Solution System Manual 55 3 Installation Pump Head Installation When Tools required The pumps are shipped
22. on the user is encouraged to try one or more of the following measures e Relocate the radio or antenna e Move the device away from the radio or television e Plug the device into a different electrical outlet so that the device and the radio or television are on separate electrical circuits e Make sure that all peripheral devices are also certified e Make sure that appropriate cables are used to connect the device to peripheral equipment e Consult your equipment dealer Agilent Technologies or an experienced technician for assistance e Changes or modifications not expressly approved by Agilent Technologies could void the user s authority to operate the equipment SD 1 Purification Solution System Manual Appendix 6 ICES NMB 001 This ISM device complies with Canadian ICES 001 Cet appareil ISM est conforme a la norme NMB 001 du Canada SD 1 Purification Solution System Manual 147 6 Appendix Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com 148 SD 1 Purification Solution System Manual Index A detector 30 AC power 62 fraction collector 31 Aci pump 29 grent delivery 26 on internet 148 detector outlet back pressure analog output 126 restrictor 69 assembling fraction collector 84 driver installation 101 autosampler connecting 80 E lifting 34 location 72 electronic waste
23. or EMC regulations Test and Measurement If test and measurement equipment is operated with unscreened cables or used for measurements on open set ups the user has to assure that under operating conditions the radio interference limits are still met within the premises SD 1 Purification Solution System Manual 145 Appendix Electromagnetic Compatibility 146 EN55011 CISPR11 Group 1 ISM equipment group 1 contains all ISM equipment in which there is intentionally generated and or used conductively coupled radio frequency energy which is necessary for the internal functioning of the equipment itself Class A equipment is equipment suitable for use in all establishments other than domestic and those directly connected to a low voltage power supply network which supplies buildings used for domestic purposes This device complies with the requirements of CISPR11 Group 1 Class A as radiation professional equipment Therefore there may be potential difficulties in ensuring electromagnetic compatibility in other environments due to conducted as well as radiated disturbances Operation is subject to the following two conditions This device may not cause harmful interference e This device must accept any interference received including interference that may cause undesired operation If this equipment does cause harmful interference to radio or television reception which can be determined by turning the equipment off and
24. side There should not be any movement If the rack location mat is loose refit it Installing the Probe and Tubing The sample probe comes preassembled with 0 050 cm 0 020 in ID tubing There are three additional coils of tubing included in the probe kit The longer piece of tubing with a nut and ferrule is used for the drain tube on the divert valve e The shorter tubing with a nut and ferrule is used to connect fraction collector divert valve to the sample output from the HPLC system e The third piece of tubing is 0 025 cm 0 010 in ID tubing and can be used for low delay volumes for applications with flow rates of 2 mL min or less For details on installing the tubing refer to Agilent 440 Fraction Collector User Manual G9340 90000 1 Turn off the fraction collector 2 Slide the Z axis slide to the top of the probe carriage 3 Manually rotate the probe arm so that it can be easily accessed 86 SD 1 Purification Solution System Manual Installation 3 4 Disassemble the probe kit by unscrewing the nut holding the metal probe from the bottom of the lower knurled mount nut and then the lower knurled mount nut from the top knurled mount nut Top knurled mount on the probe assembly I Lower knurled mount nut on the probe assembly Insert the probe into the probe mounting block see Figure 18 on page 83 co 6 Push the tubing down into the probe so that at least 0 5 cm tub
25. tee with a 9 64 inch wrench 10 Connect the inlet tubing tee to inlet check valves 11 Press ENTER to confirm the mounting screws and plumbing are connected The following message will appear Plug in BOTH connectors Press ENTER when completed 12 Connect the pressure sensor cables 13 Press ENTER to complete the head replacement procedure The following display will read with appropriate values for the actual head size HEAD REPLACEMENT IS COMPLETE Max Flow 200 mL m Max Pressure 6000 psi 40 bar Press ENTER to continue Figure 11 Pump head replacement SD 1 Purification Solution System Manual 57 3 Installation Priming the Pump Heads Preparations 58 All pump heads are self priming 1 The detector is bypassed If a prime purge valve is connected open the prime purge valve to relieve the pressure Tighten the outlet tee fitting 4 turn past finger tight 2 To switch on the pump power press the power switch After a few moments the Flow display is displayed 0 00 mL m 0 psi TIME FLOW 0 00 0 00 If the Flow field is not flashing press the RIGHT ARROW key to get the cursor to the flow field To prime the 200 mL min pump head type in 150 and confirm with ENTER OR To prime the 500 mL min pump head type in 400 and confirm with ENTER OR To prime the 800 mL min pump head type in 600 and confirm with ENTER OR To prime the 3 2 L min pump head type in 2000 and confirm with ENTER S
26. that Agilent Technologies supplies with this instrument for any other equipment SD 1 Purification Solution System Manual 19 2 Site Requirements and Specifications Condensation CAUTION Condensation within the module Condensation will damage the system electronics gt Do not store ship or use your module under conditions where temperature fluctuations could cause condensation within the module gt If your module was shipped in cold weather leave it in its box and allow it to warm slowly to room temperature to avoid condensation Area selected Explosion damage and accuracy of the module gt Select an area free from drafts corrosive atmospheres and vibration gt Select a dust free low humidity environment gt Use air conditioning for control of the environment 20 SD 1 Purification Solution System Manual Site Requirements and Specifications 2 Bench Space Make sure that the bench is designed to bear the weight of all modules For details on the space needed around the individual modules refer to the according manuals Agilent SD 1 Isocratic Solvent Delivery Module User Manual G9302 90001 Agilent 325 UV VIS Dual Wavelength Detector User Manual G9309 90000 e Agilent 410 Autosampler User Manual G9331 90000 Agilent 440 Fraction Collector User Manual G9340 90000 SD 1 Purification Solution System Manual 21 2 Site Requirements and Specifications Specifications For deta
27. that case sample will be forced into the air needle risking cross contamination of samples and fouling of the needle pair 2 Check that the seal is airtight due to maintain a pressure on the vial for air bubble prevention and to prevent evaporation of volatile samples 3 Check seal after crimping if the cap can be turned easily the seal is not airtight re adjust hand crimper When using uncapped vials the performance of the AutoSampler may not meet the specifications precision Do not re use a sample vial without replacing its cap or septum Loading the Sample Tray 1 Place the vial in the tray and link them to methods in the Series For details see Agilent 410 Autosampler User Manual G9331 90000 Chapter Using section Programming the Run Sequence or Series 2 Ifthe autosampler ist not running manually rotate the tray to gain access to all vial positions SD 1 Purification Solution System Manual 81 3 82 Installation Installing the Agilent 410 Autosampler Prep Option 1 ao ol A Ww Replace the standard injection valve with the special Agilent 410 Prep valve Replace standard sample needle air needle and buffer tubing with the ones supplied in Prep Upgrade Option Includes Needle Syringe Injection Valve and Large Volume Sample Tray 393590791 Re connect all tubing to the injection valve Replace standard Syringe with the 2500 uL syringe Install the 24 vials LSV tray Choose Prep Mode in system
28. 15 Vw aa S Figure 17 Rear View of the autosampler Fuses and voltage selector Main input 2 3 Main switch 4 P1 1 0 connector SD 1 Purification Solution System Manual 75 3 76 Installation 5 P2 I 0 connector 6 RS 232 communication interface connector 7 CE mark 8 Fan only if optional Peltier tray cooling option is installed Installing the Sample Tray 1 Place the sample tray in the autosampler and rotate it until the tray drops into the slot only one position is possible 2 Turn the tray fixation knob clock wise to fixate the tray see Overview of the Module on page 73 for an overview Connecting the Waste Tubings The following Waste Tubings must be connected to the autosampler e General waste tubing Syring waste tubing e Water and leakage drain Connecting the General Waste Tubing 1 Connect the drain tubing to the right hand drain hose connector of the autosampler and put it in a bottle which is placed on the floor All the liquid dispensed while the autosampler is in the wash position is removed through this drain Connecting the Syringe Waste Tubing 1 Place the syringe waste tubing into a small bottle next to the autosampler If no injection volumes are programmed that are larger than the buffer tubing can contain the syringe waste will only be wash solvent SD 1 Purification Solu
29. 3 Press Tray 4 Confirm each of the tray settings that appear on the display Tray type 84 3 9 24 Vial type STANDARD 2 5 mL 5 Reboot the module Setup the Detector The detector is set up at the factory with a BOOTP or DHCP IP address If need be this can be changed by a trained service engineer who will own a copy of the diagnostics software or by setting up Agilent BootP Service to provide the detector with the right IP details Setup the Fraction Collector The Fraction Collector is ready to be set up in OpenLAB and does not need to have the hardware set up 100 SD 1 Purification Solution System Manual Installation 3 Setup the Software Install Agilent OpenLAB CDS ChemStation PrepLC Drivers Parts required p n Description M8301AA OpenLAB CDS ChemStation Edition Workstation A 01 05 or higher M8500AA M8500AA LC driver M8366 64000 OpenLAB CDS Installation Driver Prep LC M8367 64000 OpenLAB CDS Installation Upgrade Driver Prep LC Hardware required Computer with OpenLAB CDS ChemStation Edition installed For details refer to the OpenLAB WorkStation Installation Guide 1 Copy AgilentDriversPrepLCChemstationSet_up msi from CD to your computer 2 Doubleclick on AgilentDriversPrepLCChemstationSet_up msi and follow the steps in the setup wizard SD 1 Purification Solution System Manual 101 3 Installation Setup the System with OpenLAB CDS ChemStation Edition Control Panel Preparations Latest driver package
30. 35 General Safety Information 136 Solvent Miscibility 142 The Waste Electrical and Electronic Equipment Directive 143 Batteries Information 144 Radio Interference 145 Electromagnetic Compatibility 146 Agilent Technologies on Internet 148 SD 1 Purification Solution System Manual Contents 6 SD 1 Purification Solution System Manual SD 1 Purification Solution System Manual 1 Introduction to the System Introduction to the System 8 Introduction to the SD 1 Isocratic Solvent Delivery Module 9 Introduction to the Agilent 325 UV VIS Dual Wavelength Detector 10 Introduction to the Agilent 410 Autosampler 11 Agilent 410 Autosampler G9331A 11 Agilent 410 Preparative Autosampler G9332A 13 Introduction to the Agilent 218 Solvent Delivery Module 14 Introduction to the Agilent 440 Fraction Collector 15 This chapter introduces to the Agilent SD 1 Purification Solution system and its components Apg Agilent Technologies 7 1 Introduction to the System Introduction to the System A complete Agilent SD 1 Purification Solution system includes Agilent SD 1 Isocratic Solvent Delivery Module s Tubing Mast kit Agilent 325 UV VIS Dual WL Detector Agilent 410 Autosampler Agilent 218 Solvent Delivery Module Agilent SD 1 Isocratic Solvent Delivery Module for sample injection and Agilent 440 Fraction Collector As an option the HPLC Control Software Agilent OpenLAB CDS ChemStation Edition is recommended Th
31. Agilent SD 1 Purification Solution System User Guide tt Agilent Technologies Notices Agilent Technologies Inc 2012 2013 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 69302 90301 Edition 03 2013 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn This product may be used as a com ponent of an in vitro diagnostic sys tem if the system is registered with the appropriate authorities and com plies with the relevant regulations Otherwise it is intended only for gen eral laboratory use Warranty The material contained in this docu ment is provided as is and is sub ject to being changed without notice in future editions Further to the max imum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or perfor mance of this document or of any information contained
32. Communication established with COM1 l a 3 Verify the connection by clicking on Activate communication Information Communication established with COM1 is visible on the screen 4 Click OK Configuration dialog closes Autosampler configuration 1 Doubleclick in Configurable Modules on Autosampler Autosampler Configuration dialog opens SD 1 Purification Solution System Manual 105 3 106 Installation 2 Select the COM Port as COM 1 i p Autosampler Configuration Instrument 1 COM Port com X ID 60 Activate communication FW version Options Tray 84 standard vials Loop volume 100 pL Syringe volume Tubing volume Preparative option No v Column oven W Tray cooling V Alarm buzzer i Communication established with COM1 n ie Select the Tray84 standard vials as an example Double check your actual configured Tray Check the other variables present in the Autosampler Configuration screen ao oO A WwW Verify the connection by clicking on Activate communication Information Communication established with COM1 is visible on the screen 7 Click OK Configuration dialog closes Detector Configuration 1 Doubleclick in Configurable Modules on Detector Detector Configuration dialog opens 2 Select the Browse function to start discovery your Detector The IP address will be populated by the searching results
33. D 1 Purification Solution System Manual 97 3 Installation Setup Hardware Setup Hardware Setup the Hardware This is done on the modules regardless of whether you are using HPLC control software or using one of the pumps as a master controller including following modules Different pumps e 325 UV VIS Dual WL Detector 440 Fraction Collector and 410 Autosampler Setup the Pump 1 Turn the module on 2 Press 98 SD 1 Purification Solution System Manual Installation 3 3 Press Enter 4 With the left arrow key select Headsize is defined as NO ID of the Pump 3 select a different ID for every devices Available choices are 0 63 MC master controller or no ID For OpenLAB an ID between 1 63 must be used CIM 5 5 Press Enter 6 Reboot the module Setup the Autosampler Preparation for general and tray settings 1 Press Serial on the autosampler keyboard To set up the general system settings 1 Turn the module on 2 Press SYSTEM 3 Press GENERAL 4 Confirm or change each of the settings that appear on the display Volume of installed loop 0 5000 uL Volume of tubing needlesvalve 0 999 uL Syringe volume 250 1000 Syringe speed LOW NORMAL HIGH Skip missing vials YES NO Air segment YES NO Headspace pressure YES NO To set up the tray settings 1 Turn the module on 2 Press SYSTEM SD 1 Purification Solution System Manual 99 3 Installation
34. NG Heavy weight The Agilent 440 Fraction Collector weighs in excess of 18 kg gt Carry the instrument at least with 2 people gt Avoid back strain or injury by following all precautions for lifting heavy objects gt Ensure that the load is as close to your body as possible gt Ensure that you can cope with the weight of your load 1 Carefully unpack the unit from the shipping carton and place it on the bench 2 Make sure to check carefully for all miscellaneous components that might be contained in the inner compartments The fraction collector is a sensitive instrument and should always be handled with the degree of care appropriate for laboratory instrumentation Keep the shipping carton as it provides excellent protection if you have to transport or store the detector in the future 36 SD 1 Purification Solution System Manual Installation 3 Optimizing the Stack Configuration This section contains information on how to stack your modules depending on the preparative method For optimal performance for the given examples respect the following rules e The orientation is also suggested if you are only installing the Agilent SD 1 Pump For a two modules systems the modules can be stacked one on the other On the side of the stacked modules a mast can be attached to hold the mixer drain valve inject valve and column hanger e For three modules systems stack two of the modules and place the third on the
35. System Manual 125 5 Cables Analog Output Analog Output For analog output signals install the optional Analog signal cable 110744200 into the J14 receptacle Pin designations are shown below J14 2 Channel A 4 Channel B Figure 24 Pin designation for J14 The open ends of the analog output cable have labels with the signal names Channel A Channel A and Channel B Channel B 126 SD 1 Purification Solution System Manual Cables 5 Relay Output Relay Output For time programming external events a contact closure Relay output is available To configure the Relay output install the optional Assy PWB relay interface 325 210187590 into the J4 receptacle Pin designations are shown below Figure 25 Pin designation for J4 There are four general purpose output relays and one dedicated Peak relay Each output uses a DIP relay that is capable of handling 500 mA of contact current At reset or power up the output relay contacts are set to the default parameters open After loading a method they will be set as defined in the method s time 0 parameters SD 1 Purification Solution System Manual 127 5 Cables The Peak relay is software programmable for duration delay and active sense At power up the relay contact will be set to the inactive state as defined by the value of the active sense parameter stored in the detector Upon being triggered relay activation will occur for the time inte
36. activated for 600 ms when the Agilent 325 Detector starts a time program This polarized edge triggered input signal informs the Agilent 325 Detector that a fault condition exists in another instrument in the system The Agilent 325 Detector halts the time program and sends a Fault Out signal The lamp can be programmed to either remain on or turn off upon receiving a fault signal This polarized output signal will activate for 600 ms when either of the following conditions occurs The Agilent 325 Detector discovers an internal fault condition that warrants aborting the run The Agilent 325 Detector receives a Fault In signal and it has no internal fault condition itself This edge triggered contact closure causes an auto zero adjustment This edge triggered contact closure switches the lamp off It is possible to turn the lamp back on manually if the contact is still closed An optional Assy PWB sync interface 325 210186590 is available to interface between the Agilent 325 UV VIS Dual Wavelength Detector synchronization signals and other devices This board is inserted into the P9 and J10 connectors and connects to a terminal strip on the adapter board This terminal strip accepts bare wire leads from cables connecting other devices These cables may originate from the other device or a dedicated cable can be used if available for the particular application SD 1 Purification Solution System Manual 133 5 Cables Synchronizat
37. and Control Instrumentation product Do not dispose off in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com for more information SD 1 Purification Solution System Manual 143 6 Appendix Batteries Information Lithium batteries may not be disposed off into the domestic waste Transportation of discharged Lithium batteries through carriers regulated by IATA ICAO ADR RID IMDG is not allowed Danger of explosion if battery is incorrectly replaced gt Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries gt Replace only with the same or equivalent type recommended by the equipment manufacturer Lithiumbatteri Eksplosionsfare ved fejlagtig handtering Udskiftning ma kun ske med batteri af samme fabrikat og type gt Lever det brugte batteri tilbage til leverand ren Lithiumbatteri Eksplosionsfare Ved udskiftning benyttes kun batteri som anbefalt av apparatfabrikanten gt Brukt batteri returneres appararleverandoren 144 Bij dit apparaat zijn batterijen geleverd Wanneer deze leeg zijn moet u ze niet weggooien maar inleveren als KCA SD 1 Purification Solution System Manual Appendix 6 Radio Interference Cables supplied by Agilent Technologies are screened to provide optimized protection against radio interference All cables are in compliance with safety
38. both Agilent SD 1 pumps are connected to a high pressure mixer to ensure that both solvents are mixed thoroughly The system drain valve is plumbed after the mixer The injector valve is plumbed after the drain valve then the column then the detector flow cell The outlet from the detector can be directed to waste or collected 40 SD 1 Purification Solution System Manual Installation 3 Optimizing the Stack Configuration Auto Preparative System Detector Column Drain valve High pressure mixer From solvent reservoir A To faction collector Instrument control lt Sample inlet to inject pump From solvent reservoir B SD 1 pump B Injection pump Figure4 Auto Preparative HPLC System Instead of an injection valve this special binary gradient HPLC system uses a third pump for sample injection All pumps are controlled by applicable instrument control software on a PC The high pressure outlets from both Agilent SD 1 solvent pumps are connected to a high pressure mixer The system drain valve is plumbed after the mixer The sample inject pump is plumbed into the system with a tee The column is plumbed after the tee then the detector The outlet from the detector flow cell would normally be connected to a fraction collector SD 1 Purification Solution System Manual 41 3 Installation Scale up the HPLC System 150 mL min Model Agilent 218 injection pump 42 E
39. ccess further details on the system components 5 Cables This chapter provides information on cables used with the instrument 6 Appendix This chapter provides addition information on safety legal and web SD 1 Purification Solution System Manual Contents Contents 1 Introduction tothe System 7 Introduction to the System 8 Introduction to the SD 1 Isocratic Solvent Delivery Module 9 Introduction to the Agilent 325 UV VIS Dual Wavelength Detector 10 Introduction to the Agilent 410 Autosampler 11 Introduction to the Agilent 218 Solvent Delivery Module 14 Introduction to the Agilent 440 Fraction Collector 15 2 Site Requirements and Specifications 17 Site Requirements 18 Specifications 22 3 Installation 23 Delivery 26 Damaged Packaging 28 Check Delivery 29 Unpacking and Inspection 32 Optimizing the Stack Configuration 37 Installing the Solvent Delivery Module 45 Installing the Detector 60 Installing the Autosampler 72 Installing the Fraction Collector 83 Installing the RS 422 485 Communication Kit 95 Installing the Stream Splitter 97 Setup Hardware 98 Setup the Software 101 4 Using Troubleshooting Maintenance and Parts 121 Using Troubleshooting Maintenance and Parts 122 4 SD 1 Purification Solution System Manual Contents 5 Cables 123 Cable Overview 124 Cable Connections 125 Analog Output 126 Relay Output 127 Desktop PC Communications 130 Synchronization Signals 131 6 Appendix 1
40. concept that combines high precision with simplicity and reliability Three injection modes can be selected Full loop e Partial loop filling uL Pick up Maximum precision maximum flexibility and zero sample loss can be achieved with these features Side Port Needle The strong side port needle combines the optimum point style for septa piercing with a minimum risk of blockage by septum particles SD 1 Purification Solution System Manual 11 1 Introduction to the System Column Oven A column oven is an integral part of the Agilent 410 Autosampler because constant column temperature is important for long term stability of a chromatographic separation and may be required for GLP compliance Reagent Addition Internal Standard addition sample dilution or derivatization can be programmed in a very simple manner A single stage derivatization of a sample in a separate destination vial requires no more than 4 program lines Multi reagent addition is also possible two large volume reagent vials are available on the sample tray Service Autosampler Low instrument down time is accomplished by a high Mean Time Between Failure and quick instrument service Special attention has been paid to these aspects of the concept as is illustrated by the injection valve The Agilent 410 Autosampler will alert you when the lifetime of the seal is exceeded or if the switching torque becomes too high This allows preventive maintenance before i
41. control software If there is no link method specified the method will stop looping after the current method pass If there is a link method specified the method will stop looping and transfer to the link method at the end of the current method pass Connect these inputs to the position sensing switch of the injector or to the injection complete output from the automatic sample injector The contact should close when the valve is in the inject position or when the autosampler completes injection Contact closure cancels inject wait programmed in the pump Inputs can accept all contact closures relays open collector transistors and open collector integrated circuits When there is no event the input must be greater than 4 75 V with a contact closure the input must be equal to or less than 1 2 V with a duration of 0 1 s or longer Provides 5 V logic voltage with a 47 Q resistor in series Low current loads less than 20 mA such as sensitive relays LEDs and simple logic circuits can be run off this output To maintain output greater than 4 75 V the load must be less than 5 mA Connected internally to case ground 48 Terminal Block 3 TB 3 Relay Output The relay out connectors are for switching power to user defined external devices Each pair of output connectors is connected to a relay inside the Agilent SD 1 To use the relay outputs to operate any inductive load devices please contact your Agile
42. detector fluid cells or at the UV light source When inspecting the light source or fluid cell always use protective eye covering such as borosilicate glass or polystyrene gt Ventilate the area surrounding the detector such that the concentration of ozone does not exceed the maximum permissible level All venting must be to outside air never within the building Ozon generation Ozone can be generated by radiation from the source lamps The maximum permissible exposure level is 0 1 ppm 0 2 mg m SD 1 Purification Solution System Manual 141 6 Appendix Solvent Miscibility Solvents should mix with each other in all proportions This is important during elution and during solvent changeover Refer to Figure 30 on page 142 for miscibility of some common HPLC solvents Acetic acid Acetone BB immiscible Acetonitrile Benzene __ Miscible Butyl alcohol Carbon tetrachloride Chloroform Cyclohexane Cyclopentane Dichloroethane Dichloromethane Dimethylformamide Dimethylsulfoxide Dioxane Ethylacetate Ethyl alcohol Di ethylether Heptane Hexane Methyl alcohol Methylethyl ketone Iso octane E Pentane Isopropyl alcohol Di Propylether Tetrachloroethane Tetrahydrofuran Toluene Trichloroethane Water in a
43. dio or antenna 2 Move the device away from the radio or television 3 Plug the device into a different electrical outlet so that the device and the radio or television are on separate electrical circuits 4 Make sure that all peripheral devices are also certified Make sure that appropriate cables are used to connect the device to peripheral equipment SD 1 Purification Solution System Manual 63 3 Installation 6 Consult your equipment dealer Agilent Technologies or an experienced technician for assistance 7 Changes or modifications not expressly approved by Agilent Technologies could void the user s authority to operate the equipment Removing the Front Panel 1 If installed remove the door from the Agilent 325 Detector see Removing the Door on page 71 for more information 2 Remove the panel on the front right side of the detector by unscrewing the captive screw in the top left corner of the panel Figure 13 Removing the front panel Hydraulic Connections Flowcells Hydraulic connections are located at the front of the Agilent 325 Detector The only line installed by the user where dead volume and low holdup are critical is the line from the column exit to the flowcell inlet port This line should be as short as possible The Agilent 325 Detector can be fitted with any one of four flowcells ordered separately Each one has an inlet and outlet connection and quartz optics cell 64 SD 1 Purification
44. e 22 on page 92 is used to connect the Agilent 440 Fraction Collector G9340A to the computer or MIB controlling the instrument Auxiliary Communication Port The auxiliary communications port provided on the Agilent 440 Fraction Collector G9340A is not used with current Agilent software or hardware Connecting the Fraction Collector to the HPLC System For details on setting up the fraction collector to the HPLC System see Setup the System with OpenLAB CDS ChemStation Edition Control Panel on page 102 Determining the Delay Time 1 For information refer to the online help of the Agilent 440 Fraction Collector Determining the Correct Probe Depth 1 For information refer to the online help of the Agilent 440 Fraction Collector 94 SD 1 Purification Solution System Manual Installation 3 Installing the RS 422 485 Communication Kit Installing the RS 422 485 Communication Kit 1 Connect the Serial extension cable R000815107 to the end of RS 422 connector on the Converter RS 232 to RS 422 893597601 Connection to the serial port on the computer il PC RS 232 Ez aa eee STAN ze Connection of the RS 422 Communication Cable to the RS 422 end of the RS 232 RS 422 Converter To Purification System 1 Converter RS 232 to RS 422 393597601 2 Serial extension cable R000815107 SD 1 Purification Solution System Manual 95 3 Installation 2 Connect the 9 pin D shell connector on th
45. e Agilent SD 1 Purification Solution allows to combine the modules listed above with the following Agilent 1200 Infinity Series modules Diode Array Detector G1315 C D Multiple Wavelength Detector G1365 C D Variable Wavelength Detector G1314 B C E F Preparative Autosampler G2260A Dual Loop Autosampler G2258A Fraction Collector G1364B Binary Pump G4220B Manual Injector G1328C combined with one or two Agilent SD 1 Pumps The option to combine several modules requires the Agilent OpenLAB CDS ChemStation software as master controller The SD 1 Solvent Delivery Module as master controller supports only the modules listed above SD 1 Purification Solution System Manual Introduction to the System 1 Introduction to the SD 1 Isocratic Solvent Delivery Module The Agilent SD 1 is an innovative HPLC solvent delivery system engineered with preparative chromatographers in mind Corrosion resistant titanium pump heads address the needs of biochemists for compatibility with salt containing buffers and freedom from unwanted metal ions Each pump head has a piston washing chamber to prevent deposition of abrasive salt residues behind the high pressure seal thereby greatly extending seal life Major new technology includes dual independent linear piston drives Rather than operating both heads from cams attached to a single motor as in conventional dual piston pumps the Agilent SD 1 uses two independent stepper motors which con
46. e RS 232 end of the Converter RS 232 to RS 422 893597601 to a serial communication port on the computer The screws on the RS 232 end of the RS 232 RS 422 Converter should be screwed into the nuts on the computer 9 pin D shell serial port connector 96 SD 1 Purification Solution System Manual Installation 3 Installing the Stream Splitter Agilent Stream Splitters are designed for preparative HPLC applications with flow rates up to 1200 mL min to split stream between preparative HPLC detector and an analytical detector If modules in the flow pass are not capable of the pressure the stream splitter must be installed PCG426000001 is designed for flow rates up to 200 mL min It uses 1 16 inch connection fittings PTFE tubing PCG426000002 is designed for higher flow rates up to 1200 mL min It uses 1 8 inch and 1 16 inch connection fittings PTFE tubing depending on the detector being used Some tubing s and fitting are supplied to connect with both preparative and analytical flow cells as required 1 Install the stream splitter as close as possible to the outlet of the UV detector the inlet of the ELSD and the fraction collector Cut the appropriate lengths of the chosen diameter tubing Install outlet from the UV detector to the IN port on the stream splitter Connect the OUT port on the stream splitter to the fraction collector oF Ww N Connect To Detector port in the back of stream splitter to the ELSD detector S
47. ed maximum ratings for the terminal block 3 use an auxiliary power relay to isolate the module from the instrument 46 2 Attach the connections for each terminal block see Table 2 on page 47 Table 3 on page 48 and Terminal Block 3 TB 3 Relay Output on page 48 SD 1 Purification Solution System Manual Installation 3 3 Replace the panel by carefully aligning the main connector and firmly pushing it in place 4 Tighten the captive screws finger tight Terminal Block 1 TB1 Analog Table 2 Terminal Block 1 TB 1 Analog Name Connection INTGR 1 HI Connect the high signal line from the channel A detector Range from 0 5 2 5 V INTGR 1 LO Connect the low signal line from the channel A detector INTGR 1 GND Connect the ground line if present from the channel A detector INTGR 2 HI Connect the high signal line from the channel B detector Range from 0 5 2 5 V INTGR 2 LO Connect the low signal line from the channel B detector INTGR 2 GND Connect the ground line if present from the channel B detector CHASSIS GND Connected internally to case ground CHASSIS GND Connected internally to case ground CHASSIS GND Connected internally to case ground ANALOG OUT The analog out connections are bi functional ANALOG GND 1 CHASSIS GND For wavelength control using a P325 UV VIS Dual Wavelength Detector connect this output to the External Wavelength
48. ense expires in 60 days 2 Set CIM parameters ee I E a ua BS Pepe gt Aosan Adcuonole rect Pogan P5325 E ouz Fraction colector E lt Instrument Curves Analog channel Acquisibon frequency dike bd Run tne 100m Relays Pulse wich 10s t LTO a T e e S ress Open Open Open lt mape Tene rar Rely 3 Rely 2 a Open 0pm I ii I E snow smetate graph L 3 Click OK to confirm method SD 1 Purification Solution System Manual R SD 1 Purification Solution System Manual e J a e ee 4 7 e Using Troubleshooting Maintenance a an and Parts Using Troubleshooting Maintenance and Parts 122 This chapter provides information on how to access further details on the system components te Agilent Technologies 121 4 Using Troubleshooting Maintenance and Parts Using Troubleshooting Maintenance and Parts 122 For details on using troubleshooting maintenance and necessary parts for the individual modules please refer to the according manuals Agilent SD 1 Isocratic Solvent Delivery Module User Manual G9302 90001 Agilent 325 UV VIS Dual Wavelength Detector User Manual G9309 90000 Agilent 410 Autosampler User Manual G9331 90000 Agilent 440 Fraction Collector User Manual G9340 90000 Agilent 218 Solvent Delivery Module User Manual G9300 90001 SD 1 Purification Solution System Manual SD 1 Purification Solution System Man
49. er to the according manuals e Agilent SD 1 Isocratic Solvent Delivery Module User Manual G9302 90001 Agilent 325 UV VIS Dual Wavelength Detector User Manual G9309 90000 Agilent 410 Autosampler User Manual G9331 90000 e Agilent 440 Fraction Collector User Manual G9340 90000 Agilent 218 Solvent Delivery Module User Manual G9300 90001 And to the User Manuals of the Agilent 1200 Infinity Series which allows combining with the modules listed above see Introduction to the System on page 8 Components of a Complete System Hardware Modules A complete system comprises following modules as ordered p n Description G9302A Agilent SD 1 Isocratic Solvent Delivery Module G9303A Agilent SD 1 Add on Solvent Delivery Module G9309A Agilent 325 UV VIS Dual WL Detector G9331A Agilent 410 Autosampler G9332A Agilent 410 Preparative Autosampler OPTIONAL G9340A Agilent 440 Fraction Collector SD 1 Purification Solution System Manual Software p n M8366 64000 M8367 64000 M8500AA M8301AA SD 1 Purification Solution System Manual Installation Description OpenLAB CDS Installation Driver Prep LC OpenLAB CDS Installation Upgrade Driver Prep LC LC driver OpenLAB CDS ChemStation Edition Workstation A 01 05 or higher 27 3 Installation Damaged Packaging If the delivery packaging shows signs of external damage please call your Agilent Technologies sales and service office immediately Inform your
50. ermine the flow rate increase on your preparative column F2 with the following formula F a x 1D x L2 N ID1 x Ly F1 F2 ID1 ID2 L1 L2 Flow rate on your analytical column Flow rate on your preparative column Inner diameter of your analytical column Inner diameter of your preparative column Length of your analytical column Length of your preparative column OR Determine the linear scale up factor LSF and then multiply your analytical flow rate and volume to determine your preparative scale flow rate and volume 1D x L gt LSF DFX ly LSF Linear scale up factor ID1 Inner diameter of your analytical column ID2 Inner diameter of your preparative column L1 Length of your analytical column L2 Length of your preparative column 2 Scale the method to maximum load on analytical column 3 Scale flow rate and loading for preparative column with same particle size and column length 44 SD 1 Purification Solution System Manual Installation 3 Installing the Solvent Delivery Module Electrical Setup Electrical Setup 1 Setup electrical connections 2 Check that the ON OFF power switch is off in the O position 3 Connect the power cord to the back panel of the module and plug it into a grounded power socket A good ground connection is necessary to ensure safety for users and proper communications 4 Turn on the power switch If the pump does not start check following items 1
51. etector Module Place the detector conveniently near your HPLC system The modular design of the detector enables you to locate it anywhere within the limitations imposed by the length of the power cord fluid lines and signal cables In order to keep liquid dead volume as low as possible and to minimize peak broadening in the lines the distance between the column outlet and the flowcell inlet should be kept to a minimum For best performance the detector should be located on a clean sturdy vibration free bench in an area free of Heat sources such as direct sunlight or a heater vent Drafts such as an open doorway window or air conditioner vent e Smoke or UV absorbing vapor Corrosive or dusty atmosphere Potential liquid spills Provide approximately 4 inches of space behind the unit so that the cooling fan intake is not impeded and to allow easy access to the rear panel services see Power Connection and Rear Panel Services on page 61 SD 1 Purification Solution System Manual Installation 3 Power Connection and Rear Panel Services Power Connection and Rear Panel Services WARNING Electrical shock Risk of stroke and other personal injury gt Turn off the power to the detector before making power and signal cable connections The detector can communicate with other modules and devices in the entire HPLC system All power and signal connections are made on the rear panel of the detector see Figure 12 on pa
52. f the Autosampler Module The best place to install your Agilent 410 Autosampler is at the top of the module stack This stack would normally be solvent delivery module on the bench detector on top of the SDM and finally the AutoSampler From the right hand side you have the shortest connection to the injection valve of the Agilent 410 Autosampler to the column 72 SD 1 Purification Solution System Manual Overview of the Module Figure 16 Autosampler overview Installation 3 Installing the Autosampler 1 Vial wash drain 2 Condensed water and leakage drain 3 Tray fixation knob 4 Sample tray 5 Syringe dispenser SD 1 Purification Solution System Manual 73 3 74 Installation 10 11 12 13 Keyboard Buffer tubing Needle arm Injection valve Oven compartment Tubing guide Wash position Position for transport solvent and reagent vials The rear view of the autosampler is shown in Figure 17 on page 75 SD 1 Purification Solution System Manual Installation 3 Installing the Autosampler WARNING RISK OF ELECTRIC SHOCK DISCONNECT POWER BEFORE SERVICING AVERTISSEMENT RISQUE DE CHOC ELECTRIQUE COUPER L ALIMENTATION AVANT LA MAINTENANCE Mt RI Fit area FUSE nating WARNING RISK OF FIRE AVERTISSEMENT RISQUE DE FEU REMPLACEZ FUSE COMME INDIQU 230 1
53. ge 61 The connectors on the rear panel support communication configurations to a wide range of Agilent modules and non Agilent devices Main power receptacle J1 Comm J4 Relay out J14 Analog out P9 Sync signal J10 Sync signal Figure 12 Agilent 325 Detector rear panel services The following table summarizes the function of each connection SD 1 Purification Solution System Manual 61 3 62 Installation Table5 Rear panel services functions Connection Function Main power receptacle 3 pin receptacle with 2 fuses J14 Analog out 9 pin female D shell connector used for two channels A and B of analog output J4 Relay out 15 pin female D shell connector used for time programmed contact closures J1 Comm RJ 45 type connector used to interface the Agilent 325 to a desktop PC P9 Sync signal 15 pin male D shell connector used with synchronization signal cable J10 Sync signal 9 pin female D shell connector used with synchronization signal cable For more information about the connections see chapter Cables AC Power The Agilent 325 UV VIS Dual Wavelength Detector may be connected to any voltage in the range 100 240 VAC 10 50 60 Hz 1 Hz single phase without modification or the need to change fuses Before connecting power to the detector ensure that the power switch on the front of the instrument is OFF the rocker switch O is pressed The power switch is a rocker s
54. herein Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms the warranty terms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcon tract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commercial item as defined in FAR 2 101 a or as Restricted computer soft ware as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or dis closure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION notice denotes a hazard It calls attention to an operating procedure practice or the like that if not c
55. ils on specifications of the individual modules please refer to the Agilent 1200 Infinity Series Specifications Compendium or to the corresponding User Manuals 22 SD 1 Purification Solution System Manual SD 1 Purification Solution System Manual 3 Installation Delivery 26 Damaged Packaging 28 Check Delivery 29 Delivery Checklists 29 Unpacking and Inspection 32 Optimizing the Stack Configuration 37 Isocratic System 38 Gradient System 39 Auto Preparative System 41 Scale up the HPLC System 42 Installing the Solvent Delivery Module 45 Electrical Setup 45 Plumbing Connections 200 to 800 mL Pump Heads 51 Plumbing Connections 3 2 L Pump Head 54 Pump Head Installation 56 Priming the Pump Heads 58 Flushing the HPLC System 59 Installing the Detector 60 Location of the Detector Module 60 Power Connection and Rear Panel Services 61 Avoiding Harmful Interferences to Radio or Television Reception 63 Removing the Front Panel 64 Hydraulic Connections Flowcells 64 Installing a Flowcell 66 Detector Outlet Back Pressure Restrictor 69 Installing the Door 70 Removing the Door 71 Ee Agilent Technologies 23 3 24 Installing the Autosampler 72 Location of the Autosampler Module 72 Overview of the Module 73 Installing the Sample Tray 76 Connecting the Waste Tubings 76 Starting the Autosampler 78 Rinsing the System with Wash Solvent 79 Connecting to the Autosampler 80 Filling and Sealing the Vials 81 Loading the
56. ing protrudes from the end of the probe Secure the lower knurled mount nut to the top knurled mount nut co Secure the nut holding the metal probe into the bottom of the lower knurled mount nut 9 Clip the tubing into the tube restraint which is the small hook at the top of the Z axis slider Allow for a small length in the tubing to prevent kinking the tubing 10 Run the tubing along the back side of the probe arm housing SD 1 Purification Solution System Manual 87 3 Installation Installing the Fraction Collector 11 Attach the split ring also called the retaining ring as shown below The retaining ring is split to attach it through the loop on the underside of the probe arm housing a Split ring retaining ring 12 Feed the tubing through the retaining loop attached to the underside of the housing 13 Screw the tubing fitting into the bottom port 3 of the valve Port 1 to waste Port 2 from detector outlet or back pressure restrictor Port 3 to the probe NOTE It is important to ensure that the length of the tubing from the probe to the valve allows the probe arm to move freely in all axes If it is too tight it will restrict movement and may cause movement failure If it is too loose the probe arm may become tangled in the tubing as it moves Tubing length between the valve and the detector depends on fraction collector placement When choosing the length of tubing ensure it is lo
57. ing on Activate communication Information Communication established with COM2 is visible on the screen SD 1 Purification Solution System Manual Terminating configuration Installation Setup the Software 1 Before closing the Configure Instrument windows deselect the 3D spectral evaluation check box Conteguraibie Mosses EDS reen 12700 Bic sree 12800 Agilent Prep iC Qe amp Pure HF oar th Fraction Cotecor Generic Modules emt crise ceriey wx Aak for configuration charge at Oam Raton aatup 2 Click OK Selonteot Modes Agitent Prep LC Ato Contigrton Qe verre ps rwrsxsono HH eaor P5325 L0z129021 Fraton collector 14408C AY1TOTMOTS You re back in Agilent OpenLAB Control Panel SD 1 Purification Solution System Manual 109 3 3 Installation S he Setup Method 1 Select Launch to start the OpenLab CDS Chemstation Edition is i i si 7 h X Edit Delete Refresh Edit Lock Create Configure Notifications Shortcuts Instrument Instruments and Locations Properties Actions Navigation Not Connected mam Instruments Start Instrument 3 Prepic a Launch Launch Offline EL instruments X Administration Your startup license expires in 60 days 110 SD 1 Purification Solution System Manual Installation 3 Setup the Software 2 Set Pumps parameters 3 Click OK to confirm method SD 1 Purification So
58. input of the detector For wavelength control a 1 V analog output from the pump equates to 100 nm from the detector Alternatively analog out can be used to output the pressure signal in mV when the contacts are not used for wavelength control and when the ANALOG PRESSURE MONITOR menu item in the SD 1 pressure menu is selected to ON For Analog Out 1 V 1000 psi 68 bar or 6 9 MPa The pressure signal output is cancelled when using these outputs for wavelength control Connected internally to case ground SD 1 Purification Solution System Manual 47 3 Installation Terminal Block 2 TB 2 Digital Input Table3 Terminal Block 2 TB 2 Digital Input Name Connection STOP D GND HOLD TRANSFER INJECT D GND MARK D GND AUX 5V CHASSIS GND Contact closure sends a stop pump signal to the Agilent SD 1 which will send it to the data system software controlling the instrument If there is no shutdown method specified this input stops the pump immediately and informs the instrument control software that the pump has stopped If there is a shutdown method specified control will branch to that method either immediately or after the current method pass depending on the preference set Contact closure sends a hold flow rate signal to the instrument control software Contact closure duplicates the HOLD key on the front panel Contact closure sends a transfer method signal to the instrument
59. ion Signals 3 G C Q E e v Figure 29 The 0 adapter board 134 SD 1 Purification Solution System Manual SD 1 Purification Solution System Manual 6 Appendix General Safety Information 136 Solvent Miscibility 142 The Waste Electrical and Electronic Equipment Directive 143 Batteries Information 144 Radio Interference 145 Electromagnetic Compatibility 146 Agilent Technologies on Internet 148 This chapter provides addition information on safety legal and web Apg Agilent Technologies 135 6 Appendix General Safety Information General Safety Information The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements WARNING Ensure the proper usage of the equipment The protection provided by the equipment may be impaired gt The operator of this instrument is advised to use the equipment in a manner as specified in this manual 136 SD 1 Purification Solution System Manual Appendix 6 Information Symbols The following is a list of symbols that appear with warnings in this manual or on the liquid chromatograph The hazard they desc
60. k pressure restrictor 110743300 should be added to all flow cells unless a fraction collector is installed after the detector The back pressure restrictor assembly that was supplied with your detector should be threaded into the outlet line from the flowcell The back pressure restrictor applies approximately 2 76 bar 40 psi back pressure on the flowcell This prevents outgassing and bubbles from forming or being trapped in the flowcell which can cause an unstable baseline Note the arrow stamped on the restrictor body This arrow must point away from the flowcell outlet port and toward the waste receiver The threaded plastic fittings should be finger tightened only enough to prevent leaks About 122 cm 48 of 1 6 mm 1 16 tubing is supplied at both the inlet and outlet of the restrictor The inlet tubing is provided with a 1 6 mm 1 16 plastic tubing fitting for connecting to the flowcell outlet port Either the outlet tubing can be directed to the waste container or the tubing removed and the restrictor itself dropped to the bottom of the waste bottle SD 1 Purification Solution System Manual 69 3 Installation Installing the Detector The restrictor pressure setting is not adjustable If the restrictor fails or becomes plugged replace the existing cartridge with a new 2 76 bar 40 psi replacement Installing the Door The module door may be attached to the front of the Agilent 325 Detector to cover the tubing connectio
61. l 67 3 Installation 3 Remove the front panel see Removing the Front 4 Carefully position the flowcell so that the two Panel on page 64 for more information thumbscrews are positioned in the threaded holes in the flowcell compartment a Push at the center of the flowcell to ensure it is positioned squarely in its housing and that it is not tilted in any way It is critical to the performance of the detector that the flowcell is inserted correctly The internal optical components of the flowcell are an integral part of the detector s optical system If the flowcell is not fitted correctly it will have an adverse effect on detector performance 68 SD 1 Purification Solution System Manual Installation 3 Next Steps 5 Secure the flowcell by tightening the thumbscrews with your fingers Alternate tightening the thumbscrews until they are snug 6 Replace the front panel For optimum performance the detector should be operated with the front panel in place This is because the foam on the inside of the panel stops breezes which may cause instability and noise from reaching the flowcell The flowcell should be removed with the connecting tubing fitted These must be removed outside the detector compartment 7 Perform a lamp calibration see chapter maintenance in Agilent 325 UV VIS Dual Wavelength Detector User Manual G9309 90000 Detector Outlet Back Pressure Restrictor The Bac
62. lution System Manual 111 3 Installation Setup the Software 4 Set Autosampler parameters 5 Click OK to confirm method 112 SD 1 Purification Solution System Manual Installation 3 Setup the Software 6 Set Autosampler Injector Program 7 Click OK to confirm method SD 1 Purification Solution System Manual 113 3 Installation Setup the Software 8 Set PS 325 parameters W P5325 Fraton colector NOTE The Run time must be defined to the detector parameters 9 Click OK to confirm method 114 SD 1 Purification Solution System Manual Installation 3 Setup the Software 10 Set Fraction collector 11 Click OK to confirm method Setup is completed SD 1 Purification Solution System Manual 115 3 Installation Setup the CIM in the OpenLAB CDS ChemStation PrepLC Drivers Parts required Preparations 116 The Control Interface Module CIM in the OpenLAB CDS ChemStation PrepLC Drivers can be used for acquiring signals from extern detectors If 218 SD 1 and 1260 modules are connected via remote cable error messages will be properly relayed With the remote cable it is also possible to run 218 SD 1 preparative HPLC system with any Agilent 1200 Infinity Series detector using the CIM as trigger source for fractionation For this analog input interface one or two 218 SD 1 pump modules can be mixed The CIM offers differe
63. lution pumps Scale up the HPLC System Model Agilent 218 37251 C3 injection pump rame Prep inj Prep column Detector Pump A 50 mL min valve valve model SD 1 Inline et 200 mL min Mixer filter Tee pump head QO ea Jh Prime 7030 ial purge Switch Jb i pB valve valve C miadel SD 1 lt Analytical or 200 mL min 7125i scout column pump head Analytical EN ace valve PC L G Waste WUUWUUY Sample Solvent A Solvent B Taction collector Start gradient z from 20 Model SD 1 to XX B for separation Reduce flow to 7 ve at Injection for injection Injection pump K Elution pump The diagram shows the SD 1 based system for preparative scale up The system is controlled by a PC using instrument control software The two elution pumps are Agilent SD 1 s with 200 mL min pump heads fitted Downstream from the elution pumps is a high pressure mixer filter drain valve and a switching valve The switching valve selects between the analytical components injection valve column and the preparative components preparative injection valve preparative column In this example both a preparative injection valve and an injection pump are shown this provides more flexibility The injection pump is an Agilent 218 with a 50 mL min head SD 1 Purification Solution System Manual Installation 3 The injection pump s outlet is sent to a tee upstream of the preparative column The eluent from either column fl
64. nect to pistons via linear screw drives The motors reciprocate rather than running only in one direction Independent drive frees the Agilent SD 1 from the operating constraints of mechanical cam profiles and makes it the first dual piston pump to produce entirely pulse free flow under all operating conditions without auxiliary hydromechanical pulse dampers Totally pulse free flow favors improved column performance and extended column life by saving expensive preparative columns from the constant pressure pulse pounding typical of other large piston and diaphragm pumps In addition the Agilent SD 1 meters flow at a constant rate independent of solvent compressibility and without the slight refill associated flow deficits seen with conventional single motor dual piston models In gradient operation this produces more precise composition profiles without the time and volume delays introduced by large mixing chambers Plus flow rates extend well into the analytical HPLC range permitting method development on smaller columns without interchanging heads Each Agilent SD 1 pump includes a standard serial interface for flow control A built in two channel analog to digital converter allows the computer to collect data from HPLC detectors Contact closure inputs and outputs are provided for system automation Firmware includes Good Laboratory Practices GLP logging features SD 1 Purification Solution System Manual 9 1 Introduction to the S
65. ng enough to allow free movement of the arm but not too long to delay sample delivery into the tubes If the tubing is too long between the detector output and the fraction collector probe end your samples may not correspond correctly to the fraction collector markers on your chromatogram The delay volume calculation will compensate for this effect 14 Move the probe arm to the front right side of the fraction collector and rotate the probe arm fully to the right to check that the tubing is completely free to move 15 Manually position the probe arm in the middle along the X axis 16 Rotate the probe arm through its full extent to check that the tubing is free to allow full movement in all directions 88 SD 1 Purification Solution System Manual Installation 3 If the length is not correct remove and then replace the tubing install the fittings and tubing onto the fraction collector Repeat step 14 on page 88 step 16 on page 88 to test the tubing length 17 Adjust the length of the sample line from the HPLC system In port 2 see Figure on page 88 screw in the fitting with ETFE tubing Connect the other end of this tubing to the HPLC system s detector outlet or to the back pressure restrictor if one is present This tubing should be as short as possible 18 In port 1 see Figure on page 88 screw in the fitting with PTFE tubing Put the other end of the tubing into your waste container Assembling the Sample Racks CAUTION Lo
66. njection performance degrades And if necessary the entire injection valve can be replaced in seconds with the unique Quick fit valve mounting mechanism 12 SD 1 Purification Solution System Manual Introduction to the System 1 Agilent 410 Preparative Autosampler G9332A By just choosing Prep mode in your system settings you can use the Agilent 410 Autosampler to inject all of your sample into a Preparative LC system or in other areas where large injection volumes are required The combination of large sample vials 10 mL a large sample volume needle and a 2 5 mL syringe enable you to inject large volumes very reproducible with high speeds and only 45 uL of sample loss The installed large bore valve 0 75 mm with 10 mL sample loop enables you to inject from microliters to milliliters with the same AutoSampler Flow rates up to 200 mL per minute are possible when in the Prep mode Table 1 Tubing of the Agilent 410 Autosampler prep option Tubing Material Dimensions Volume LSV sample needle Stainless Steel 70 mm x 0 81 mm o d x 0 51 mm i d 45 uL and tubing LSV sample needleto ETFE 155 mm x 1 16 o d x 0 50 mm i d 45 uL high pressure valve Buffer tubing from PTFE 2550 mm x 1 16 o d x 1 mm i d 2000 pL high pressure valve to syringe valve If the Prep option is factory installed the installation instructions can be skipped If the Prep option is bought as a kit carry out the installation instructions see Ins
67. ns to the flowcell ITE If the Agilent 325 Detector is the top module in the stack the door cap should be installed before installing the door on the module Installing the Door Cap If the Agilent 325 Detector is not at the top of the stack do not install the cap and proceed to the instructions describing door installation 1 Stand the door upside down on a flat surface i e with the two ribs towards the bottom Ribs Magnetic latch Door cap z Figure 14 Installing the door cap 70 SD 1 Purification Solution System Manual Installation 3 Installing the Detector 2 Take the cap and remove the protective paper exposing the adhesive that will attach the cap to the door 3 Insert the cap into the door and press the adhesive onto the inside of the door lip Be sure to keep the door edges and cap edges flush Installing the Door 1 Insert the top hinge pin into the top hinge 2 Gently press down on the top of the door and slide the lower hinge pin into the lower hinge The door should now pivot on the pins and close The magnetic door latch should stick to the instrument Figure 15 Installing the Agilent 325 Detector door Removing the Door 1 Gently push down on the door and slide the lower hinge pin out of the lower hinge 2 Lift and slide out the top of the door SD 1 Purification Solution System Manual 71 3 Installation Installing the Autosampler Location o
68. nt Technologies sales and service office SD 1 Purification Solution System Manual SD 1 Pump A Personal Computer SD 1 Pump B Converter RS232 to RS 422 Serial COM port Installation 3 Connecting Cables to the Injection Pump Start and stop of the injection pump is controlled by a contact closure which is set up in the external event table in the PC configuration 1 Connect a cable between the inject and ground of the injection pump to a contact closure on the SS 420 board Connect a cable between stop and ground of the injection pump to another contact closure on the SS 420 board Set up the trigger of these contact closures at the appropriate time in the external event table The injection pump must not be on the bus or it will limit the maximum flow rate to the maximum allowable system flow rate of the injection pump Serial Interface Connections for Remote Control Figure 6 Connections for instrument control software IBM PC compatible SD 1 Purification Solution System Manual 49 3 50 Installation Plug the serial interface cable into serial COM port 1 on the back of the PC Connect the serial interface cable with the RS 232 to RS 422 converter The four 9 pin female connectors on the serial interface cable are all equivalent Connect one of the connectors to the serial interface port on each SD 1 pump being used Extra connectors
69. nt features from the ability to configure the module to establish communication with the module and re establish in case of communication loss e to edit the CIM detector method to perform a run and acquire data to view the CIM status in the RC NET Status Dashboard e to activate the CIM relays manually to monitor the CIM signal to fractionate and to detect the 440 Fraction Collector peaks on the CIM signal p n Description 5062 3378 Remote cable OpenLab CDS Chemstation Control Panel is configured as described in Setup the CIM in the OpenLAB CDS ChemStation PrepLC Drivers on page 116 SD 1 Purification Solution System Manual Installation 3 1 Select Configure Instrument PEO ER R Edit Delete Refresh Lock Create Configure Edit Notifications Shortcuts Instrument Instruments and Locations Properties Actions Navigation PrepLc Not Connected EEEE Instruments Start Instrument X Prepic iann Launch omne EE instruments X Administration Your startup license expires in 60 days 2 Select No to avoid the auto configuration It doesn t work with this version peers Z 20 woas evaluation T Enable rteigert Repoting Configurable Mosses Selected Moses Agilent LC Modules and System e Ato d Fracton Colector d Congr sha tow Pow Fraction Colector iroa 2 HP Sampler Ors trony cergetin f I 4 2 Low Row HP Sampler There s ne configuration salable for this instrument De you want t
70. o i My vacrccnteyret Aak tor configuration change at Chem Staton satup ox Cancel Hep SD 1 Purification Solution System Manual 117 3 Installation 3 Select the 218 SD 1 CIM on the left panel of the Configurable Modules Agilent LC Syst len tlem g ys TI 3D spectral evaluation Use classic drivers VE Intelligent Reporting Method load on startup Always ask user to choose an option Zz Configurable Modules Selected Modules Agilent LC Modules and Systems Agilent LC Modules and Systems Auto e 410 Autosampler Configuration QD suorana P5419 at 218 SD 1 Purp GE Puros PS21S01 ne B r 3 440 Fraction Colector Fraction Collector ae Low Flow Fraction Collector Sampler Q HP Sampler Additional configuration _careet_ __Heb 4 Click to add the modules to the Selected Modules The configuration dialog for the selected module opens 5 Doubleclick in Configurable Modules on 218 SD 1 CIM 218 SD 1 CIM Configuration dialog opens Select the COM Port the CIM Model Detector ID and enter the ID value 7 Verify the connection by clicking on Activate communication r 218 SD 1 CIM Configuration Instrument 1 a COM Port COM2 X 1D 5 CIM Model 210 218 X Detector ID 1 Ea Activate communication FW version CM300V1 1 i Communication established with COM2 OK i Cancel Help E d 118 SD 1 Purification Solution Sy
71. occurs by an Ethernet connection Communication by an Ethernet connection is required to control the detector remotely by OpenLAB When the Workstation provides HPLC system control the synchronization cables from P9 and J10 are not used To create an Ethernet connection insert an RJ45 cable included in the ship kit into the J1 receptacle and into the PC The Ethernet cable that comes with the detector is a cross over cable which is appropriate for connecting the detector directly to a PC Connecting the detector to a network or a hub will usually require a patch cable A Ethernet cable for use in a network 392612901 can be purchased from Agilent or either locally Most PCs come pre configured with an Ethernet connection which is usually built into the motherboard or with an Ethernet network card installed However if you have a PC that has no network interface you will need to install and configure a Network Interface Card PCI bus The PC must have a spare PCI slot for the installation of this device You are also responsible for setting up and maintaining any LAN configuration where a detector may be used All network issues are to be dealt with by the user SD 1 Purification Solution System Manual Cables 5 Synchronization Signals Synchronization Signals The synchronization signals at P9 and J10 are used to synchronize the operation of a group of instruments that are not interfaced to OpenLAB The synchronization signals come
72. om the power line at any time gt Make sure the power connector of the instrument can be easily reached and unplugged gt Provide sufficient space behind the power socket of the instrument to unplug the cable 18 SD 1 Purification Solution System Manual Site Requirements and Specifications 2 Power Cords Different power cords are offered as options with the module The female end of all power cords is identical It plugs into the power input socket at the rear The male end of each power cord is different and designed to match the wall socket of a particular country or region Absence of ground connection or use of unspecified power cord The absence of ground connection or the use of unspecified power cord can lead to electric shock or short circuit gt Never operate your instrumentation from a power outlet that has no ground connection gt Never use a power cord other than the Agilent Technologies power cord designed for your region Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury gt Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Unintended use of supplied power cords Using power cords for unintended purposes can lead to personal injury or damage of electronic equipment gt Never use the power cords
73. on J Enable reeigert Repotng 2 Sects Empty confguration euto configure a Gen Ch Rh na o Pump Yes Aak tor configuration change at ChemStaton statue f 2 Low Plow HP Sampler i There is ne configuration available for this instrument De you want to i x Cancel Hep 6 The left panel of the Configurable Modules contains the Agilent Prep LC Ortens Agilent LC System Use classe devers Ti 2D spectra evatuaton 7 Enable rtebgert Rrpoting Contgurabie Mosses EPs Sten zinc pi sree rasa Aak for confiqueition change at ChamStaton startup Additional configuration x Orce Hep 7 Select the module you have available in your system 8 Click to add the modules to the Selected Modules The configuration dialog for the selected module opens 104 SD 1 Purification Solution System Manual Installation 3 Pump Configuration 1 Doubleclick in Configurable Modules on Pump Pump Configuration dialog opens 2 Select the COM Port as COM 1 and the desired Pressure unit bar available kPa PSI bar MPa Pump Configuration Instrument 1 a COM Port com Numberofpumps 2 Pressure unit bar 5 E Injection pump present Pump ID Model Firmware Head version A 1 PrepStar SD 1 wv HPXLV2 0SD300V1 1 200mL Titanium B 2 200mL Titanium SD 1 CIM Control CO Use D 1 CIM for manual injection Activate communication i
74. ories Three racks are included with the fraction collector and are made of polypropylene to resist most chemical spills Up to three racks of many configurations can be placed on the fraction collector Additional sample racks can be set up in sequence and manually changed during an analysis as each rack s analysis is completed The rack closest to the rear of the fraction collector next to the pillar is considered rack number one SD 1 Purification Solution System Manual 15 1 Introduction to the System Introduction to the Agilent 440 Fraction Collector 16 SD 1 Purification Solution System Manual R SD 1 Purification Solution System Manual e e r a o e 00 e 2 7 e Site Requirements and Specifications e i Site Requirements 18 4 Specifications 22 This chapter provides information on site requirements and specifications of your system ea Agilent Technologies 2 Site Requirements and Specifications Site Requirements Power Considerations The instrument power supply has wide ranging capability It accepts any line voltage in the range described in Physical Specifications Hazard of electrical shock or damage of your instrumentation can result if the devices are connected to a line voltage higher than specified gt Connect your instrument to the specified line voltage only CAUTION Inaccessible power plug In case of emergency it must be possible to disconnect the instrument fr
75. orrectly per formed or adhered to could result in damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated condi tions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indi cated conditions are fully under stood and met SD 1 Purification Solution System Manual In This Book In This Book This manual provides setup information on following modules e Agilent SD 1 Solvent Delivery Module G9302A G9303A e Agilent 325 UV VIS Dual WL Detector G9309A e Agilent 410 Autosampler G9331A G9332A e Agilent 218 Solvent Delivery Module G9300A G9301A e Agilent 440 Fraction Collector G9340A 1 Introduction to the System This chapter introduces to the Agilent SD 1 Purification Solution system and its components 2 Site Requirements and Specifications This chapter provides information on site requirements and specifications of your system 3 Installation This chapter gives information about the installation of your Agilent SD 1 Solvent Delivery Module Agilent 325 UV VIS Dual WL Detector Agilent 410 Autosampler and Agilent 440 Fraction Collector 4 Using Troubleshooting Maintenance and Parts This chapter provides information on how to a
76. over 172 bar up to 172 bar 500 800 mL min 0 318 cm 1 8 inch PEEK tubing Ferrule collar PEEK ferrule up to 172 bar 3 2 L min 0 635 cm 1 4 inch Heat forming flare 1 Unit conversion 172 bar 2500 psi 17 2 MPa 52 SD 1 Purification Solution System Manual Installation 3 Small opening at top Figure 7 Detail of PEEK ferrule and ferrule collar Tools required Description Wrench open ended 5 16 inch 1 Remove the plug from the outlet tee port a Store the plug in a safe place Assemble the ferrule and ferrule collar for PEEK tubing and compression fitting onto the outlet tubing see Table 4 on page 52 Assemble the ferrule and ferrule collar for PEEK tubing and compression fitting onto the outlet tubing as shown a For PEEK ferrules place the ferrule collar onto the shoulder of the ferrule large opening toward the ferrule The collar will seat properly as you tighten the fitting Holding the compression fitting ferrule and collar in place on the tubing push the end of the tubing as far as possible into the port on the outlet tee Carefully thread the compression fitting into the outlet port on the tee Tighten the compression fitting finger tight Tighten the fitting in the outlet tee with the 5 16 inch open ended wrench and tighten turn past finger tight Immerse the other end of the outlet tubing into the solvent in the reservoir and tape the outlet tubing firmly to the
77. ows to the detector flow cell then to collection Processing the Scale up The HPLC system has all the characteristics necessary to effectively handle both analytical and preparative HPLC with small particle columns As with all method development one needs to develop analytical methods which meet purity requirements For example there may be a specific contaminant which must be completely removed while other peptides must be lower than some specific level and specific buffers or salts may be prohibited Once purity requirements are met with the analytical method the method is scaled up to maximum load on the analytical column Again knowing purity requirements is very beneficial since sample displacement with an overloaded column can often provide adequate resolution with greatly increased loading capacity compared to a separation with optimal efficiency Once the analytical method is perfected all that is needed is to increase the flow rate and loading by the ratio of the cross sectional areas Maintaining the same particle size linear velocity and proportional load will give the same results with a prep column as with an analytical column The next step is to develop a strategy for scale up from analytical to preparative purifications of protein samples There are three basic steps to scale up SD 1 Purification Solution System Manual 43 3 Installation 1 Develop the analytical separation method to meet purity requirements Det
78. ploy static measuring and static discharge devices to safeguard against the buildup of static electricity gt In unattended operation do not use organic solvents having an ignition point below 70 C gt Do not bring a heat or flame source near the instrument gt The area in which solvents are stored and the area surrounding the instrument must be adequately ventilated to prevent accumulations of gas gt Always check the condition of the instrument leakage of solvent or waste solution leakage of solvent inside the instrument If an abnormality is found stop operation immediately gt When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste gt Use only approved regulator and hose connectors refer to the supplier s instructions gt Keep solvents cool and properly labeled Ensure that you have the correct solvent before connecting it to the instrument SD 1 Purification Solution System Manual 139 Appendix WARNING Inflammation or injury due to toxic corrosive or stimulative solvent gt Do not contact toxic corrosive or stimulative solvent gt For details of the properties of each solvent and how to handle it refer to the relevant Material Safety Data Sheets MSDS gt Be sure to handle each solvent properly gt Wear proper personal protective clothes e g safety goggles
79. r coding and physical design of the cable connectors ensure that correct signals and polarity are matched The outputs are optical isolators and simulate a relay contact closure when they are activated see Figure 28 on page 132 The minimum requirement for an input signal to be detected is 200 ms OUTPUT 57 Figure 28 Input output schematics 132 SD 1 Purification Solution System Manual Table 7 Signal Enable Out Ready In Ready Out Start In Start Out Fault In Fault Out Auto zero Lamp off Cables 5 Signal Description J10 and P9 Description A non polarized constantly active output a short This output can be used to activate Enable In on the next instrument When Enable Ready In is set software switch this polarized input signal must be present before the Agilent 325 Detector can go to the Ready state Specifically when the Agilent 325 Detector is in the NOT Ready Lamp On state on receiving a Ready In signal a monitor period will occur after which the Agilent 325 Detector goes to the Ready state It must stay active until the Agilent 325 Detector starts Ready In will be ignored in all other states This polarized output signal indicates that the Agilent 325 Detector is in the Ready state and is ready to start a time program This polarized edge triggered input signal will start the active method if the Agilent 325 Detector is in the Ready state This polarized output signal will be
80. raction Collector Installing the Spill Tray Alignement pin underneath the raised location tabs Back side of the fraction collector closest to the fraction Figure 19 Spill tray alignment pin and mat for the rack location raised locating tabs Preparations Position the fraction collector closest to the detector output This decreases the delay volume NOTE The spill tray will catch most solvent spills Always clean up spills immediately 1 Locate the alignment pins protruding above the base support tube 2 Lower the tray so that the two alignment pins closest to the fraction collector pillar fit into the slots in the spill tray 3 Lower the spill tray until the front edge rests on the front of the base support tube 4 Check that the spill tray is firmly pushed down on all alignment pins NOTE The spill tray must be firmly in position so that it does not move SD 1 Purification Solution System Manual 85 3 Installation Installing the Rack Location Mat The rack location mat is installed on top of the spill tray Preparations Spill tray installed There are cut outs around the rack location mat The cut outs slot over the raised locating tabs that are molded into the spill tray to ensure proper alignment see Figure 20 on page 90 1 Position the rack location mat over the spill tray and press the mat onto the locating tabs 2 Check that the rack location mat fits firmly in place by trying to move it side to
81. ribe is also shown A triangular symbol indicates a warning The meanings of the symbols that may appear alongside warnings in the documentation or on the instrument itself are as follows Table 8 Warning symbols gt gt gt Broken glass Chemical Electrical hazard gt gt Explosion Eye hazard Fire hazard hazard Hot surface g ee lt f 9 9 lt lt weight danger to danger to hands gt gt Moving parts Respiratory Attention hazard 1 The symbol may be used on warning labels attached to the instrument When you see this symbol refer to the relevant operation or service manual for the correct procedure re ferred to by that warning label SD 1 Purification Solution System Manual 137 6 138 Appendix Table9 Information symbols Symbol Description l Mains power on 0 Mains power off eS LA Single phase alternating current Direct current Confirms that the product complies with the requirements of all applicable European Community directives SD 1 Purification Solution System Manual Appendix 6 Solvent Hazards WARNING Explosion fire asphyxiation This instrument is not explosion proof Certain solvents may cause weakening and leaks of tubings or fitthings with possible bursting Even small leaks in solvent supply systems can be dangerous gt Only use solvents compatible with the HPLC system tubings and fittings gt Em
82. rval equal to the Peak Sense duration parameter as stored in the method The Peak relay can be activated from any of the following sources only one source can be active at any one time Time Slice event Once time slice has been turned on it will provide a periodic activation of the Peak Sense relay at an interval defined in Time Slice period within the method Time Slice can be turned on and off by time e Pulse event A single timed programmed activation of the Peak Sense relay as defined in the method Peak sense has been turned on To connect open ended wires to the relay signals available at J4 use the optional Assy PWB relay interface 325 210187590 see Figure 26 on page 128 Simply plug this PWB into the rear panel connector 5 P Figure 26 Relay output board 128 SD 1 Purification Solution System Manual Cables 5 The Relay interface cable for relay interface board one relay contact per cable 110743800 is used to attach to the 3 pin connectors at the relay output board With the 3 pin connectors the contact closure is between pins 1 and 2 of the plugs Pin 3 is connected to ground The relay interface cable has three open ended wires The relay contact is connected between the clear and the black wire The green wire is connected to ground SD 1 Purification Solution System Manual 129 5 Cables Desktop PC Communications 130 Communication between the detector and a desktop PC
83. service representative that the instrument may have been damaged during shipment CAUTION Defective on arrival problems If there are signs of damage please do not attempt to install the module Inspection by Agilent is required to evaluate if the instrument is in good condition or damaged gt Notify your Agilent sales and service office about the damage gt An Agilent service representative will inspect the instrument at your site and initiate appropriate actions 28 SD 1 Purification Solution System Manual Installation 3 Check Delivery Delivery Checklists Delivery Checklist Pump The pump is packed in a single carton The pressure module ordered with the pump is shipped separately and needs to be installed Any pump head ordered with the pump is packed separately The following list shows all items delivered in a standard delivery Your personal list depends on your order therefore countercheck delivery with your order Agilent SD 1 Solvent Delivery Module e Power cord Solvent inlet assembly Compression fitting e Ferrule Pump head kit Plumbing kit e Pressure transducer module Mast kit Internal mixer SD 1 Purification Solution System Manual 29 3 Installation Delivery Checklist Detector The following list shows all items delivered in a standard delivery Your personal list depends on your order therefore countercheck delivery with your order Agilent 325 UV VIS Dual Wavelength detector
84. ss of sample If a tube sits at an angle in the rack the probe may hit the side of the tube as it enters or leaves the tube This can affect the alignment of the probe and or damage the tube gt Ensure that the tubes sit vertically within the sample rack 1 Follow the manufacturer s instructions to assemble the sample racks 2 If needed Insert the overlay by placing the overlay over the top of the rack SD 1 Purification Solution System Manual 89 3 Installation Installing the Sample Racks 1 Standard racks Fit the pegs on the rack into the holes on the rack location mat The rack closest to the pillar of the fraction collector is considered rack number one OR Autosampler rack Type 128 or Type 200 Slide the extended portion on the bottom of the rack into the long slit on the rack location mat 4 Figure 20 Rack location mat 1 Cut outs on the rack location mat 2 Holes for regular tube racks 3 Holes for the autosampler rack 90 SD 1 Purification Solution System Manual Installation 3 Rack Orientation 1 Place the rack in the correct orientation to get your samples in the desired order The following image shows an example of where the first sample is delivered to and the orientation of the regular racks provided with the fraction collector First sample dispensed in this position rack 1 tube 1 Rear of the fraction collector next to the 500000000006 pillar OOO0O0O00000000
85. stem Manual Installation 3 Information Communication established with COMn is visible on the screen 8 Click OK Configuration dialog closes 9 Doubleclick in Configurable Modules on 218 SD 1 Pump 218 SD 1 Pump Configuration dialog opens 10 Select the check box Pulse relay 1 of pump A on start 218 SD 1 Pump Configuration Instrument 1 sc COM Pest COMI x Number of pumps 2 Pressure unit bar Injection pump present F Pulse relay 1 of Kanaan Pump action on pressure error reas Nar Ii Node Serial mumber Farmuare Head version One ore more SD 1 pumps have been configured in the instrument A 1 PrepStar SD1 Please make sure to select the stop action in the pressure screen of all as the pumps 8 2 PrepStar D 1 a t 1 Press the PRESS button on the pump 2 Select stop below the ACTION parameter with the arrow keys of the pump D 1 CIM Control 7 Use SD 1 CIM for injection OM ID 1 Activate communication oK Cancel Help The CIM is able to send a start or stop pulse 11 Click OK Configuration dialog closes 12 Click OK You re back in Agilent OpenLAB Control Panel SD 1 Purification Solution System Manual 119 3 120 Installation in th PRO R R Edit Delete Refresh Lock Create Configure Edit Notifications Shortcuts Instrument Instruments and Locations Properties Actions Navigation Not Connected mm Instr i X PrepLC K Launch Offline Ey instruments X Administration Your startup lic
86. talling the Agilent 410 Autosampler Prep Option on page 82 for more information SD 1 Purification Solution System Manual 13 1 Introduction to the System Introduction to the Agilent 218 Solvent Delivery Module 14 For preparative scale HPLC systems the Agilent 218 Pump can be used to quickly and reliably deliver samples to the column instead of an injection valve or auto sampler All pumps are controlled by applicable instrument control software on a PC via OpenLAB CDS ChemStation Edition recommended The sample injection pump Agilent 218 Pump is plumbed into the system with a tee The column is plumbed after the tee When such an injection occurs the Thru Pump Injector Agilent SD 1 Pump automatically begins to ramp up to the correct flow rate At that instant delivers the sample and ramps back down to ensure consistent flow rate at all times during the analysis The Solvent Delivery Module s work with the Thru Pump Injector and lower their flow rate during the injection to maintain a constant overall solvent flow rate SD 1 Purification Solution System Manual Introduction to the System 1 Introduction to the Agilent 440 Fraction Collector The Agilent 440 Fraction Collector is a random access single probe fraction collector and can accommodate a variety of racks It is designed to automate the sample collection process This fraction collector is designed to meet the diverse requirements of high throughput laborat
87. tart the pump by pressing ENTER The pump will start to run and solvent will be drawn into the solvent inlet line After the inlet line is full let the pump continue to run for a few moments until the pressure display is steady Press STOP to stop the pump The SD 1 pump is now primed 7 Switch off the SD 1 by pressing the power switch SD 1 Purification Solution System Manual Installation 3 Flushing the HPLC System Before pumping solvent through an HPLC system it is important to flush all tubing to prevent impurities or particulates from the new tubing such as dust cutting oils metal swarf etc from clogging the column frit or contaminating the column WARNING Chemical Hazard gt Danger of burns To avoid injury to personnel or damage to equipment always follow appropriate safety guidelines when using chemicals and always wear appropriate safety equipment and clothing 1 Disconnect the tubing fitting at the column inlet and place the fitting into a waste container It is vital that the tubing is thoroughly flushed before flow is introduced to the column 2 To set the FLOW to 15 mL min on each Agilent SD 1 pump press 15 and confirm with ENTER 3 Press RUN to start each pump 4 Pump solvent through the tubing for several minutes The tubing is thoroughly flushed before flow is introduced to the column SD 1 Purification Solution System Manual 59 3 Installing the Detector 60 Location of the D
88. tion System Manual Installation Connecting the Water and Leakage Drain All solvents that result from a leak in the system and condensed water are drained through the left hand hose connector CAUTION Risk of damaging the autosampler Drain and waste tubing are twisted thereby obstructing the flow path gt Be sure that the drain and waste tubing are not twisted 3 1 Connect the hose connector to a waste container on the floor SD 1 Purification Solution System Manual 71 3 Installation Starting the Autosampler Tools required OR Preparations Description Distilled Water lsopropanol Helium Ultrasonic bath Allow the Agilent 410 Autosampler to reach ambient temperature for at least one hour Connect the waste tubings see Connecting the Waste Tubings on page 76 for more information Electrical shock Risk of stroke and other personal injury due to reduced safety protection or unwanted fusing gt Ensure that the code on the fuse cap matchs the information next to the fuse holders Risk of fire and damaging the module gt For 115 VAC 15 use two 5 A T fuses slow blow gt For 230 VAC 15 use two 2 5 A T fuses slow blow gt All fuses must be UL listed and CSA certified or IEC 127 type 78 Keep the keyboard front cover closed during operation Remove the safety screw on the right hand side of the front cover Check fuses and voltage settings on the rear of the instr
89. ual ee 5 a e Oe Cables 7 Cable Overview 124 Cable Connections 125 Analog Output 126 Relay Output 127 Desktop PC Communications 130 Synchronization Signals 131 This chapter provides information on cables used with the instrument Apg Agilent Technologies 123 5 Cables Cable Overview Necessary cables p n Description 392612901 OR 5023 0203 392607969 392607975 393546291 393597601 7910046300 Optional cables p n 110743800 110744200 124 Ethernet cable for use in a network Ethernet cable cross over for standalone use Inject marker cable Next injection cable Serial communication ribbon Converter RS 232 to RS 422 Serial cable Description Relay interface cable for relay interface board one relay contact per cable Analog signal cable SD 1 Purification Solution System Manual Cables 5 Cable Connections Cable Connections Back connectors for SD 1 to internal CIM pin connectors Serial communication ribbon NL Es Serial cable Converter RS 232 to RS 422 GPIB 1 SD 1 pump 410 Autosampler 3 325 Detector 440 Fraction Collector CPU Inject marker cable Figure 23 Cable connections for workstation control of Agilent SD 1 Solvent Delivery Modules Agilent 325 Detector Agilent 410 Autosampler and Agilent 440 Fraction Collector SD 1 Purification Solution
90. ument Connect the power cable FP O N Turn the power switch to ON The Ready screen appears displaying the firmware revision number SD 1 Purification Solution System Manual Installation 3 Rinsing the System with Wash Solvent Tools required OR CAUTION Description Distilled Water lsopropanol Helium Ultrasonic bath Damage to the system Crystals from salts or buffer solutions may block or damage the system gt Never use salts or buffer solutions as wash solvents gt Only use water organic solvents ao oo A Ww Place a clean bottle for the wash solvent at the left hand side of the autosampler Use a mixture of distilled water and isopropanol 80 20 v v or the mobile phase as wash solvent Degas the wash solvent with Helium or an ultrasonic bath Put the wash solvent tubing in the filled was solvent bottle Press MAINTENANCE to go the autosampler maintenance functions Fill the tubing using the autosampler soft function keys SYR END and SYR HOME With SYR END a syringe volume of wash solvent is aspirated from the wash solvent bottle and the wash solvent tubing is filled With SYR HOME the syringe contents will be dispensed to the syringe waste Repeat this action until the wash solvent tubing and the syringe are completely filled and no air bubbles appear in the syringe Press Escape to leave the maintenance screen SD 1 Purification Solution System Manual 79 3 Installation
91. witch that connects from the front of the detector directly to the power receptacle on the rear panel Plug one end of the power cord into the power receptacle on the rear panel and the other end into your AC power source SD 1 Purification Solution System Manual Installation 3 WARNING Absence of ground connection or use of unspecified power cord The absence of ground connection or the use of unspecified power cord can lead to electric shock or short circuit gt Never operate your instrumentation from a power outlet that has no ground connection gt Never use a power cord other than the Agilent Technologies power cord designed for your region All devices in the liquid chromatography system should be connected to the same power source using a properly grounded 8rd wire to earth multiple outlet power strip Do not turn on the AC power yet All required external devices and hydraulics must first be connected Avoiding Harmful Interferences to Radio or Television Reception 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 If this equipment does cause harmful interference to radio or television reception which can be determined by turning the equipment off and on the user is encouraged to try one or more of the following measures 1 Relocate the ra
92. without the pump head installed You will have to install the pump head before beginning to run You can also change pump heads at any time Description Wrench open ended 5 16 inch Wrench open ended inch Wrench 9 64 inch hexagonal T handle Wrench 5 32 inch hexagonal T handle Wrench 3 16 inch hexagonal T handle 1 To open the SETUP menu press the key 2 Press the DOWN ARROW key to access the setup functions HEADS DEVICE SET CLOCK CHANGE ID PUMP CIM MM DD YY HH MM SS y NOA NO 1 8 912 92 10 33 00 Figure 9 SETUP display 3 Place the cursor on HEADS CHANGE and press the DOWN ARROW key to scroll to YES 4 Press ENTER 5 Take the pump head set assembly and hold both heads in position with the piston cups inside the open piston collets Piston collet Piston cup 56 __ f NG an t Figure 10 Piston cup and piston collet 6 To begin the pump head engagement sequence press ENTER SD 1 Purification Solution System Manual Installation 3 The collets will close over the piston cups and when fully closed will draw the pump heads into place When both pump heads are in place the following message will appear Replace and tighten screws on both heads Plumb connections Press ENTER when completed 7 Tighten the mounting screws in each pump head with a 3 16 inch wrench 8 Tighten the mounting screws in the inlet tee with a 5 32 inch wrench 9 Tighten the mounting screws in the outlet
93. ystem Introduction to the Agilent 325 UV VIS Dual Wavelength Detector 10 The Agilent 325 UV VIS Dual WL Detector is integrated into a Liquid Chromatography System The detector is controlled remotely by OpenLAB through Ethernet communications In this situation all functions of the detector are controlled through the Workstation software The detector measures the sample absorbance at the user selected wavelength The absorbance is displayed Wavelength absorbance parameters are time programmable Features of the Agilent 325 UV VIS Dual WL Detector e Stackable module Interchangeable flowcells Simple lamp replacement e Comfortable control OpenLAB e Wide detection range peaks up to 40 AU cm with appropriate flowcell SD 1 Purification Solution System Manual Introduction to the System 1 Introduction to the Agilent 410 Autosampler The Autosampler is available in two configurations as the Standard Autosampler G9331A and the Preparative Autosampler G9332A Agilent 410 Autosampler G9331A The Agilent 410 Autosampler has been designed to meet the needs of the modern analytical laboratory The autosampler has the following features e Column temperature control and sample cooling guaranting consistent results e High resolution syringe control guaranting superior precision for injection and reagent addition Fast replacement of the injection valve Loop injection with Pressure Assisted Sample Aspiration is a proven

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