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1260 Infinity Multi-Detector Suite User Manual

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1. Table 1 Flow paths of MDS RI Detector with purge close open NO NORMALLY OPEN NC NORMALLY CLOSED Purge valve NO NORMALLY OPEN NC NORMALLY CLOSED Purge valve Sample cell Sample cell l 5 O O IN OUT PURGE Reference L Reference cell cell Purge close Purge open Grey lines flowing path Black lines immobilized mobile path The T connection results in both sides of the flow cell always being exposed to the same pressure The design of the cell allows the detector to be used in series with a maximum of one detector placed behind The maximum recommended flow rate that is permitted through the RI Detector is 5 mL min For more viscous solvents for example 2 propanol it is not recommended to work at the maximum flow rates Agilent MDS User Manual 19 1 20 Introduction to the 1260 Infinity MDS Before running solvent through the device make sure that the solvent within the detector is completely miscible with the intended solvent to be used In case of immiscible solvents the cell must be rinsed through with an intermediate solvent for example acetone which is miscible with both solvents The MDS RI detector is shipped in acetone Agilent MDS User Manual Introduction to the 1260 Infinity MDS 1 The 1260 Infinity MDS Viscometer The MDS Viscometer is a temperature controlled four capillary fused silica bridge viscometer t
2. This chapter gives an overview about the troubleshooting and diagnostic features Agilent MDS User Manual 3 In this book 8 Error Information This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions 9 Maintenance This chapter describes the maintenance of the 1260 Infinity Mulit Detector Suite 10 Parts and Materials for Maintenance This chapter provides information on parts for maintenance 11 Appendix 1 Theory of Operation This chapter provides an overview of the principles and theory of RI Viscometry and Light Scattering detection 12 Appendix 2 General Safety Information This chapter provides additional information on safety legal and web 4 Agilent MDS User Manual Contents Contents 1 Introduction to the 1260 Infinity MDS 9 Introduction 10 Instrument Overview 12 The 1260 Infinity MDS Refractive Index Detector 19 The 1260 Infinity MDS Viscometer 21 The 1260 Infinity MDS Dual Angle Light Scattering Detector 24 The 1260 Infinity MDS Dynamic Light Scattering Detector 25 2 Site Requirements and Specifications 27 Pre installation Requirements 28 Site Requirements 29 Physical Specifications 33 Performance Specifications 34 3 Installation 37 Unpacking the Module 38 Installing the Instrument 42 Fluid Connections 49 Other Connections 54 4 Controlling the 1260 Infinity MDS 59 Contro
3. Back This option returns the display back to the Main Menu screen Agilent MDS User Manual 85 4 Controlling the 1260 Infinity MDS The VS Parameters Menu Screen The VS Parameters Menu screen is used to access the Viscometer parameters To access the VS Parameters screen select the Parameters sub menu option from the VS Detector Menu screen The items available in the menu are as follows Purge Time This parameter defines the time delay between the DP and IP purge valves opening and closing during a DP or IP purge action selected from the VS Detector Menu screen The time range and default value are shown below Range 0 600s Default 60s Temperature This parameter sets the temperature of the Viscometer in increments of 1 C There is also the option to turn the heater off The temperature range and default value are shown below Range 30 60 C with an Off Option Default Off Back This option returns the display back to the VS Detector Menu screen 86 Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The LS Detector Menus The 1260 Infinity MDS LS detector menus are used to access the specific options component and parameters for the LS detector To access these menus select the LS Detector option from the Main Menu screen The LS Detector menu screens that are available are as follows The LS Detector Screen The LS Parameters Screen User required component and parameters are located in the
4. Clean the flow cell thoroughly Refer to Routine Maintenance of the MDS System on page 105 for further information Suggested actions Check purge valve is closed Check for liquid in front drain tube or drip gutter e Please contact your Agilent service representative 125 7 Troubleshooting and Diagnostics Unable to autozero detector Probable cause Suggested actions 1 Sample and reference cells do not contain Purge the RI detector thoroughly identical solutions 2 Reference cell contains air bubbles Purge the RI detector thoroughly 3 Contaminated flow cell Clean the flow cell thoroughly Refer to Routine Maintenance of the MDS System on page 105 for further information 4 Faulty light source Please contact your Agilent service representative 126 Agilent MDS User Manual Troubleshooting and Diagnostics 7 Viscometer Detector Problems DP IP excessive baseline noise Probable cause Suggested actions 1 Bubble in DP IP transducer Purge the DP IP transducers thoroughly to remove air bubble e Use only degassed mobile phase Repeatedly purge with 3 s purge time 2 Incorrect compressibility setting for mobile Use correct pump compressibility setting for phase mobile phase solvent 3 Pump flow rate fluctuating Check pump performance e Insufficient pressure on pump e Use pulse damper DP IP excessive baseline drift Probable cause Suggested actions 1 Detector not fully equilibrated with
5. Fluid Connections RI AND Viscometer Detectors 1 Establish the fluid connections as shown below From column 600 800 mm RI to Visco To waste To PURGE waste 200 mm 800 mm 800 mm 51 Agilent MDS User Manual 3 52 Installation Fluid Connections Fluid Connections LS AND Viscometer Detectors 1 Establish the fluid connections as shown below To waste 800 mm LS to Visco 200 mm From column 600 800 mm Agilent MDS User Manual Installation 3 Fluid Connections Triple Detector System Parts required p n G7800 87000 G7800 87001 PLO100 3601 PLO100 3602 Description PTFE Tubing 0 25 mm ID x 1 6 mm OD 2 m Connection from column to detector and between detectors PTFE Tubing 1 0 mm ID x 1 6 mm OD 2 m Connection from detector to waste and or purge waste Valco Nut 1 16 inch 5 EA Valco Ferrule 1 16 inch 5 EA Fluid Connections LS RI and Viscometer Detectors 1 Establish the fluid connections as shown below Agilent MDS User Manual From column 600 800 mm LS to RI 200 mm To PURGE waste 800 mm RI to Visco 300 mm To waste 800 mm 53 3 Installation Other Connections Other Connections All power signal and communication connections are made on the rear panel of the MDS Control Unit see Figure 7 on page 54 1 10 2 3 4 5 6 7 8 9 Figure 7 Rear View of the MDS Control Unit Analog outputs Analo
6. delay hold up columns 113 detector output channel assignment 47 detector status icons 67 dimensions 33 diode laser 172 drift 105 dynamic light scattering 171 188 E electric dipole moment 173 electronic waste 185 errors detector 133 system 133 F form factor 1 7 Fourier transform 179 frequency range 33 high angle light scattering 178 home screen 65 HPLC system 104 humidity 33 inspecting cables 155 installation bench space 31 installing 45 interfaces auxiliary I O port 56 RS232 56 USB 55 internet 187 intrinsic viscosity 165 K keypad locking 62 unlocking 62 L laser safety 29 laser wavelength 35 lightbeam 160 light intensities 161 light electric fields 172 magnetic fields 172 limiting concentration 167 line frequency 33 line voltage 33 location 104 Lord Rayleigh 171 low angle light scattering 178 LS detector menus 87 M main menu screen 70 Mark Houwink Sakurada 164 measuring concentration 162 menu system 69 monochromatic source of light 172 noise 105 non operating altitude 33 non operating temperature 33 Agilent MDS User Manual 0 online viscosity measurements 163 operating Altitude 33 operating temperature 33 optimizing viscometer performance 112 P packaging damaged 38 parts 158 peak broadening minimizing 104 performance degradation 105 performance specifications DLS detector 35 dual angle LS detectors 35 refractive index detector 34 viscometer
7. 1260 Infinity MDS USB Cable PTFE Tubing 0 25 mm ID x 1 6 mm OD 2 m PTFE Tubing 1 0 mm ID x 1 6 mm OD 2 m Agilent 1200 to 1260 MDS Analogue cable Agilent 1260 Infinity MDS Auxiliary 1 0 cable Agilent 1260 Infinity MDS LS DLS Installation Kit Corrugated tubing PP 6 5 mm id 5 m Union stand LD flow no fitting RS232 Serial Cable MDS to 1200 Series Auxiliary Cable Valco Nut 1 16 inch 5 EA Valco Ferrule 1 16 inch 5 EA Agilent MDS User Manual Agilent MDS User Manual 11 Appendix 1 Theory of Operation The 1260 Infinity MDS Refractive Index Detector 160 Measurement Principle and Light Path 160 Using Refractive Index Measurements to Measure Concentration 162 The 1260 Infinity MDS Viscometer 163 Theory of Online Viscosity Measurements 163 Universal Calibration 165 Polymer Branching 166 Four Capillary Viscometry Theory 166 Viscometer Troubleshooting Charts 168 The 1260 Infinity MDS Light Scattering Detector 171 Overview 171 The Physical Basis Of Light Scattering 172 Static Light Scattering 173 Measuring Rh Using Dynamic Light Scattering 179 This chapter provides an overview of the principles and theory of RI Viscometry and Light Scattering detection Brae Agilent Technologies 159 11 Appendix 1 Theory of Operation The 1260 Infinity MDS Refractive Index Detector 160 The MDS differential refractive index detector is a high performance device specifically designed for GPC The RI detector features high signal
8. 3 Obstruction in fan 4 Defective main board in control unit Agilent MDS User Manual Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative 137 8 Error Information Fan Failed in Lower Enclosure Error ID SYSTEM 1120 Thermal shut down of the cooling fan at rear of lower enclosure Probable cause Suggested actions 1 Fan cable disconnected Please contact your Agilent service representative 2 Defective fan Please contact your Agilent service representative 3 Obstruction in fan Please contact your Agilent service representative 4 Defective main board in control unit Please contact your Agilent service representative Fan Failed on Control Unit Power Supply Error ID SYSTEM 1130 Thermal shut down of the cooling fan located next to power supply in control unit Probable cause Suggested actions 1 Fan cable disconnected Please contact your Agilent service representative 2 Defective fan Please contact your Agilent service representative 3 Defective main board in control unit Please contact your Agilent service representative 138 Agilent MDS User Manual Error Information 8 Communication to RI Detector Failed Error ID SYSTEM 1230 Communication between RI detector and Control unit has failed Probable cause Suggested action
9. Infinity MDS The Instrument Display The Start up Screen The Start up screen is displayed when the MDS is powered on The screen displays the product name and copyright and that the instrument is initializing checking onboard components and probing the detector bays for the MDS detector s connected Once the instrument has been initialized the Home screen is displayed The keypad is not functional during the Start up screen 64 Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The Home Screen The Home screen is first displayed on the completion of the instrument initialization during which the Start up screen was displayed The Home screen is dynamic and only shows information for the MDS detectors that are present in the detector enclosures This screen can be regarded as a summary page which displays the following e The status of the system The type of detector connected The status of each detector connected The current outputs of each detector connected Any errors that occur The Home screen consists of four Detector Areas even if the instrument is a single or dual detector system and a System Status Area lt Detector 1 Area gt lt Detector 2 Area gt lt Detector 3 Area gt lt Detector 4 Area gt lt System Status Area gt Figure 10 Layout of the MDS Home Screen Each Detector Area on the screen displays specific information for a detector and corresponds to the actual physical location of
10. LS Detector and LS Parameters screens The complete structure of the MDS LS Detector Menu screens is as follows _Main Menu _ LS Detector gt LS Detector _ Parameters gt LS Parameters Figure 19 The MDS LS Detector Menus Agilent MDS User Manual 87 4 Controlling the 1260 Infinity MDS The LS and LS DLS Detector Menu Screen The LS Detector Menu screen is used to access the Laser component for the LS detector and the detector parameters option To access the LS Detector screen select the LS Detector option from the Main Menu screen The items available in the menu are as follows Laser This component is used to manually turn the LS Laser on and off The information text displayed is dynamic and is dependent on the state of the Laser If the Laser is off default position On Selecting This will turn the Laser on with the text LS Laser On displayed in the System Status Area The Laser status icon will be displayed as static in the LS Detector Area of the Home screen If the Laser is on On Selecting This will turn the Laser off with the text LS Laser Off displayed in the System Status Area The Laser status icon will be displayed as flashing with a cross in the LS Detector Area of the Home screen Parameters This sub menu option displays the LS Parameters Menu screen Back This option returns the display back to the Main Menu screen 88 Agilent MDS User Manual Controlling the 1260
11. MDS Controlling the Instrument 60 The Keypad 61 The Instrument Display 64 The Start up Screen 64 The Home Screen 65 The Menu System 69 The RI Detector Menus 76 The RI Detector Menu Screen 77 The RI Parameters Menu Screen 79 The Viscometer Menus 82 The VS Detector Menu Screen 84 The VS Parameters Menu Screen 86 The LS Detector Menus 87 The LS and LS DLS Detector Menu Screen 88 The LS Parameters Menu Screen 89 The Analog Input Menus 90 The Analog Input Menu Screen 91 The Analog Input Parameters Menu Screen 92 The System Options Menus 93 The System Options Menu Screen 94 The System Options Parameters Menu Screen 95 This chapter describes how to control the instrument Be Agilent Technologies 59 4 Controlling the 1260 Infinity MDS Controlling the Instrument The MDS can be controlled via PC or using the built in keypad and display on the MDS Control Unit The control unit provides the following Monitoring detector temperature and signal outputs Setting parameters on each detector for example temperature or purge time Performing actions on a detector for example autozero or purge Access to service parameters for each detector Monitoring the status of the system for example a detector heating the LS laser off or any errors Access to system information for example firmware version of a detector Figure 8 MDS Control Unit Agilent MDS User Manual The Keypad Controlling the 1260 Infinity MDS 4
12. P 3 q lt Rg gt Figure 35 Values of p as a function of q lt R gt for various particle shapes 1 Sphere 2 Gaussian Coils 3 Rods It is clear that all three molecular shapes yield the same value of P O when q lt R gt is less than approximately 1 As the value of P O increases the shape of the molecule clearly influences the light scattering intensity The Form Factor The form factor at a particular angle is the ratio of the signal at that angle when compared to the signal expected at the theoretical angle of 0 where there is no form factor as indicated by equation 6 The importance of the form factor is that small molecules e g those which have a radius that is lt 10 nm which is small when compared to the wavelength of the incident light are studied generate comparable signals at all angles while large molecules generate signals that are smaller at higher angles and larger at small angles Agilent MDS User Manual 177 11 Appendix 1 Theory of Operation 178 Characteristics of Low Angle 15 Light Scattering Low angle light scattering data is collected at a 15 angle to the incident beam and is typically used for determination of the molecular weights of large molecules This measurement angle is especially useful for the study of proteins with molecular weight of greater than 1 10 Da and for random coils with molecular weight between 2 10 Da and about 1 10 Da In addit
13. any specified solvent solute pair under constant operating conditions 162 Agilent MDS User Manual Appendix 1 Theory of Operation 11 The 1260 Infinity MDS Viscometer Theory of Online Viscosity Measurements When a polymer dissolves in a liquid the interaction of the two components stimulates an increase in polymer dimensions over that of the unsolved state Due to the vast difference in size between solvent and solute the frictional properties of the solvent in the mixture are drastically altered and an increase in viscosity occurs which should reflect the size and shape of the dissolved solute even in dilute solutions The dissolved polymer coil disturbs the linear Oe flow of solvent resulting in a change in viscosity ane This was first recognized in 1930 by Staudinger who found an empirical relation between the relative magnitude of increase in viscosity and the molar mass of the polymer The Intrinsic viscosity yn is a measure of the viscosity of a polymer solution as the concentration tends to zero i e at very low concentrations It is this parameter therefore that is a characteristic of isolated polymer chains in solution and can be considered to be proportional to the density of the polymer coil Agilent MDS User Manual 163 11 Appendix 1 Theory of Operation For a given polymer and solvent system at a specified temperature n can be related to molecular weight M through the Mark Houwink Sakurada e
14. as specifies he manual 1 IP 2DP 3 Visc ml min 2 hours Figure 31 Viscometer Troubleshooting Chart 1 168 Agilent MDS User Manual Appendix 1 Theory of Operation 11 The 1260 Infinity MDS Viscometer Open DP purge n Zero DP while in Close DP purge OP 100210 OC test using Dow 1683 If IP is also gt 60KPa when the DP purge valve is closed then P suspect a partial blockage on Replace bridge the front of the bridge if IP is also lt 30KPa when the DP purge valve is closed then suspect 1 pump problem 2 bridge 1 Check pump flow leak at the front of the 3 Leaking IP purge valve 4 IP transducer problem 2 Check for leak at bridge 3 Check for leak at purge val 4 Replace IP transducer Figure 32 Viscometer Troubleshooting Chart 2 Agilent MDS User Manual 169 11 Appendix 1 Theory of Operation The 1260 Infinity MDS Viscometer Figure 33 Viscometer Troubleshooting Chart 3 170 Agilent MDS User Manual Appendix 1 Theory of Operation 11 The 1260 Infinity MDS Light Scattering Detector Overview Light Scattering refers to the process in which light from an incident polarized laser beam is scattered in all directions when it interacts with a molecule or particle Light scattering is an everyday occurrence and was first described by Lord Rayleigh in the late 1800 s An example of light scattering is the scattering of sunlight by particles in the atmosphere the sky is blue because short
15. factor equation 6 A more detailed discussion of the form factor is presented in The Form Factor on page 177 sub section _ Scattering int ensity at angle P O ae scattering intensity at angle It should be noted that P O can be written as a series as shown in equation 7 P 1 4 q RD h i De g 47 n sin 2 A R is the radius of gyration of the molecule g n is the index of refraction of the liquid A is the wavelength of light in a vacuum 0 Agilent MDS User Manual 175 11 Appendix 1 Theory of Operation For scattering at 15 and 90 equation 7 can be expressed as equations 8 and 9 respectively ple 1 263 25 aj 0 R n P 1 0 0897 j 0 Table 13 on page 176 shows values of P forl5 and 90 degrees as a function of molecular weight These values assume that the molecules are random coils Table 13 Values of P as a function of molecular weight My R approx nm P 90 P 15 5 108 2 3 0 9993 1 0000 5 104 7 0 9993 0 9928 5 105 23 0 9993 0 9976 5 108 70 2 0 9880 5 107 230 2 0 7622 1 Value of P 90 and P 15 for Aj 685 nm n 1 5 2 values depend on shape 176 Agilent MDS User Manual Appendix 1 Theory of Operation 11 If the value of P O found in equation 7 is below 0 7 higher order components become important In this case P O depends on Rg and also on the shape of the molecule as shown in Figure 35 on page 177 1 2
16. in the following section Agilent MDS User Manual 49 3 Installation Fluid Connections Single Detector System Parts required p n Description G7800 87000 PTFE Tubing 0 25 mm ID x 1 6 mm OD 2 m Connection from column to detector G7800 87001 PTFE Tubing 1 0 mm ID x 1 6 mm OD 2 m Connection from detector to waste and or purge waste PL0100 3601 Valco Nut 1 16 inch 5 EA PLO100 3602 Valco Ferrule 1 16 inch 5 EA IN4 34055 5PSI Back Pressure Regulator BPR Connection from RI detector to waste Fluid connections LS Detector or Viscometer only 1 Establish the fluid connections as shown below From column 600 800 mm To waste 800 mm Fluid Connections RI Detector only 1 Establish the fluid connections as shown below To waste 800 mm with 5 Psi BPR To PURGE waste 800 mm From column 600 800 mm 50 Agilent MDS User Manual Installation 3 Fluid Connections Dual Detector System Parts required p n Description G7800 87000 PTFE Tubing 0 25 mm ID x 1 6 mm OD 2 m Connection from column to detector and between detectors G7800 87001 PTFE Tubing 1 0 mm ID x 1 6 mm OD 2 m Connection from detector to waste and or purge waste PL0100 3601 Valco Nut 1 16 inch 5 EA PL0100 3602 Valco Ferrule 1 16 inch 5 EA Fluid Connections LS AND RI Detectors 1 Establish the fluid connections as shown below To waste 800 mm From column LS to RI 600 800 mm 200 mm To PURGE waste 800 mm
17. moves toward the detector the frequency increases and as it moves away the frequency decreases The amount of the increase decrease of the change in the frequency is related to the diffusion rate of the scattering molecule in the solvent While the diffusion coefficient could be obtained from the frequency spectrum it is easier to measure the small intensity fluctuations and then compute the autocorrelation function The autocorrelation function is related to the frequency spectrum by the Fourier transform i e the data processing is performed in the time domain rather than the frequency domain From an experimental perspective the intensity of the scattered light is detected by counting the photons scattered via an avalanche photodiode an electronic device that emits a pulse every time a photon passes through its detector This high sensitivity detector sees a time varying signal rather than a relatively constant in batch mode or slowly varying total intensity signal It should be noted that even when measurements are taken in flow mode the sample can be considered as slowly varying This is due to the time frame of the scattered light measurement relative to the rate of elution of the light scattering molecules from the column The photon counting measurement is performed over a very short period of time to record the very rapid diffusion that is taking place Small particles or biomolecules diffuse quickly with the scattere
18. non aqueous solvent is in use flush the cells with a solvent that is e miscible with your mobile phase e a good solvent for the predicted contaminant A typical RI chromatogram is shown below Figure 22 Typical RI chromatogram Agilent MDS User Manual 111 Optimizing Performance Optimizing Viscometer Performance 112 The Agilent 1260 MDS Viscometer employs the fluid flow equivalent of the analogous Wheatstone bridge electrical circuit see The 1260 Infinity MDS Viscometer on page 163 for detailed theory of operation When mobile phase is pumped into the viscometer solvent travels down a bridge of four capillaries of equal resistance However when the sample is introduced an imbalance is created This change in pressure AP is proportional to the specific viscosity and the instrument makes a true differential measurement directly making it very sensitive to changes in viscosity Consequently the performance of the viscometer is highly dependent on the pump performance The solvent delivery module must be thoroughly purged and able to deliver solvent at the desired flow rate without pulsation Viscometer performance is also dependent on how thoroughly the detector has been purged Any air bubbles or residual traces of previous solvent in the system will result in poor results It is therefore important to follow the purging procedures that are described in this manual and allow enough time for the detector to equili
19. page 31 for more information Add a second damper Add a restrictor coil backpressure regulator between pump and injector valve Use correct pump compressibility setting for mobile phase solvent Repair or replace defective recorder or cable Investigate external detector Agilent MDS User Manual Excessive baseline drift Probable cause 1 Environmental temperature fluctuations 2 Formation of gases in the mobile phase reservoir 3 System not fully equilibrated Long retention times Probable cause 1 Pump flow rate fluctuating 2 Solvent leak within the system 3 System not fully equilibrated Agilent MDS User Manual Troubleshooting and Diagnostics 7 Suggested actions Move instrument to a more stable environment see Location of the Instrument on page 31 for more information Use only premixed degassed mobile phase Use an in line degasser Allow sufficient time for the system to equilibrate with the mobile phase and environment Suggested actions Check pump performance Check system for solvent leaks Allow sufficient time for the system to equilibrate with the mobile phase and environment 123 7 Troubleshooting and Diagnostics RI Detector Problems 124 Excessive baseline noise Probable cause 1 Air bubble in pump 2 Air bubble in detector tubing 3 Contaminated flow cell 4 Environmental temperature fluctuations 5 Faulty light source Excessive baseline drift
20. representative Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative Agilent MDS User Manual Error Information 8 DP Purge Valve Error Error ID VS 4320 Purge valve failed to operate Probable cause Suggested actions 1 Purge valve is defective Please contact your Agilent service representative 2 Purge valve assembly not connected to Please contact your Agilent service viscometer main board representative 3 Defective main board in viscometer Please contact your Agilent service representative Agilent MDS User Manual 145 8 Error Information LS and DLS Detector Specific Error Messages Temperature Sensor Error Error ID LS 6110 Temperature sensor reading outside normal limits Probable cause Suggested actions 1 Defective temperature sensor Please contact your Agilent service representative 2 Defective LS Detector main board Please contact your Agilent service representative Unable to reach temperature set point Error ID LS 6120 Heater has timed out and unable to reach set temperature Probable cause Suggested actions 1 Defective heater Please contact your Agilent service representative 2 Defective LS Detector main board Please contact your Agilent service representative 146 Agilent MDS User Manual Error Information 8 Heater Error Error ID LS 6130 Heater has fa
21. see The RI Detector Menus on page 76 and following chapters Agilent MDS User Manual 75 4 Controlling the 1260 Infinity MDS The RI Detector Menus The 1260 Infinity MDS RI detector menus are used to access the specific options actions components and parameters for the RI detector To access these menus select the RI Detector option from the Main Menu screen The RI Detector menu screens that are available are as follows The RI Detector Screen The RI Parameters Screen The RI Service Screen The RI Service Settings Screen User required actions and parameters are located in the RI Detector and RI Parameters screens Components and parameters for service and checking the RI detector are located in the RI Service and RI Service Settings screens The complete structure of the MDS RI Detector Menu screens is as follows RI Detector gt Autozero Purge Time Temperature Polarity Signal Time LED Gain Signal Gain Zero Offset Sum Value LFSC Value Max LED Value Back Purge Valve Autozero Motor Settings Parameters gt Service gt Back gt gt RI Service Settings LFSC Value Max LED Value Figure 17 The MDS RI Detector Menus 76 Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The RI Detector Menu Screen The RI Detector Menu screen is used to access the autozero and purge actions for the RI detector the detector parameters and service opt
22. sensor located in upper enclosure bay has failed Probable cause Suggested actions 1 Leak sensor not connected to the main Please contact your Agilent service board in the control unit representative 2 Defective vapor sensor Please contact your Agilent service representative Upper Leak Sensor Failed Error ID SYSTEM 1020 The lower thermistor on the leak sensor located in upper enclosure bay has failed Probable cause Suggested actions 1 Leak sensor not connected to the main Please contact your Agilent service board in the control unit representative 2 Defective vapor sensor Please contact your Agilent service representative 134 Agilent MDS User Manual Error Information 8 Lower Leak Sensor Failed Error ID SYSTEM 1030 The upper thermistor on the leak sensor located in lower enclosure bay has failed Probable cause Suggested actions 1 Leak sensor not connected to the main Please contact your Agilent service board in the control unit representative 2 Defective vapor sensor Please contact your Agilent service representative Lower Leak Sensor Failed Error ID SYSTEM 1040 The lower thermistor on the leak sensor located in lower enclosure bay has failed Probable cause Suggested actions 1 Leak sensor not connected to the main Please contact your Agilent service board in the control unit representative 2 Defective vapor sensor Please contact your Agilent service representative Agilent MDS Use
23. the detectors in the MDS Detector Enclosures For example if the MDS RI detector is located in the left hand detector bay of the top detector enclosure then the RI detector outputs and status appears in the top left Detector Area of the Home screen If a detector bay has no detector present then the Detector Area on the Home screen will be left blank Agilent MDS User Manual 65 4 66 Controlling the 1260 Infinity MDS This mapping of detectors is done during the initialization of the instrument where each detector bay is probed to determine if any MDS detectors are present See Powering the Instrument On or Off on page 46 for further information on the instrument initialization Example Configuration Actual detector configuration Home Screen displayed Figure 11 MODS with RI LS and Viscometer VS Detectors The information displayed in the Detector Area is specific to the MDS detector connected but in general the following information is displayed The detector type that is RI LS and VS Viscometer The detector signal output s e The current temperature of the detector The detector status icons For the LS Detector Area the L and H refer to the Low and High angles of the dual angle MDS LS detector the 90 is the High angle and the 15 is the Low angle For the VS Detector Area the DP and IP refer to the Differential and Inlet Pressures of the MDS Viscometer Agilent MDS User Manual Controlling t
24. the last set of parameters used e The detector output s are assigned according to the location of the detector s installed The Home screen and the menu system are setup The MDS Control Unit automatically probes the detector bays to discover which detectors are present The detector bays are probed in the following order Bay3 Bay4 Oo Agilent MDS User Manual 47 3 48 Installation As the system finds each detector it assigns the detector s data outputs onto the output channels digital and analog so the lowest numbered channel will be the output from the first detector For the viscometer and light scattering detector the channels are ordered as follows Table 7 Detector channel assignment Detector Channel 1 Channel 2 Viscometer Differential Pressure DP Inlet Pressure IP Light Scattering Detector 15 low Angle 90 high Angle The two analog inputs are always added as the last two channels of the system An example is shown in Table 8 on page 48 where RI Viscometer and Light scattering detectors are installed Table 8 Analog input channel assignment Detector Position Detector Detector Output Assigned Output Channel Top Left RI RI 1 Top Right LS Low Angle 15 2 High Angle 90 3 Bottom Left Viscometer Differential Pressure DP 4 Inlet Pressure IP 5 Analog Inputs Chi Analog input channel 1 6 Ch2 Analog input channel 1 7 Spare 8 Only digital output chann
25. the pressure drop through the bridge P When the sample is introduced across capillary 4 C4 of the bridge an imbalance is caused due to the holdup columns This change in pressure AP is proportional to the specific viscosity Nsp according to the following equation _ 4AP P 2AP Where AP is the differential pressure across the bridge and P is the pressure of the flow through the capillary bridge The instrument makes a true differential measurement directly making it very sensitive to dilute solution viscosity measurements Nes The intrinsic viscosity yn is ideally obtained by measuring the specific viscosity values at several finite concentrations and extrapolate to zero concentration 7 lim 0 c However the concentrations used in GPC are low enough for the equation to be valid over a typical chromatogram and thus an extrapolation to the true intrinsic viscosity is not required since the concentration is close enough to the limiting concentration All of the data acquisition and data processing are accomplished using Agilent GPC SEC software which enables calculation of molecular weight and intrinsic viscosity distributions using algorithms for Universal Calibration Branching information can also be obtained from Agilent GPC SEC software Agilent MDS User Manual 167 11 Appendix 1 Theory of Operation The 1260 Infinity MDS Viscometer Viscometer Troubleshooting Charts Use flushing purging system
26. to the 1260 Infinity MDS 1 The 1260 Infinity MDS Dynamic Light Scattering Detector The MDS DLS detector is a 90 Light Scattering Detector with a further Dynamic Light Scattering detector on the same sample cell This allows all the same functionality as the Dual Angle Light Scattering Detector but with hydrodynamic size measurements without increasing dead volume Before pumping solvent through any of the detector modules make sure that the solvent within the detector is completely miscible with the intended solvent to be used In case of immiscible solvents the detector must be purged through with an intermediate solvent for example acetone which is miscible with both solvents The MDS LS detector and Bio SEC DLS detector are shipped in 2 propanol IPA Agilent MDS User Manual 25 1 26 Introduction to the 1260 Infinity MDS The 1260 Infinity MDS Dynamic Light Scattering Detector Agilent MDS User Manual Agilent MDS User Manual 2 Site Requirements and Specifications Pre installation Requirements 28 Site Requirements 29 Physical Specifications 33 Performance Specifications 34 This chapter provides information on environmental requirements physical and performance specifications ott Agilent Technologies 27 2 Site Requirements and Specifications Pre installation Requirements The MDS operation manual describes the environmental and operating requirements of the instrument You must prepare your labora
27. 00 Infinity LC Control of the MDS is not integrated into OpenLAB chromatography software or the Instant Pilot so use of the keypad or the Agilent GPC SEC software is required To perform GPC calculations on the collected data the Agilent GPC SEC Software is required especially in case of multi detector calculations For this reason it is highly recommended to always use Agilent GPC SEC Software for control and collection Agilent MDS User Manual Installation 3 Dual Stack Configuration Ensure optimum performance by installing the modules of the Agilent 1200 Infinity LC System in the following configuration see Figure 6 on page 43 This configuration optimizes the flow path for minimum delay volume and minimizes the bench space required It is recommended to place the Agilent 1260 Infinity MDS on the left hand side of the LC system for easier access to the detector modules Solvent cabinet Vacuum degasser rP ee a i Autosampler L ae Column compartment Detector Figure 6 Recommended Configuration Agilent MDS User Manual 43 3 Installation Connection to a 3rd Party LC System The MDS system can be connected to any LC system fully integrated or modular that is capable of providing an isocratic flow of eluent The MDS can be used with such systems by connecting the column or UV detector outlet to the MDS and the MDS waste line either back to the LC was
28. Agilent 1260 Infinity Multi Detector Suite User Manual tt Agilent Technologies Notices Agilent Technologies Inc 2014 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 67800 90390 Edition 01 2014 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 here
29. Allow sufficient time for the viscometer to environment equilibrate with the mobile phase and environment 2 Environmental temperature fluctuations Move instrument to a more stable environment see Location of the Instrument on page 31 for more information 3 DP IP transducers not fully flushed with Purge the DP IP transducers thoroughly mobile phase Agilent MDS User Manual 127 7 Troubleshooting and Diagnostics Low sensitivity Probable cause 1 DP IP transducers not fully flushed with mobile phase Excessive DP Offset Probable cause 1 DP transducer leaking 2 Partial blockage of the bridge 3 Distorted pressure transducer membrane 4 Hold up column defective High IP Output Probable cause 1 Partial blockage on front of the bridge Low IP Output Probable cause 1 Incorrect flow rate 2 Leak before viscometer bridge 128 Suggested actions Purge the DP IP transducers thoroughly Suggested actions Check system for solvent leaks Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative Suggested actions Please contact your Agilent service representative Suggested actions Check pump performance Check system for solvent leaks Agilent MDS User Manual Troubleshooting and Diagnostics 7 Light Scattering Detector Problems Excessive baseline noise Probable cause Suggested actio
30. Detector LS Detector VS Detector Analog Input System Options Back To select the required menu option use the up and down arrow keys on the keypad to highlight the menu and then press either the Select or Enter keys Selecting the Back option returns the display to the Home screen The Options Information Area displays information about the highlighted menu option The System Status Area within the Main Menu screen only displays the system status states either Ready or Not Ready See Table 10 on page 67 for details Agilent MDS User Manual 71 4 Controlling the 1260 Infinity MDS The Detector and System Menu screens The Detector and System Menu screens are used to access the options e g parameters and detector actions available for the detector s connected and the actual instrument These are all the menu screens accessed from the Main Menu screen The content of the individual screen will depend on the option selected however the screens will follow a similar format and consist of the following Items List Information Area e Detector Status Area e System Status Area lt ltems Menu gt lt Information Area gt lt Detector Status Area gt lt System Status Area gt Figure 15 Layout of the MDS Detector and System Menu Screens PURGE Press SELECT or the PARAMETERS ENTER key to autozero SERVICE the RI BACK PURGE TIME TEMPERATURE POLARITY 10 SIGNAL TIME LED GA
31. Detector 160 The 1260 Infinity MDS Viscometer 163 The 1260 Infinity MDS Light Scattering Detector 171 12 Appendix 2 General Safety Information 181 General Safety Information 182 The Waste Electrical and Electronic Equipment Directive 185 Radio Interference 186 Agilent Technologies on Internet 187 Agilent MDS User Manual Contents 8 Agilent MDS User Manual Agilent MDS User Manual 1 Introduction to the 1260 Infinity MDS Introduction 10 Instrument Overview 12 The 1260 Infinity MDS Refractive Index Detector 19 The 1260 Infinity MDS Viscometer 21 The 1260 Infinity MDS Dual Angle Light Scattering Detector 24 The 1260 Infinity MDS Dynamic Light Scattering Detector 25 This chapter gives an instrument overview and an introduction to the function of the MDS detectors Apg Agilent Technologies 1 Introduction to the 1260 Infinity MDS Introduction 10 The Agilent 1260 Infinity Multi Detector Suite MDS is a high end multiple detector platform which provides not only accurate molecular weight data independent of the chemistry of the standards but also gives insight into the behavior of the polymer in solution The system is available as two configurations 1 Agilent 1260 Infinity GPC SEC MDS G7800A A system optimized for organic use with options of refractive index detector dual angle light scattering detector and viscometer Agilent 1260 Infinity Bio SEC MDS G7805A A system optimized for aqueou
32. F The solution is prepared at 1 0 mg mL and 100 uL injected into a 1 mL min flow stream of THF on a PLgel MIXED C column Typical QC Results for HT LS 15 90 Aa oe ee Response mtv L ji f c lt 140mV gt SmV LS15 1 lt 70mv r B ECE ECN ae age iE BER oa E E 8G ek Nee a En E a eh Oe Bs 9 o 0 oS 8 2 28 3 38 4 48 amp SS 6 68 7 78 8 10 10S 19 NS 12 128 t3 135 14 taS 15 155 6 Retention Time Figure 25 Example QC data from a Light scattering detector It should be remembered that the light scattering offset is a direct measurement of the solvent or eluent scattering and if the solvent is dirty and contains particulates the scattering will be higher The table below compiled from empirical data should be used as a general guideline for the expected offsets of a few commonly used eluents The best performance and the lowest solvent scattering are generally obtained when the eluent has been filtered to 0 02 um best or lt 0 2 um acceptable Agilent MDS User Manual Optimizing Performance 6 Table of typical solvent scattering values under conditions specified in the comment column Table 12 LS baseline offsets in common solvents Eluent LS 15 Baseline LS 90 Baseline Comments Tetrahydrofuran THF lt 140 mV lt 70 mV 1 mL min flow HPLC Water 0 02 Sodium Azide lt 200 mV lt 200 mV As a visual indication of good and bad baselines see the graph below
33. Figu Home Agilent MDS User Manual re9 Select Enter E i The MDS Keypad Displays the Home screen Abandons any non committed changes From the Home screen Selects the Main Menu screen From menu screens Selects the highlighted menu item Actions the highlighted menu action Commits the new parameter value typed in From the Home screen Selects the Main Menu screen From other menu screens Selects the highlighted menu item Actions the highlighted menu action Commits the new parameter value typed in Cancels a not committed parameter entry the original value is redisplayed Stops the purge detector action Goes back one menu screen Changes the sign of the parameter value being entered 61 4 Controlling the 1260 Infinity MDS CAUTION During Menu navigation Moves the cursor up or down a menu list While Editing a Parameter Increments decrements numerical parameters by step value Cycles through parameter states e g Normal Invert The Right arrow acts as Select The Left arrow acts as Cancel e Pressing both keys simultaneously locks unlocks the keypad Locking and Unlocking the Keypad The MDS Keypad automatically locks when The MDS Control Unit receives a sample injection trigger via the Auxiliary I O port or from a Start Collection command from the Agilent GPC SEC software if used The injection icon is displayed The software is used t
34. For further details on locking and unlocking the keypad see Locking and Unlocking the Keypad on page 62 The data collection injection status indicates that an injection has been made and data collection is in progress This is indicated with the Injection icon N being displayed and will occur when e The Control Unit receives a sample injection trigger via the Auxiliary I O port or from a Start Collection command from the Agilent GPC SEC software if used This will also automatically lock the keypad with the Lock icon displayed in the System Status Area If Agilent GPC SEC software is used for data collection then on completion of the sample injection run or on an Abort Run command sent then the Injection icon will be removed from the System Status Area Otherwise manually unlocking the keypad will remove the Injection icon The System Status Area will also display any error that occurs with error code and error message From the Home screen pressing either the Select or Enter keys on the keypad accesses the MDS Menu System The Home screen can be displayed at anytime by pressing the Home key on the keypad Agilent MDS User Manual Controlling the 1260 Infinity MDS The Menu System 4 The Instrument Display The MDS Menu System is accessed from the Home screen of the display by pressing either the Select or Enter keys on the keypad The Menu System comprises of a series of screens which allows access to system and de
35. I O cable The auxiliary I O cable provides the following A Stop Pump Request allowing a pump to be stopped if any error occurs on the MDS Receive a sample injection trigger for synchronized data acquisition Table9 MDS 1 0 Connections 1 0 Description Pin Number Wire ID Inputs Sample Injection Trigger Input 5 amp Ground 7 amp GND Spare TTL Input 6 8 Outputs Pump Stop Contact Closure Normally Open 3 amp 10 1 amp 2 Sample Injection Trigger Output Normally Open 48 amp 11 5 amp 6 Pump Stop TTL Active Low 2 amp Ground 4 amp GND Pump Stop TTL Active High 9 amp Ground 3 amp GND Ground to case 1 7 13 amp 14 GND Serial RS232 Port The MDS is fitted with two serial RS232 ports These two ports are reserved for future use 56 Agilent MDS User Manual Installation 3 Service Port and Switch The 1260 Infinity MDS is fitted with a serial RS232 service port and service switch for debugging and firmware upgrading of the instrument If the instrument is inadvertently powered on with the service switch set to Flash then the front panel screen will display EE SERVICE MODE Set rear switch to RUN then reboot system for normal operation For normal operation ensure the Service Switch is in the Run position prior to normal operation Agilent MDS User Manual 57 3 Installation Other Connections 58 Agilent MDS User Manual Agilent MDS User Manual 4 Controlling the 1260 Infinity
36. IN Range 0 3600 Secs SIGNAL GAIN fault ZERO OFFSET Default 30 Secs NOT READY Figure 16 RI Detector Menu Screens 72 Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The Items List consists of a scrollable list of items that are available for the detector or system menu option selected The items available in the menu option will be one or more of the following Sub Menu This provides access to further options for the detector s connected and the actual instrument Sub Menus are identified by the appended to the end of the item text Action This is an action that can be performed on the selected detector e g RI Autozero or Purge DP e Parameter This is a specific parameter for the selected detector or system It is either editable or read only All editable values are stored when the instrument is powered off Except Temperature and Laser Power Component This is a component of the selected detector that can be controlled and it s state changed for example LS Laser On Off or RI Purge Valve Open Closed Back This returns the menu screen up one level in the menu system In the Item List a Y and or 4 character can be displayed This indicates that more items are available either down or up the list To navigate through the Item List use the up and down arrow keys on the keypad During some actions the keypad will be locked with the Lock icon displayed in the Syst
37. Infinity MDS 4 The LS Parameters Menu Screen The LS Parameters Menu screen is used to access the LS detector parameters To access the LS Parameters screen select the Parameters sub menu option from the LS Detector Menu screen The items available in the menu are as follows Temperature This parameter sets the temperature of the LS detector in increments of 1 C There is also the option to turn the heater off The temperature range and default value are shown below Range 30 60 C Default off Laser Power This parameter sets the power level of the LS Laser as a percentage If a sample peak response is off scale then reducing the Laser power from 100 will bring the peak response back on scale The Laser power range and default value are shown below Range 10 100 Default 100 Back This option returns the display back to the LS Detector Menu screen Agilent MDS User Manual 89 4 Controlling the 1260 Infinity MDS The Analog Input Menus The 1260 Infinity MDS analog input menus are used to access the specific options actions and parameters for the two independent analog inputs located at the rear of the MDS Control Unit To access these menus select the Analog Input option from the Main Menu screen The Analog Input menu screens that are available are as follows The Analog Input Screen The Analog Input Parameters Screen User required components and parameters are located in the Analog Input and Anal
38. Manual Optimizing Performance 6 Purging the Viscometer The viscometer detector can be flushed with any miscible solvent 1 Before starting to flush the viscometer open the IP purge to allow the solvent flow to bypass the bridge and flush out the IP transducer 2 Pumping at 1 mL min flush the IP transducer for 15 min to ensure the solvent is fully exchanged 3 Now open the DP purge valve and close the IP valve The flow solvent will now flush the first half of the bridge and the DP transducer passing to waste from the transducer Again flush for 15 min at a flow of 1 mL min 4 Closing the DP purge valve will direct all the flow to the viscometer bridge and start flushing out the delay columns Each column has a flushing volume of 10 mL and therefore the total delay column flushing time will be approximately one hour at 1 mL min 5 If lower flow rates are used it is advisable to flush the viscometer overnight Monitor the pressure during the flushing procedure Do not exceed 5000 Pa DP and 100 kPa IP as this may damage the pressure transducers Before operation the viscometer should be again purged and the DP zeroed 1 Perform 3x IP Purge action with a 5 min purge time setting 2 Perform 3x DP Purge action with a 5 min purge time setting 3 Zero the DP out put The detector is fully equilibrated and ready to use Depending on the solvent choice some equilibration of the detector may be required This may last sev
39. Performance Specifications Type Specification Detection type Deflection Wavelength 658 nm Short term noise lt 80 pV Cell volume 6 uL Pressure rating 350 kPa 50 psi Wetted materials Temperature range Temperature stability pH range 316 SST Quartz 30 60 C 0 2 C 2 10 Table 4 Optional Viscometer Detector Performance Specifications Type Specification Shear rate typical 3000s Sensitivity Nsp 1 105 Pa s Pressure rating Temperature range Temperature stability pH range 50 kPa 7 psi 30 60 C 0 2 C 2 10 34 Agilent MDS User Manual Site Requirements and Specifications 2 Table5 Optional Dual Angle LS Detectors Performance Specifications Type Specification Sample cell volume 10 uL Scattering volume 0 01 pL Laser wavelength 658 nm Scattering angles 15 and 90 Temperature range 30 60 C Temperature stability 0 2 C pH range 2 10 Table 6 Optional DLS Detector Performance Specifications Type Specification Cell volume 10 pL Scattering Volume 0 01 pL Measurement range Rh 1 1000 nm Laser wavelength 658 nm Measuring angle 90 Minimum sample loading 40 pg Temperature range 30 60 C Temperature stability 0 2 C Correlator Data acquisition time pH range 512 channels multi tau 0 1 3600 s 2 10 1 150 KDa Monoclonial Antibody Conditions Agilent Bio SEC 3 300 A 7 8 x 300 mm 3 ym p n 5190 2511 Mobile phase PBS pH 7 4 Flow rat
40. Probable cause 1 Detector not fully equilibrated with environment 2 Contaminated flow cell 3 Damaged flow cell 4 Solvent in reference cell has deteriorated oxidised Suggested actions e Purge the RI detector thoroughly to remove air bubble e Use only degassed mobile phase Elevate waste reservoir above the level of flow cell Clean the flow cell thoroughly Refer to Maintaining and Cleaning the RI Flow Cell on page 109 for further information Move instrument to a more stable environment see Location of the Instrument on page 31 for more information Please contact your Agilent service representative Suggested actions Allow sufficient time for the system to thermally equilibrate with its environment Clean the flow cell thoroughly Refer to Routine Maintenance of the MDS System on page 105 for further information Check for liquid in front drain tube or drip gutter Contact Agilent for further assistance Purge the RI detector to refill the reference cell Add antioxidant to mobile phase Agilent MDS User Manual Flat baseline with no noise Probable cause 1 Faulty light source Low sensitivity Probable cause 1 Contaminated flow cell Mirrored peaks Probable cause 1 Purge valve not closed 2 Damaged flow cell Agilent MDS User Manual Troubleshooting and Diagnostics 7 Suggested actions Please contact your Agilent service representative Suggested actions
41. SD G7809A Agilent 1260 Infinity Bio SEC LS DLS 40 Agilent MDS User Manual Installation Kit Installation Agilent 1260 Infinity MDS Installation Kit G7800 68000 contains the following accessories required to install the instrument p n 5062 2463 G7800 63001 PLO100 3601 G7800 87000 G7800 87001 PLO100 3602 R005400012 G7800 90000 G7800 10000 Agilent MDS User Manual Description Corrugated tubing PP 6 5 mm id 5 m Agilent 1260 Infinity MDS USB Cable Valco Nut 1 16 inch 5 EA PTFE Tubing 0 25 mm ID x 1 6 mm OD 2 m PTFE Tubing 1 0 mm ID x 1 6 mm OD 2 m Valco Ferrule 1 16 inch 5 EA Double ended wrench 1 4 in and 5 16 in Agilent 1260 Infinity MDS Operators Manual CD Agilent 1260 Infinity MDS USB driver 3 41 3 Installation Installing the Instrument 42 If your 1260 Infinity MDS is part of a complete Agilent 1200 Infinity Series liquid chromatograph you can ensure optimum performance by installing the following configurations These configurations optimize the system flow path ensuring minimum delay volume The MDS with the Agilent 1200 Infinity Series The 1260 Infinity MDS is designed to operate with Agilent 1200 Infinity LC modules The instruments are connected by feeding the outlet from the column or UV detector to the MDS and then back into either the waste bottle or into the HPLC detector compartment depending on whether you wish to employ the detector that is already housed with the 12
42. Service This sub menu option displays the Service Options Menu screen To action any of the options within this Service screen a Pass Code is required This Service Menu screen should only be accessed by an Agilent engineer Back This option returns the display back to the Main Menu screen Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The System Options Parameters Menu Screen The System Options Parameters Menu screen is used to access the system options parameters To access the System Options Parameters screen select the Parameters sub menu option from the System Options Menu screen The items available in the menu are as follows Display Power This parameter sets the display power brightness of the display screen in increments of 25 Therefore a set value of 100 would be full brightness The display power range and default value are shown below Range 25 100 Default 75 Display Wait This parameter sets the display wait of the display screen in increments of 1 min It is the time of inactivity before the system automatically reduces the display power to minimum 25 This is done to extend the lifetime of the display screen If required there is the option to turn this off so that the display power is not automatically set to minimum The display wait range and default value are shown below Range 1 120 min with an Off option Default 20 min Screen Saver This parameter controls the scree
43. Space The module dimensions and weight see Table 2 on page 33 allow you to place the module on almost any desk or laboratory bench It needs an additional 2 5 cm 1 0 inches of space on either side and approximately 8 cm 8 1 inches in the rear for air circulation and electric connections If the bench shall carry a complete HPLC system make sure that the bench is designed to bear the weight of all modules The instrument is heavy 20 kg 44 Ib for an MDS dual compartment and 40 kg 88 Ib for quad compartment and thus it is advisable to locate the system on a sturdy bench Allow additional bench space for a PC if the instrument is to be computer controlled Location of the Instrument Place the instrument in an area that does not experience large temperature fluctuations Avoid positioning the MDS e in direct sunlight near heating equipment e near ventilation fans near sources of vibration and electrical noise near open windows and doors e in areas where corrosive gases exist e in dusty areas The instrument should not be stacked more than two enclosures high and suitable precautions should be taken to prevent the unit being knocked over Do not place solvent bottles or additional 1200 Infinity LC modules on the instrument Agilent MDS User Manual 31 2 Site Requirements and Specifications Extraction Requirement The MDS is not fitted with extraction but depending on the solvents used it might be neces
44. The graphic shows some of the symptoms that are prevalent with light scattering and the common reasons for such behavior Comparison of Good and Bad Baselines an Baseline spiking due to debris in the column or eluting from the columns Eluent particulates gives low level spiking Sinusoidal oscillation due to scattering from contaminated cell and destructive interference affects Figure 26 Example of typical light scattering baseline problems In most cases the cell can be cleaned and particulate matter can be removed by pumping pure solvent through it for several hours Agilent MDS User Manual 117 6 Optimizing Performance Shutting down the Instrument CAUTION Corrosive and oxidizing solvents Some solvents may corrode the detector s if they are not fully flushed from the system after use gt Remove corrosive solvents thoroughly from the entire system before switching off the instrument A continuous low flow rate of solvent through the MDS should be maintained during short term shut down especially if buffers tetrahydrofuran or organohalogens are used If the instrument is not to be used for short periods of time such as overnight or weekend it is recommended to follow the shut down procedure outlined below 1 Reduce the flow to 0 5 0 1 mL min 2 Leave the MDS powered on with the installed detector s at temperature if heating is used on overnight and on weekends This will keep the MDS detector
45. and I of the two halves of the RI cell When the reference and sample sides of the RI Cell are flushed into the same solvent and an autozero action performed then typically this value should be 1000 mV If the sum value is lt 200 mV the RI detector will be unable to perform an autozero action RI Error 3410 Sum values below 200 mV may indicate that there is an air bubble in the cell the cell is dirty or the RI detector needs servicing See Maintaining and Cleaning the RI Flow Cell on page 109 for further details This parameter is read only LFSC Value This parameter is the set LED Full Scale Current of the RI detector in mA This parameter is set during manufacture to give the specified detector sensitivity This parameter is read only Max LED Value This parameter is the maximum LED current value of the RI detector in mA This is the absolute maximum current that should be passed through the LED The value is determined from the manufacturer s data sheet and includes a temperature de rating factor This parameter is read only Agilent MDS User Manual 81 4 Controlling the 1260 Infinity MDS The Viscometer Menus 82 The MDS Viscometer menus are used to access the specific options actions components and parameters for the viscometer To access these menus select the VS Detector option from the Main Menu screen The Viscometer menu screens that are available are as follows The VS Detector Screen The VS Para
46. brate in the desired solvent Agilent MDS User Manual Optimizing Performance 6 Delay Hold Up Columns The delay columns play an important role in the viscometer operation While the polymer sample is passing through the detector s capillaries the hold up columns delay the polymer elution across one side of the viscometer bridge leading to an imbalance in the pressure across the viscometer Once the sample passes through the delay columns it creates a breakthrough peak The hold up columns are of sufficient volume that the breakthrough peak elutes after the sample peak has eluted The delay volume is provided by 2x delay columns that are fitted internally to the viscometer assembly A typical chromatogram showing the breakthrough peak is shown below Figure 23 Typical viscometer chromatogramm An early eluting breakthrough peak too close to the DP sample peak response may indicate a problem with the stability of the delay columns Typically the baseline noise that is expected from a viscometer should be 0 25 0 5 mV Greater values are often a result of poor pump performance The pattern of baseline noise observed on a viscometer can indicate the source of the problem Agilent MDS User Manual 113 114 Optimizing Performance A regular noise pattern as shown by the black trace in Figure 24 on page 114 is typical for a viscometer baseline with a pulsating pump This pattern can be suppressed by using a pulse dampen
47. built in detectors directly into Agilent Software via the USB port at the rear of the control unit The data is collected at 24 bit resolution with collecting rates of 1 2 5 and 10 Hz selectable within the software The software that is used to control and collect data from the 1260 Infinity MDS is dependent on the model Agilent GPC SEC Software is designed and optimized for use with the 1260 Infinity GPC SEC MDS system Agilent Bio SEC Software is designed amp optimized for use with the Agilent 1260 Infinity Bio SEC MDS system The 1260 Infinity MDS detector outputs are also available as analog signals 8 x 1 V A D outputs accessed from the rear of the control unit allowing the MDS to be used with any existing liquid chromatography system that supports Analog to Digital data collection It should be noted that a significant number of external HPLC software packages are not designed to perform multi detector GPC calculations Agilent MDS User Manual Introduction to the 1260 Infinity MDS 1 The 1260 Infinity MDS Refractive Index Detector The MDS differential refractive index detector is a high performance device that is specifically designed for GPC The RI detector features high signal to noise and low levels of drift and is fitted with a low dispersion cell to maintain peak shapes throughout the sample injection The heated cell environment means that excellent temperature stability is maintained giving ultra stable baselines
48. ction Additionally the following must be observed Do not remove instrument covers when operating Before the instrument is switched on all protective earth terminals extension cords auto transformers and devices connected to it must be connected to a protective earth via a ground socket Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury Whenever it is likely that the protection has been impaired the instrument must be made inoperative and be secured against any intended operation Make sure that only fuses with the required rated current and of the specified type normal blow time delay and so on are used for Agilent MDS User Manual 183 12 Appendix 2 General Safety Information replacement The use of repaired fuses and the short circuiting of fuse holders must be avoided Some adjustments described in the manual are made with power supplied to the instrument and protective covers removed Energy available at many points may if contacted result in personal injury Any adjustment maintenance and repair of the opened instrument under voltage should be avoided whenever possible When inevitable this has to be carried out by a skilled person who is aware of the hazard involved Do not attempt internal service or adjustment unless another person capable of rendering first aid and resuscitation is present Do not replace components with powe
49. ctly 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 Agilent MDS User Manual In this book In this book This manual contains information on e Agilent 1260 Infinity GPC SEC MDS G7800A e Agilent 1260 Infinity Bio SEC MDS G7805A 1 Introduction to the 1260 Infinity MDS This chapter gives an instrument overview and an introduction to the function of the MDS detectors 2 Site Requirements and Specifications This chapter provides information on environmental requirements physical and performance specifications 3 Installation This chapter gives information about the installation of your MDS instrument 4 Controlling the 1260 Infinity MDS This chapter describes how to control the instrument 5 Operating the 1260 Infinity Multi Detector Suite MDS This chapter describes the operational parameters of the instrument 6 Optimizing Performance This chapter gives hints on how to optimize the performance or use additional devices 7 Troubleshooting and Diagnostics
50. ctor Some solvents may corrode the detector s installed if they are not removed from the system after use However certain solvents can be left in the detector s at the end of operation For example water acetonitrile 2 propanol and paraffin derived hydrocarbons are quite innocuous They may be left in the MDS overnight or over a weekend Buffers The use of buffers even non corrosive buffers can lead to salt precipitation in the MDS detector s and tubings installed Keep the solvent flowing at a reduced rate to eliminate the possibility of salt precipitation Tetrahydrofuran THF is prone to auto oxidization Keeping the solvent flowing at a reduced rate minimizes re stabilization time upon startup of the chromatographic system Organohalogens A small amount of flow will minimize the amount of corrosive chloride impurities in the cell when using solvents such as methylene chloride and chloroform 102 Agilent MDS User Manual Agilent MDS User Manual 6 Optimizing Performance Location of the 1260 Infinity MDS 104 Routine Maintenance of the MDS System 105 Purging the Detectors 106 Purging the RI Detector 106 Purging the Viscometer 107 Purging the Light Scattering Detector 108 Purging the Dynamic Light Scattering Detector 108 Optimizing RI Performance 109 Maintaining and Cleaning the RI Flow Cell 109 Flushing the RI Flow Cell 109 Alternative Cell Cleaning Procedures 111 Optimizing Viscometer Performance 112 Dela
51. d Purge IP This action purges the IP transducer of the viscometer for the set Purge Time parameter value On Selecting The text IP Purge will be displayed in the System Status Area together with a count down clock of the IP purge time remaining The keypad is locked with the Lock icon displayed On Completion The text IP Purge Completed will be displayed in the System Status Area The keypad is unlocked with the Lock icon removed On Cancelling The text IP Purge Cancelled will be displayed in the in the System Status Area The keypad is unlocked with the Lock icon removed 84 Agilent MDS User Manual CAUTION Controlling the 1260 Infinity MDS 4 Autozero DP This action autozeros the DP transducer output of the viscometer to a fixed zero offset of 0 Pa On Selecting The text DP Autozero Completed will be displayed in the System Status Area Autozero IP This action autozeros the IP transducer output of the viscometer to a fixed zero offset of 0 kPa On Selecting The text IP Autozero Completed will be displayed in the System Status Area Autozero IP Incorrect use of autozero IP can lead to poor results gt Only Autozero the IP when flow rate is stopped and with no pressure on the system Parameters This sub menu option displays the VS Parameters Menu screen Service This sub menu option displays the VS Service Menu screen Only Agilent qualified engineers should access the VS Service Menu screen
52. d light showing rapid small fluctuations while larger particles such as protein aggregates nanoparticles polymers etc diffuse more slowly resulting in lower frequency fluctuations Agilent MDS User Manual 179 11 Appendix 1 Theory of Operation 180 The Autocorrelator The autocorrelation function of these short interval counts is computed by an autocorrelator which is a special purpose proprietary parallel computer that has been specially designed by Agilent Technologies The correlator uses 256 channels that can be distributed over a maximum channel space of 1024 channels Each channel can be considered as a separate bucket in which the emitted photons are counted during the sample period which is in the order of a few is The 1024 channel spaces occupy a total time space of 1024 equal sampling times that can be set by the operator according to the size and shape of the molecule of interest Counts are collected in up to 256 of these channel spaces which are arranged logarithmically throughout the total channel space by the software the higher density being at the start The autocorrelator function over the 1024 channel space is computed by correlating the counts in each of the channels Observation of the correlation function provides information that is useful to optimize the analysis In addition the display indicates the fraction of the sample with the indicated particle size Using Diffusion Coefficient
53. dard of solvent purity and general system cleanliness be maintained A contaminated flow cell can lead to noise and drift problems that are often mistakenly attributed to other areas of the system The use of filtered solvents with solvent reservoir filters in line filter between the pump and detector and a pre column will protect the cell from contamination and decrease the amount of cleaning required However contamination from trapped particulates or bubbles from precipitates or from thin films of residues can still occur Flushing the RI Flow Cell Connect the tubing directly from the pump outlet to the MDS RI Detector INLET port to bypass the column Connect the outlet port to waste Do not connect the MDS detectors in series when performing a cleaning procedure Some materials should be injected directly into the RI Detector by syringe due to their high corrosivity or safety risk If you encounter a large backpressure while flushing the cell proceed with caution as you could rupture the cell The following recommendations may be applicable to a variety of cleaning conditions Agilent MDS User Manual 109 110 Optimizing Performance Liquid purging Clean all internal lines of the RI detector by injecting cleaning solution with Purge off and inject cleaning solution again with Purge on Particulate matter can be removed by forcing liquid through the cell using a syringe Sometimes it helps to reverse flow and inject i
54. detector 34 photons 179 physical specifications 33 polarizability 173 polymer branching 166 polymer 163 power consideration 29 power consumption 33 power cords 30 power switch 45 pre installation requirements 28 pressure rating 34 34 purging DLS detector 108 LS detector 108 RI detector 106 viscometer 107 radio interference 186 Agilent MDS User Manual Rayleigh 35 refractive index 162 RI detector menus 76 S safety class 183 safety general information 183 standards 33 symbols 182 sample cell volume 35 scattering volume 35 sensitivity 34 serial RS232 port 56 shear rate 34 short term noise 34 site requirements power cords 30 Snell s refraction law 160 specification physical 33 specifications performance 34 start up screen 64 static light scattering 171 Staudinger 163 Stokes Einstein equation 180 storing the instrument 156 system menus 93 system problems 122 T temperature range 35 35 34 stability 35 35 34 temperature range 34 stability 34 Index U unpacking 38 USB 55 V viscometer menus 82 voltage range 33 W waste electrical and electronic equipment 185 wavelength 34 WEEE directive 185 weight 33 wetted materials 34 Wheatstone bridge 112 Wheatstonte bridge 166 189 www agilent com In This Book This manual contains information on Agilent 1260 Infinity GPC SEC MDS G7800A Agilent 1260 Infinity Bio SEC MDS G7805A The manual describes the following Int
55. detectors feature low dispersion tubing and minimized tubing distances to maintain low dispersion levels in the system resulting in excellent peak shapes with minimal band broadening Figure 3 Front view of the 2 and 4 Bay MDS systems 14 Agilent MDS User Manual Introduction to the 1260 Infinity MDS 1 Safety and GLP Features The 1260 Infinity MDS comes complete with several safety features and good laboratory practice GLP features to aid user confidence in the laboratory The instrument is equipped with a leak sensor should a spillage occur within the instrument a signal is sent via the Auxiliary I O Port The port may be connected to the LC system operating with the 1260 Infinity MDS to shut down the pump and minimize solvent spillage The keypad is locked on receiving a sample injection trigger via the Auxiliary I O port or from a Start Collection command from the Agilent GPC SEC Software if used Locking the keypad ensures that the parameters of the detector s cannot be changed while the sample injection run is in progress Application Areas The versatile setup of the 1260 Infinity MDS allows different types of analysis to be performed from the traditional conventional GPC SEC using a column calibration to the information rich multi detector GPC SEC techniques that allow both accurate and reliable molecular weight information to be determined as well as giving key information on the behavior of the polymer molecule
56. down with a cloth moistened with deionized water Ensure that no moisture enters the instrument WARNING Electrical shock and burns Liquid in the module electronics can cause shock hazard and damage the module gt Switch off and disconnect power cord from instrument before cleaning gt Do not use an excessively damp cloth during cleaning gt Drain all solvent lines before opening any fittings gt Allow the instrument to dry off completely before reconnecting power 154 Agilent MDS User Manual Maintenance 9 Inspection of Cables Periodically inspect the connecting cables for signs of physical damage caused by abrasion solvent spillage impact etc Replace damaged cables particularly the power cord if any damage is observed Agilent MDS User Manual 155 9 Maintenance Putting the Instrument into Long Term Storage CAUTION Corrosive and oxidizing solvents Some solvents may corrode the detector s if they are not fully flushed from the system after use gt Remove corrosive solvents thoroughly from the entire system before switching off the instrument For flushing use solvent with the following characteristics No dissolved salts acids bases or halides Low vapour pressure at storage temperatures Does not allow bacterial growth Does not oxidize or form peroxides Follow this procedure if the instrument is to be stored or not used for an extended period of time 1 Purge the pump with a mixtu
57. e 0 75 mL min Agilent MDS User Manual 35 2 Site Requirements and Specifications Performance Specifications 36 Agilent MDS User Manual Agilent MDS User Manual 3 Installation Unpacking the Module 38 Installing the Instrument 42 The MDS with the Agilent 1200 Infinity Series 42 Dual Stack Configuration 43 Connection to a 3rd Party LC System 44 Installing the G7800 MDS 45 Powering the Instrument On or Off 46 Detector Output Channel Assignment 47 Fluid Connections 49 Single Detector System 50 Dual Detector System 51 Triple Detector System 53 Other Connections 54 USB Port 55 Analog Outputs 55 Analog Inputs 55 Auxiliary 1 0 Port 56 Serial RS232 Port 56 Service Port and Switch 57 This chapter gives information about the installation of your MDS instrument Ee Agilent Technologies 37 3 Installation Unpacking the Module Damaged Packaging CAUTION If the delivery packaging shows signs of external damage please call your Agilent Technologies sales and service office immediately Inform your service representative that the instrument may have been damaged during shipment 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 you
58. e performed at a wavelength of 658 nm The signal detection and signal processing method allows the refractive index to be given out in the online mode without absorption components The autozero range includes the complete measurement range The refractive index is highly temperature dependent The change per 1 C for pure water is 1 10 RIU and for typical organic solvents is 5 10 RIU Agilent MDS User Manual 161 11 Appendix 1 Theory of Operation Using Refractive Index Measurements to Measure Concentration Refractive index measurements can be used to determine the compound concentration in the chromatographic slice The difference in refractive index between the solution under study and the pure solvent is measured by passing a light beam through two cells One of the cells contains pure solvent and the other contains the eluent as it passes through the cell after the column The cell with the pure solvent should be filled with the solvent before the separation and should have the same temperature as the eluent The observed signal RI which corresponds to the light beam deviation is proportional to the difference in the refractive index of the fluid in the two cells as shown in the following equation RI K dn dc c where gt K instrument constant C sample concentration in the solvent dn de the change in the refractive index as a function of the change in concentration It is considered to be a constant for
59. ed in the System Status Area Parameters This sub menu option displays the Analog Input Parameters Menu screen Back This option returns the display back to the Main Menu screen Agilent MDS User Manual 91 4 92 Controlling the 1260 Infinity MDS The Analog Input Parameters Menu Screen The Analog Input Parameters Menu screen is used to access the parameters for the two analog input channels To access the Analog Input Parameters screen select the Parameters sub menu option from the Analog Input Menu screen The items available in the menu are as follows CH1 and CH2 Time Constant This parameter sets the applied smoothing level for the output of the channel 1 or 2 analog input in increments of 1 s The larger the value set the more the signal will be smoothed The CH1 and CH2 time constant range and default value are shown below Range 0 10s Default 1s Back This option returns the display back to the Analog Input Menu screen Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The System Options Menus The MDS System Options menus are used to access system information and parameters for the system To access these menus select the System Options option from the Main Menu screen The System Options menu screens that are available are as follows The System Options screen The System Parameters screen The System Service screen User required parameters are located in the System Options Para
60. els 1 4 can be collected when using Cirrus software Agilent MDS User Manual Installation 3 Fluid Connections CAUTION The fluid connections are located on the front panel of each detector module the inlet port is on the left while the right port is the outlet Ensure the capillaries that are connected to the inlet and outlet ports are not reversed since this could cause damage to the detector The MDS RI detector has a pressure rating of 350 kPa 50 psi so additional detectors can be connected after the outlet e g the MDS Viscometer However exceeding this backpressure on the RI detector will lead to internal leaks and damage to the flow cell The MDS Viscometer has a pressure rating of 50 kPa 7 psi so it is recommended that no additional detectors be connected after the detector The maximum recommended flow rate that is permitted through the viscometer is 2 0 mL min For more viscous solvents for example 2 propanol it is not recommended to work at the maximum flow rates Do not exceed 5000 Pa differential pressure DP and 100 kPa for the inlet pressure IP The MDS LS and LS DLS detectors have pressure ratings of 350 kPa 50 psi so additional detectors can be connected after the outlet High backpressure Exceeding backpressure limits will lead to internal leaks and damage to the detector gt Do not exceed the backpressure limit of the detectors The tubing required for all detector configurations is shown
61. em Status Area Some actions can be cancelled by pressing the CE key on the keypad See The Keypad on page 61 The Information Area for Sub Menu Action Component and Back items displays information about the currently highlighted item and how to select it For the Component item the information displayed is dynamic and depends on the current state of the component e g LS Laser On or Off Agilent MDS User Manual 73 4 74 Controlling the 1260 Infinity MDS The Information Area for a highlighted Parameter item displays the current set value the settable range for the parameter and the default value To edit a highlighted parameter press either the Select Enter or right arrow keys on the keypad The current set value of the parameter will now be highlighted in the Information Area Either type in the required value from the keypad or use the up and down arrow keys to scroll through the available values Press either the Enter or Select keys on the keypad to set the new parameter value The set value will no longer be highlighted and the cursor returns to the Items List If an invalid value is entered the entry will be ignored and the parameter value reverts to the last valid value set To cancel an entry and return the cursor to the Items List press either the CE or left arrow keys on the keypad For read only parameter values Read Only and the value units will be displayed in the range and default value respectively T
62. ent types in the WEEE Directive Annex I this product is classed as a Monitoring 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 Agilent MDS User Manual 185 12 Appendix 2 General Safety Information Radio Interference Cables supplied by Agilent Technologies are screened to provide optimized protection against radio interference All cables are in compliance with safety 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 186 Agilent MDS User Manual Appendix 2 General Safety Information 12 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 Agilent MDS User Manual 187 Index Index A Agilent oninternet 187 ambient non operating temperature 33 ambient operating temperature 33 analog input menus 90 analog inputs 55 autocorrelator 180 auxiliary I O port 56 avalanche photodiode 179 B bench space 31 Benoit 165 Brownian movement 179 C cell contamination 105 cell volume 34 cleaning 154 D dead volume 104 defect on arrival 38
63. enu screen Back This option returns the display back to the Main Menu screen Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The RI Parameters Menu Screen The RI Parameters Menu screen is used to access the RI detector parameters To access the RI Parameters screen select the Parameters sub menu option from the RI Detector Menu screen The items available in the menu are as follows Purge Time This parameter defines the time delay between the RI purge valve opening and closing during a purge action selected from the RI Detector Menu screen The time range and default value are shown below Range 0 600s Default 30s Temperature This parameter sets the temperature of the RI detector in increments of 1 C There is also the option to turn the heater off The temperature range and default value are shown below Range 30 60 C with an Off option Default Off Polarity This parameter sets the polarity of the RI detector output If the polarity is set to ve then the detector signal is flipped i e sample peaks with a negative output in ve mode become positive outputs in ve mode The polarity range and default value are shown below Range ve ve Default ve Agilent MDS User Manual 79 4 80 Controlling the 1260 Infinity MDS Signal Time This parameter sets the applied smoothing level of the RI detector output in increments of 0 1 sec The larger the value set the more the
64. er visible wavelength radiation blue light is scattered more strongly by the gas molecules in air than light of longer wavelengths red light There are two general techniques for the measurement of physical properties of polymers synthetic polymers and natural polymers such as proteins and polysaccharides and particles Static Light Scattering Also known as Rayleigh scattering or classical light scattering the intensity of the scattered light from the sample dissolved in the solvent This difference between the two measurements can be used to determine the average molecular weight and Rg radius of gyration To complete the molecular weight determination the concentration of the compound of interest is required typically obtained from a refractive index detector or an absorbance detector Static Light Scattering is described in Static Light Scattering on page 173 Dynamic Light Scattering Also known as Quasi elastic scattering Photocorrelation Spectroscopy or Beat Spectroscopy the fluctuations of the intensity of the scattered light is used to determine the diffusion coefficient of the molecules as they move in solution Brownian motion The Stokes Einstein equation is used to determine Rh the hydrodynamic radius of the molecule Dynamic Light Scattering is described in Measuring Rh Using Dynamic Light Scattering on page 179 Static and Dynamic measurements can be made on a sample in a cuvette or in a flowing s
65. eral hours Agilent MDS User Manual 107 6 Optimizing Performance Purging the Light Scattering Detector The LS detector can be flushed with any miscible solvent Monitor the pressure during the flushing procedure to ensure that excessive pressure does not occur Depending on the solvent choice some equilibration of the detector may be required This may last several hours 1 Introduce the solvent at a reduced flow of typically no higher than 0 5 mL min into the flow cell 2 Flush the sample cell for a minimum of 5 min 3 Increase the flow to the operating flow typically 1 0 mL min The detector is fully equilibrated and ready to use Purging the Dynamic Light Scattering Detector The LS detector can be flushed with any miscible solvent Monitor the pressure during the flushing procedure to ensure that excessive pressure does not occur Depending on the solvent choice some equilibration of the detector may be required This may last several hours 1 Introduce the solvent at a reduced flow of typically no higher than 0 5 mL min into the flow cell 2 Flush the sample cell for a minimum of 5 min 3 Increase the flow to the operating flow typically 1 0 mL min The detector is fully equilibrated and ready to use 108 Agilent MDS User Manual Optimizing Performance 6 Optimizing RI Performance Maintaining and Cleaning the RI Flow Cell The high sensitivity of the RI detector makes it imperative that a high stan
66. g inputs Auxiliary 1 0 port Service port USB port Service switch Run Flash Serial RS232 ports reserved Mains input oo ont oo nan FF wo PDP Fuses Mains switch 54 Agilent MDS User Manual Installation 3 USB Port CAUTION USB drivers not installed gt Install the USB drivers before you connect the USB cable to the PC The Agilent 1260 Infinity MDS is fitted with a USB 2 0 full speed connection for digital data acquisition into Agilent GPC SEC or Bio SEC software Analog Outputs The MDS is supplied with 8 1 V analog outputs The analog outputs are not fixed to specific detectors but are assigned according to the detector s present in the instrument Analog Inputs The MDS has two independent analog input channels located on the rear panel of the Control Unit These are used for connecting signal outputs from external detectors to be collected digitally into Agilent GPC SEC software via the USB cable Each input can have a zero offset applied Agilent MDS User Manual 55 3 Installation Auxiliary 1 0 Port CAUTION The Pump stop facility must be employed if the instrument is to be left unattended gt Connect the auxiliary cable Agilent 1260 Infinity MDS Auxiliary 1 0 cable G7800 63003 between MDS auxiliary port and remote port on 1200 Series LC System The MDS is fitted with an auxiliary 15 pin I O connection for connecting the supplied auxiliary
67. h the filtered mobile phase to waste and then allow to stabilize Fit an in line filter between pump and injection valve Clean the flow cell thoroughly Refer to Routine Maintenance of the MDS System on page 105 for further information Suggested actions Check laser is switched on Please contact your Agilent service representative Agilent MDS User Manual Agilent MDS User Manual 8 Error Information What Are Error Messages 133 System Error Messages 134 Upper Leak Sensor Failed 134 Upper Leak Sensor Failed 134 Lower Leak Sensor Failed 135 Lower Leak Sensor Failed 135 Leak Detected in Upper Enclosure 136 Leak Detected in Bottom Enclosure 136 Rear Fan Failed in Control Unit 137 Fan Failed in Upper Enclosure 137 Fan Failed in Lower Enclosure 138 Fan Failed on Control Unit Power Supply 138 Communication to RI Detector Failed 139 Communication to VS Detector Failed 139 Communication to ADC Failed 140 Communication to LS Detector Failed 140 Communication to Control Unit Failed 140 RI Detector Specific Error Messages 141 Heated Block exceeded lower limit 141 Heated Block exceeded upper limit 141 LED Light Source Error 141 Autozero Error 142 Viscometer Specific Error Messages 143 Temperature Sensor Error 143 Unable to reach temperature set point 143 Heater Error 144 IP Purge Valve Error 144 DP Purge Valve Error 145 ote Agilent Technologies 131 8 Error Information LS and DLS Detector Specific Error Mes
68. hat is capable of measuring solution based viscosities for a wide range of polymer samples and molecular weights The balanced bridge design ensures that high sensitivity and a low shearing rate are maintained throughout the molecular weight range of analysis giving excellent baseline stability The pressure transducers that are used in the system give a high sensitivity and fast response time ensuring that sharp clean peaks are obtained The viscometer outputs of differential and inlet pressure values allow a dynamic measurement of inlet pressure to be used in calculations for greater accuracy in results The MDS Viscometer has a pressure rating of 50 kPa 7 psi so it is recommended that no additional detectors be connected after the detector Exceeding this backpressure on the viscometer will lead to internal leaks The maximum recommended flow rate that is permitted through the viscometer is 2 mL min For more viscous solvents for example 2 propanol it is not recommended to work at the maximum flow rates Do not exceed 5000 Pa for the differential pressure DP and 100 kPa for the inlet pressure IP Agilent MDS User Manual 21 1 Introductio n to the 1260 Infinity MDS Waste DP purge valve Outlet Delay Columns IP purge valve Figure 4 Flow path of MDS Viscometer during purge Red lines flowing path Black lines immobilized mobile path The T connection results in both sides of t
69. he 1260 Infinity MDS 4 The detector status icons displayed are Table 10 Status icon information Status Detector Area Description Icon T All Temperature Status Static Detector at set temperature Flashing Detector going to set temperature Flashing with a cross Heater is off P RI amp VS Purge Valve Status Flashing Purge Valve Open A RI Only Autozero Status Flashing Autozero in progress L LS Only Laser Status e Static Laser On Flashing with a cross Laser off The System Status Area of the Home screen displays information for the whole MDS system The following information is displayed in the System Status Area e The system status state i e Ready or Not Ready see Table 10 on page 67 e The keypad status e The data collection injection status e Any errors that occur For the keypad status there are two states locked and unlocked For the locked state the Lock icon is displayed The Lock icon will be displayed when e The keypad is manually locked e The Agilent Software GPC SEC or Bio SEC Software connects to the MDS e The Control Unit receives a sample injection trigger via the Auxiliary I O port or from a Start Collection command from the Agilent GPC SEC software if used e An error occurs Agilent MDS User Manual 67 4 68 Controlling the 1260 Infinity MDS When the keypad is unlocked the Lock icon is removed from the System Status Area
70. he Detector Status Area displays the current detector selected and the detector signal and temperature outputs For the two analog inputs only the outputs are displayed The information displayed for the individual detectors is shown overleaf Table 11 Status icon information Detector Displayed Detector Information RI lt Output gt mV lt Temperature gt C VS lt DP Output gt Pa lt IP Output gt kPa lt Temperature gt C LS lt 15 Output gt mV lt 90 Output gt mV lt Temperature gt C Analog In Ch1 lt Output gt mV Ch2 lt Output gt mV The System Status Area within the Detector and System Menu screens displays the system status states either Ready or Not Ready see Table 10 on page 67 or information about an action performed or a change in state of a component The action or component information is displayed throughout the selected Detector Menu screens unless another action or component state change is selected On returning to the Main Menu or Home screens the information is cleared Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The System Status Area also displays any detector errors that occur The system status action or component information will be replaced with the error An error code and message will be displayed For further details on system and detector errors see What Are Error Messages on page 133 For detailed information on the individual Detector and System Menu screens
71. he flow cell always being exposed to the same pressure 22 Agilent MDS User Manual Introduction to the 1260 Infinity MDS 1 Waste DP purge valve 7 gt Inlet Outlet Delay Columns IP purge valve Figure 5 Flow path of MDS Viscometer during DP purge Red lines flowing path Black lines immobilized mobile path The T connection results in both sides of the flow cell always being exposed to the same pressure Before running solvent through the device make sure that the solvent within the detector is completely miscible with the intended solvent to be used In case of immiscible solvents the bridge and transducers must be rinsed through with an intermediate solvent for example acetone which is miscible with both solvents The GPC SEC MDS viscometer is shipped in tetrahydrofuran Agilent MDS User Manual 23 1 Introduction to the 1260 Infinity MDS The 1260 Infinity MDS Dual Angle Light Scattering Detector 24 The MDS LS detector is a Dual Angle 15 90 Light Scattering Detector which is capable of measuring the molecular weight and molecular dimensions of polymer molecules in solution without the need for a column calibration The light scattering detectors maintain excellent signal to noise and the small cell volume size and heated cell environment ensure that excellent peak shapes are maintained Agilent MDS User Manual Introduction
72. if required 4 Install the MDS drivers on the PC if required Ensure the power switch at the rear of the instrument is OFF Connect the power cable to the power connector at the rear of the instrument 7 Connect the USB cable to the PC 8 Connect the remote start cable to the remote port on any 1260 Infinity series LC module Connect the fluid tubings see Fluid Connections on page 49 10 Turn on the power by switching the main power rocker located at the rear of the control unit to ON Agilent MDS User Manual 45 3 46 Installation Powering the Instrument On or Off 1 Turn on the power by switching the main power rocker located at the rear of the control unit to ON The front panel display screen initially shows the Start up screen Switching the MDS on provides power to all the components integrated in the system The control unit also sets up the Home screen see The Home Screen on page 65 The display should resemble the physical location of the detector s in the MDS and the Menu system see The Menu System on page 69 so that only the installed detector options are available Agilent MDS User Manual Installation 3 Detector Output Channel Assignment When powered on the MDS Control Unit performs the following initializing procedure Instrument components are checked and set e The detector bays are probed to determine the detector s installed with the detector s set to
73. iled Probable cause Suggested actions 1 Defective heater Please contact your Agilent service representative 2 Heater not connected to LS detector main Please contact your Agilent service board representative 3 Defective LS Detector main board Please contact your Agilent service representative Laser Error Laser current outside of normal operating range Probable cause Suggested actions 1 Laser Assembly is defective Please contact your Agilent service representative 2 Laser Assembly not connected to detector Please contact your Agilent service main board representative 3 Laser Interlock switch not connected to Please contact your Agilent service detector main board representative 4 Laser Interlock switch is defective Please contact your Agilent service representative 5 Defective LS Detector main board Please contact your Agilent service representative Agilent MDS User Manual 147 8 Error Information LS and DLS Detector Specific Error Messages 148 Agilent MDS User Manual Agilent MDS User Manual 9 Maintenance Introduction to Maintenance 150 Information for Service Personnel 151 Warnings and Cautions 152 Cleaning the Module 154 Inspection of Cables 155 Putting the Instrument into Long Term Storage 156 This chapter describes the maintenance of the 1260 Infinity Mulit Detector Suite Apg Agilent Technologies 149 9 Maintenance Introduction to Maintenance Trained personnel only should carry o
74. in 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 corre
75. ing device and or increasing the backpressure on the pump Liquid chromatography pumps function more effectively when they are working against some pressure 71 5 MPa Comparison of Pulsation Traces for Varian 212 Pump at Imi min Figure 24 Example of typical viscometer baseline problems High levels of baseline noise can also be seen when the viscometer hasn t been purged correctly see Purging the Detectors on page 106 and or the viscometer hasn t been given enough time to equilibrate before starting the analysis Agilent MDS User Manual Optimizing Performance 6 Optimizing Light Scattering Performance Maintaining and Cleaning the LS Flow Cell A typical mistake when using light scattering especially with a new unit is pumping the fines that are typically present in new columns into the light scattering cell This causes a high baseline offset and in the worst case a dirty flow cell requiring cleaning When using light scattering it is highly recommended to flush new columns with at least 10 column volumes of solvent before connecting them to the light scattering detector In addition another common mistake is to turn the pump on and off without proper flow rate control Turning the pump from zero flow to 1 mL min has the effect of shocking the column bed This again releases fines from the column and radically affects the light scattering baselines causing increased off set and spikes It is therefore recommended t
76. internal fluid leakage Never allow the DP transducer to exceed 5000 Pa and the IP transducer to exceed 100 kPa e When transferring the viscometer between solvents always start the pump at reduced flow rates lt 0 2 mL min See Purging the Viscometer on page 107 e Note that the DP value may be offset with the autozero function at anytime e Autozero should be applied to the IP value only if the flow through the viscometer is zero and the LC pump purge valve is opened to remove pressure in the system Agilent MDS User Manual 99 5 100 Operating the 1260 Infinity Multi Detector Suite MDS Preparing the LS and DLS Detector Always triple filter the mobile phase through 0 1 um filters Always filter the samples prior to injection If the solvent is changed make sure that the two solvents are miscible If not use an intermediate solvent such as isopropanol If you are using a buffer make certain that the buffer salt is soluble in the mobile phase If a new column is used flush it with five volumes of mobile phase before connecting it to the detector The cell should not be allowed to dry out Keep the LS cell clean see Maintaining and Cleaning the LS Flow Cell on page 115 Agilent MDS User Manual Operating the 1260 Infinity Multi Detector Suite MDS 5 Pumping Systems It is recommended to use a high performance pumping system with no flow pulses to maximise viscometer performance Inconsiste
77. ion 15 data is also used with 90 data to measure Rg the radius of gyration of molecules over a limited range of sizes 12 150 nm using static light scattering analysis High Angle Light Scattering High angle light scattering data is collected at a 90 angle to the incident beam and is typically used with static light scattering analysis to measure the molecular weight of smaller molecules such as proteins with a molecular weight below 1 10 Da random coils with molecular weight below 2 105 Da and for lower molecular weight non spherical coil polymers In addition it is used with dynamic light scattering analysis to measure Rh the hydrodynamic radius of molecules and particles from 1 to 1000 nm n lim sp Agilent MDS User Manual Appendix 1 Theory of Operation 11 Measuring Rh Using Dynamic Light Scattering Basics of Dynamic Light Scattering The fundamental measurement for dynamic light scattering is the fluctuation of the intensity of the scattered light This data is analyzed as described to yield the diffusion of the molecules or particles moving under Brownian movement When polarized laser light is scattered the scattered light is at the same wavelength as the incident beam However it should be noted that when the light is monitored over extremely short time increments in the microsecond time regime a Doppler shift occurs and the frequency of the light appears to be changing As the particle
78. ions To access the RI Detector screen select the RI Detector option from the Main Menu screen The items available in the menu are as follows Autozero This action zeros the RI detector output to the set Zero Offset parameter value On Selecting A Z The text RI Autozero is displayed in the System Status Area The keypad is locked with the Lock icon displayed On A Z Completion The text RI Autozero Completed is displayed in the System Status Area The keypad is unlocked with the Lock icon removed It is not possible to cancel the autozero command once selected Purge This action purges the RI detector for the set Purge Time parameter value On Selecting The text RI Purge is displayed in the System Status Area together with a count down clock of the RI purge time remaining The keypad is locked with the Lock icon displayed On Completion The text RI Purge Completed is displayed in the System Status Area The keypad is unlocked with the Lock icon removed On Cancelling The text RI Purge Cancelled is displayed in the System Status Area The keypad is unlocked with the Lock icon removed To cancel the Purge action press the CE key on the keypad Agilent MDS User Manual 71 4 78 Controlling the 1260 Infinity MDS Parameters This sub menu option displays the RI Parameters Menu screen Service This sub menu option displays the RI Service Menu screen Only Agilent qualified engineers should access the RI Service M
79. lling the Instrument 60 The Instrument Display 64 The RI Detector Menus 76 The Viscometer Menus 82 The LS Detector Menus 87 The Analog Input Menus 90 The System Options Menus 93 5 Operating the 1260 Infinity Multi Detector Suite MDS 97 Using the Instrument 98 Pumping Systems 101 Agilent MDS User Manual Contents Optimizing Performance 103 Location of the 1260 Infinity MDS 104 Routine Maintenance of the MDS System 105 Purging the Detectors 106 Optimizing RI Performance 109 Optimizing Viscometer Performance 112 Optimizing Light Scattering Performance 115 Shutting down the Instrument 118 Troubleshooting and Diagnostics 119 Troubleshooting 120 Troubleshooting an LC System 121 System Problems 122 RI Detector Problems 124 Viscometer Detector Problems 127 Light Scattering Detector Problems 129 Error Information 131 What Are Error Messages 133 System ErrorMessages 134 RI Detector Specific Error Messages 141 Viscometer Specific Error Messages 143 LS and DLS Detector Specific Error Messages 146 Maintenance 149 Introduction to Maintenance 150 Information for Service Personnel 151 Warnings and Cautions 152 Cleaning the Module 154 Inspection of Cables 155 Putting the Instrument into Long Term Storage 156 10 Parts and Materials for Maintenance 157 Parts and Materials for Maintenance 158 Agilent MDS User Manual Contents 11 Appendix 1 Theory of Operation 159 The 1260 Infinity MDS Refractive Index
80. meters screen The complete structure of the MDS System Options Menu screens is as follows System Options gt System Options System Info Parameters Sys Opt Parameters Display Power Display Wait ScreenSaver Back Service Sys Opt Service Screen Test Keypad Test Simulation Mode Test Debug Mode Back Figure 21 MDS System Options Menu Structure Agilent MDS User Manual 93 4 94 Controlling the 1260 Infinity MDS The System Options Menu Screen The System Options Menu screen is used to access the system information and the system parameters To access the System Options screen select the System Options option from the Main Menu screen The items available in the menu are as follows System Info The System Info screen displays the firmware versions of the modules installed in your MDS instrument It consists of the firmware versions used in the MDS Control Unit and the installed MDS detectors The full list of modules is shown below e MMI Used in the MDS Control Unit e STB Used in the MDS Control Unit ACQ Used in the MDS Control Unit e RI Used in the MDS RI Detector e VS Used in the MDS Viscometer LS Used in the MDS LS Detector The information displayed for each module is the Version and Build of the firmware in use For example MMI 1 0 B89 is firmware version 1 0 build 89 for the MMI module Parameters This sub menu option displays the System Options Parameters Menu screen
81. meters Screen The VS Service Screen User required actions and parameters are located in the VS Detector and VS Parameters screens Components for service and checking viscometer are located in the VS Service screen The complete structures of the MDS RI Detector Menu screens are as follows Agilent MDS User Manual Controlling the 1260 Infinity MDS The Viscometer Menus VS Detector gt Service Figure 18 The MDS Viscometer Menus Agilent MDS User Manual vs Parameters _ 4 83 4 Controlling the 1260 Infinity MDS The VS Detector Menu Screen The VS Detector Menu screen is used to access the purge and autozero actions for the viscometer the detector parameters and service options To access the VS Detector screen select the VS Detector option from the Main Menu screen The items available in the menu are as follows Purge DP This action purges the DP transducer of the viscometer for the set Purge Time parameter value On Selecting The text DP Purge will be displayed in the System Status Area together with a count down clock of the DP purge time remaining The keypad is locked with the Lock icon displayed On Completion The text DP Purge Completed will be displayed in the System Status Area The keypad is unlocked with the Lock icon removed On Cancelling The text DP Purge Cancelled will be displayed in the in the System Status Area The keypad is unlocked with the Lock icon remove
82. n saver behaviour Range On Off Default On Back This option returns the display back to the System Options Menu screen Agilent MDS User Manual 95 4 Controlling the 1260 Infinity MDS The System Options Menus 96 Agilent MDS User Manual Agilent MDS User Manual Operating the 1260 Infinity Multi Detector Suite MDS Using the Instrument 98 Preparing the 1260 Infinity Multi Detector Suite 98 Preparing the RI Detector 99 Preparing the Viscometer 99 Preparing the LS and DLS Detector Pumping Systems 101 Mobile Phase Priming Solvent Information 100 101 102 This chapter describes the operational parameters of the instrument ea Agilent Technologies 97 5 Operating the 1260 Infinity Multi Detector Suite MDS Using the Instrument 98 Preparing the 1260 Infinity Multi Detector Suite Locate the 1260 Infinity MDS in an area that does not experience large temperature changes See Physical Specifications on page 33 for details Do not place solvent bottles on top of the instrument Always pre mix and de gas the mobile phase Do not allow pumps to mix solvents for the mobile phase Use only isocratic conditions Always use tubing of 1 0 mm i d 0 040 in or greater on the RI detector s viscometer s purge waste outlet When using buffer solutions flush the system with water before switching it off Growth of algae should be avoided Always use an inline filter with Light scattering detecti
83. n the OUTLET port If liquid purging does not work try gas purging See Purging the Detectors on page 106 for further details on the correct purge procedure Gas purging Replace cell liquid with a volatile solvent for example acetone Purge and dry the cells with clean gas at about 15 psi Gas flowing through the cell will sometimes dislodge particles Also try reversing the flow direction For difficult entrapments follow the above gas purge procedure with a liquid purge When liquid hits a particle in a dry cell it is generally more effective than a continuous liquid purge Entrapped bubbles If you suspect that you have a problem with entrapped bubbles purge with propan 2 ol Heating the flow cell during the cleaning procedure can help remove marginally soluble material Agilent MDS User Manual Optimizing Performance 6 Alternative Cell Cleaning Procedures If buffers or solutions of high salt content have been in use the cells may be contaminated by precipitated salt Flushing with large amounts of distilled deionized water at 1 mL min for up to several hours is the simplest clean up procedure An elevated cell temperature will speed up dissolution The water wash can be acidified if the precipitated salt is more soluble in acidic solutions do not exceed pH 2 However do not use strongly basic pH 10 or higher solutions as these will etch the refractive index cell If contamination is suspected when a
84. ne One possible implication is that the noise arises from pressure fluctuations to which the refractive index detector is more sensitive If both detectors are showing noise a power line current may be indicated If both detectors show anomalous baseline performance such as huge peaks that continue indefinitely a bleed off problem material from the column or immiscible solvents trapped in the system is more likely Agilent MDS User Manual 121 7 Troubleshooting and Diagnostics System Problems 122 Excessive baseline noise Probable cause 1 Air bubble in pump 2 Particulates in the mobile phase 3 Formation of gases in the mobile phase reservoir 4 Particles shedding from analytical column 5 Environmental temperature fluctuations 6 Damper has inadequate damping capacity for system 7 Damper is operating at a pressure where performance is poor 8 Incorrect compressibility setting for mobile phase 9 External detector inputs outputs are faulty Suggested actions Purge the pump heads Use only premixed degassed mobile phase e Filter the mobile phase e Flush the system thoroughly with the filtered mobile phase to waste and then allow to stabilise Use only premixed degassed mobile phase Use an in line degasser Condition the columns by flushing with solvent prior to use Fit an in line filter after the column Move instrument to a more stable environment see Location of the Instrument on
85. ns 1 Particles shedding from analytical column Condition with at least 10 column volumes by flushing with solvent to waste prior to use Fit an in line filter after the column 2 Particles floating in the cell that do not exit Filter the mobile phase through lt 0 2 um easily after continuous pumping membrane e Flush the system thoroughly with the filtered mobile phase to waste and then allow to stabilise Fit an in line filter between pump and injection valve 3 Contaminated flow cell dues to salt crystals Flush the system thoroughly with filtered water deposited in the cell and lens after an to re dissolve the salts in the cell and then inappropriate solvent was used to flush the allow to stabilise system following use of a salt buffer 4 Dried sample and other material when the Filter the mobile phase through lt 0 2 um cell has been allowed to run dry and the membrane solvent has evaporated e Flush the system thoroughly with the filtered mobile phase to waste and then allow to stabilize Fit an in line filter between pump and injection valve Agilent MDS User Manual 129 7 Troubleshooting and Diagnostics High baseline offset Probable cause 1 Particulates in the mobile phase 2 Contaminated flow cell No signal outputs Probable cause 1 Laser not switched on 2 Faulty laser 130 Suggested actions e Filter the mobile phase through lt 0 2 um membrane e Flush the system thoroughly wit
86. nt solvent flow will result in poor system performance A backpressure regulator maybe necessary on certain pumps in order to minimize pump pulsation This can also be achieved by the column itself or a coil of 0 127 mm 0 005 in i d tubing placed between the pump and the injector Mobile Phase Priming Make sure that the solvent within the detector s is completely miscible with the intended solvent to be used If this is not the case the detector s must be flushed through with an intermediate solvent e g acetone which is miscible with both solvents The entire flow system consisting of pump damper injector column MDS etc must be primed with the mobile phase Flush the entire system with 5 10 times the system volume until a steady baseline is obtained The mobile phase should be pre mixed and degassed before use Alternatively the mobile phase can be degassed online by a solvent degassing system Agilent MDS User Manual 101 5 Operating the 1260 Infinity Multi Detector Suite MDS Solvent Information The high sensitivity of the instrument makes it imperative that a high standard of solvent purity and general system cleanliness be maintained Use solvent reservoir filters to filter solvents Always degas solvents before use Eluents containing non volatile mineral acids or bases should be avoided Do not use strongly basic pH 10 or higher solutions as these will etch the quartz cell window of the MDS RI dete
87. o change the flow rate by no more than 0 2 mL min min Aqueous Eluents Water is a particularly poor scattering media and although this has the positive effect that the baseline offset is particularly low the negative effect is that any particle dust in the water scatters strongly giving rise to a spiky baseline To counteract this spiky baseline it is essential that the eluent is filtered down to 0 02 um the columns are thoroughly flushed to waste before being connected to the light scattering detector and an inline filter is fitted after the column immediately before the light scattering detector to minimize particles reaching the flow cell The addition of buffers to the water as long as they are fully soluble tend to have the effect of suppressing the dust and spiky appearance of the baseline but again filtration is essential The most common symptoms of a contaminated flow cell are high baseline noise and or the light scattering signals off scale Sinusoidal oscillation on the light scattering baselines Gif not temperature related is also a strong indication that the cell is dirty and requires cleaning Agilent MDS User Manual 115 116 Optimizing Performance The results that are shown in Figure 25 on page 116 demonstrate the typical QC test carried out on all the Agilent light scattering detectors with the indicated pass specifications The test probe is a polystyrene standard Mp 96000 g mol with a PDI of 1 03 dissolved in TH
88. o control the MDS If the keypad becomes unlocked the control software automatically locks it again within a couple of seconds e An error occurs The display shows the Home screen with the lock icon 8 when the keypad is automatically locked The lock and injection icons disappear from the Home screen when the keypad is unlocked The MDS Keypad remains locked when e The MDS Control Unit receives a sample injection trigger via the Auxiliary I O port without Agilent GPC SEC software used for data collection The injection icon also remains displayed Unlocked keypad Data can be lost if the keypad is unlocked and used while data collection is in progress or if the system is being controlled from a PC gt Lock the keypad during data collection or while controlling the system from the PC 62 Navigation through the menu system is not possible while the keypad is locked Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 1 To manually lock the keypad press the left and right arrow keys simultaneously When locking the keypad the display will show the Home screen with the lock icon displayed 2 To manually unlock the keypad press the left and right arrow keys simultaneously The lock icon will be removed from the Home screen when the keypad is unlocked Unlock the keypad manually in order to use the keypad and display to control the instrument Agilent MDS User Manual 63 4 Controlling the 1260
89. og Input Parameters screens The complete structure of the MDS Analog Input Menu screens is as follows Analog Input gt Analog Input CH1 Zero Offset CH2 Zero Offset Analog Input Parameters CH1 Time Constant CH1 Time Constant Back Figure 20 Analog Input Menu Structure Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The Analog Input Menu Screen The Analog Input Menu screen is used to access the zero offset actions for the two analog input channels the analog input parameters To access the Analog Input screen select the Analog Input option from the Main Menu screen The items available in the menu are as follows CH1 and CH2 Zero Offset This action is used to apply a fixed zero offset of 10 mV or clear the zero offset to the output of the channel 1 or 2 analog input When applying the 10 mV zero offset the MDS Control Unit calculates the offset required to bring the current output value for the channel 1 or 2 analog input to 10 mV This value is stored and applied to the output from then on The information text displayed is dynamic and is dependent on whether a zero offset has been applied or not If no zero offset is being applied default position On Selecting This will apply the zero offset with the text Zero Offset On displayed in the System Status Area If a zero offset is being applied On Selecting This will clear the zero offset with the text Zero Offset Off display
90. on Use a filter kit for inline filtering High pressure filter kit 5067 4638 When purging the reference side of the RID cell and viscometer transducers always use mobile phase that has eluted through the analytical column Allow mobile phase to flow through at least one column volume before purging the detector transducers See Purging the Detectors on page 106 Priming and Purging the System When the solvents have been exchanged or the system has been turned off for a certain time for example overnight oxygen will re diffuse into the solvent channel Therefore priming and purging of the system is required before starting an application Always filter solvents through 0 1 um filters Small particles reaching the MDS will result in poor performance of light scattering based detection Agilent MDS User Manual Operating the 1260 Infinity Multi Detector Suite MDS 5 Preparing the RI Detector e Never subject the detector to back pressures greater than 350 kPa 50 psi High pressures can cause internal fluid leakage or break the cell which is difficult to replace e Always fit the 5PSI bask pressure regulator on the waste outlet so that the reference side of the RI cell can be flushed during a purge Keep the RI cell clean see Maintaining and Cleaning the RI Flow Cell on page 109 Preparing the Viscometer Never subject the viscometer to backpressures greater than 50 kPa 7 psi High pressures can cause
91. ond conventional limits Performance Specifications on page 34 gives an overview of the system s performance specifications Agilent MDS User Manual 1 introduction to the 1260 Infinity MDS Instrument Overview Instrument Overview Basic Principles of Operation The 1260 Infinity MDS is designed to complement existing liquid chromatography systems to allow them to be used for GPC SEC configured with dual or quad detector cabinets depending on the detector choice see Figure 1 on page 12 Storage areas in the cabinet doors hold documentation essential instrument accessories and tools If a detector cabinet has an empty detector bay a tidy drawer system is supplied providing a convenient location for storing columns and larger accessories Figure 1 1260 Infinity MDS Quad and Dual Enclosure Configurations 12 Agilent MDS User Manual Introduction to the 1260 Infinity MDS 1 MDS Control Unit The MDS is controlled using the MDS Control Unit which is fixed on top of the detector enclosure s The control unit remains identical regardless of the configuration of detectors in the system allowing easy upgrading of additional detectors The control unit features an LCD display with built in keypad The keypad is used to control all aspects of the MDS and the LCD displays the status of the detectors within the instrument The MDS Control Unit provides the following Full control of each connected MDS detector using the buil
92. quation n KM Where K and a are coefficients specific to the polymer solvent system and temperature These coefficients can be determined by calibrating with polymer standards of known molecular weights A plot of Log n versus Log M a Mark Houwink Sakurada plot will be a straight line for a linear homopolymer as long as the Universal Calibration is obeyed Log n Log Log M Figure 28 Mark Houwink Sakurada Plot Values of a reflect the size of the molecule in solution ranging between 0 5 for a polymer behaving as a hard sphere to about 2 0 for rigid rods 164 Agilent MDS User Manual Appendix 1 Theory of Operation 11 Universal Calibration Benoit 1967 showed that polymers of different structure fall on the same calibration curve if the intrinsic viscosity is included as a calibration parameter A calibration plot of the product of intrinsic viscosity and molecular weight n M versus elution volume is a Universal Calibration as shown below in Figure 29 on page 165 This allows the system to be calibrated with polymer standards of one type and then analyze polymers of another type and still obtain accurate molecular weight distributions 40 PS 2 PS Gamb 10 PS Star 4 Hetero Graft Copol Poly methyt methacrylate log n M E Poly vinyl chloride 7 Graft Copal PS PMMA a Poly phenyl siloxane 10 Polybutadiene 18 20 22 24 26 28 30 Elution Volume 5m counts THF Solven
93. r that can provide 20 to 30 mW at 685 nm and another which provides 100 to 150 mW at 800 nm The scattered light is collected at a given angle and orientation e g 15 or 90 from the incident radiation and is used to deduce the desired molecular properties Agilent MDS User Manual Appendix 1 Theory of Operation 11 Static Light Scattering Measuring the Molecular Weight Agilent Technologies systems include polarized laser light sources the equations presented in this chapter will be slightly different than those presented in discussions of light scattering when non polarized sources are used The electric dipole moment that is induced is shown in equation 1 gt gt p Q amp E where p is the dipole moment a is the polarizability E is the electric field The polarizability can be related to measurable parameters via equation 2 2 dnl dc A M 2 m N where My is the molecular weight N is Avogadro s number 6 02 1022 molecules per mol A dn is the change in the index of refraction as a function of the change in concentration It is considered to be a constant for any specified solvent solute pair under constant operating conditions Agilent MDS User Manual 173 11 Appendix 1 Theory of Operation The oscillating dipole will radiate light in all directions at the oscillating frequency This is the origin of scattered light If a single molecule has dimensions that are small with respect
94. r Manual 135 8 Error Information Leak Detected in Upper Enclosure Error ID SYSTEM 1050 A leak was detected inside the system in the upper enclosure Probable cause Suggested actions 1 Loose connection at upper detector ports Ensure all fittings are tight Probable cause Suggested actions 1 Blocked detector inlet causing leak at Check flow path is clear of obstruction capillary fittings Leak Detected in Bottom Enclosure Error ID SYSTEM 1060 A leak was detected inside the system in the lower enclosure Probable cause Suggested actions 1 Loose connection at upper detector ports Ensure all fittings are tight 2 Blocked detector inlet causing leak at Check flow path is clear of obstruction capillary fittings 136 Agilent MDS User Manual Rear Fan Failed in Control Unit Error ID SYSTEM 1100 Error Information 8 Thermal shut down of the cooling fan at rear of control unit Probable cause 1 Fan cable disconnected 2 Defective fan 3 Obstruction in fan 4 Defective main board in control unit Fan Failed in Upper Enclosure Error ID SYSTEM 1110 Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative Thermal shut down of the cooling fan at rear of upper enclosure Probable cause 1 Fan cable disconnected 2 Defective fan
95. r cable connected Do not operate the instrument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or make any unauthorized modification to the instrument Capacitors inside the instrument may still be charged even though the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious personal injury are present in this instrument Use extreme caution when handling testing and adjusting When working with solvents observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used 184 Agilent MDS User Manual Appendix 2 General Safety Information 12 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 equipm
96. r site and initiate appropriate actions Delivery Checklist 38 Unpack the 1260 Infinity MDS and accessories and ensure that all parts and materials shown in the table below have been delivered with your module Report any missing or damaged parts to your local Agilent Technologies sales and service office The system and detector s are supplied separately in their own packaging Agilent MDS User Manual Delivery Checklist 1260 Infinity GPC SEC MDS p n G7800A G7800 68000 G7800 63000 G7800 68001 G7800 68002 Description 1260 Infinity MDS Dual OR Quad Compartment Power cord Agilent 1260 Infinity MDS Installation Kit Drawer Unit OPTIONAL 1260 Infinity GPC SEC MDS 1200 Accessory Kit OPTIONAL Universal Accessory Kit OPTIONAL Optional Detectors p n G7801A G7802A G7803A Agilent MDS User Manual Description Agilent 1260 Infinity GPC SEC MDS RI Detector Agilent 1260 Infinity GPC SEC MDS Viscometer Agilent 1260 Infinity GPC SEC GPC MDS Dual Angle LSD Installation 3 39 3 Installation Delivery Checklist 1260 Infinity Bio SEC MDS p n Description G7805A 1260 Infinity Bio SEC MDS Dual Compartment Power cord G7800 68000 Agilent 1260 Infinity MDS Installation Kit G7800 63000 Drawer Unit OPTIONAL G7800 68001 1260 Infinity GPC SEC MDS 1200 Accessory Kit OPTIONAL G7800 68002 Universal Accessory Kit OPTIONAL Optional Detectors p n Description G7808A Agilent 1260 Infinity Bio SEC L
97. re of Acetone Water 50 50 at 1 mL min for 15 min 2 Flush out all 1260 Infinity Multi Detector Suite detector lines 3 Flush the reference side of the RI cell and the viscometer transducers thoroughly by using the purge actions 4 Power the MDS off 156 Remove the tubing lines to MDS detector s installed and insert a blank plug into the inlet and outlet ports and the purge port if an RI detector is installed Label the instrument with a tag describing the storage solvent Agilent MDS User Manual 7 Agilent MDS User Manual r a ee 10 7 e Parts and Materials for Maintenance amp e Parts and Materials for Maintenance 158 This chapter provides information on parts for maintenance a Agilent Technologies 157 10 Parts and Materials for Maintenance Parts and Materials for Maintenance 158 p n G7801A G7802A G7803A G7808A G7809A G7800 68000 G7800 64003 G7800 68001 G7800 63001 G7800 87000 G7800 87001 G7800 63002 G7800 63003 G7809 68000 5062 2463 5022 2184 PL1 24950 PL1 28327 PLO100 3601 PLO100 3602 Description Agilent 1260 Infinity GPC SEC MDS RI Detector Agilent 1260 Infinity GPC SEC MDS Viscometer Agilent 1260 Infinity GPC SEC GPC MDS Dual Angle LSD Agilent 1260 Infinity Bio SEC LSD Agilent 1260 Infinity Bio SEC LS DLS Agilent 1260 Infinity MDS Installation Kit 1260 Infinity GPC SEC MDS Enclosure Expansion 1260 Infinity GPC SEC MDS 1200 Accessory Kit Agilent
98. roduction e specifications e installation controlling and operating e optimization e troubleshooting and diagnostic error information e maintenance e parts information hardware information Agilent Technologies 2014 Printed in Germany 01 2014 G7800 90390 EE Agilent Technologies
99. s 1 RI Detector not connected to main board in Please contact your Agilent service control unit representative 2 Defective RI Detector Please contact your Agilent service representative 3 Defective main board in control unit Please contact your Agilent service representative Communication to VS Detector Failed Error ID SYSTEM 1240 Communication between Viscometer and Control unit has failed Probable cause Suggested actions 1 Viscometer not connected to main boardin Please contact your Agilent service control unit representative 2 Defective Viscometer Please contact your Agilent service representative 3 Defective main board in control unit Please contact your Agilent service representative Agilent MDS User Manual 139 140 Error Information Communication to ADC Failed Error ID SYSTEM 1250 Communication between ADC and main processor has failed Probable cause 1 Main control firmware corrupt 2 Defective main board in control unit Communication to LS Detector Failed Error ID SYSTEM 1260 Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Communication between LS or LS DLS Detector and Control unit has failed Probable cause 1 LS Detector not connected to main board in control unit 2 Defective LS Detector 3 Defective main board in control unit Communication to Control Unit Failed Error ID SYSTEM 1280 S
100. s close to operating conditions and minimize stabilization time 118 Agilent MDS User Manual Agilent MDS User Manual 7 Troubleshooting and Diagnostics 120 Troubleshooting an LC System 122 Excessive baseline noise Troubleshooting 121 System Problems 122 123 123 124 Excessive baseline noise Excessive baseline drift Long retention times RI Detector Problems 124 124 125 Excessive baseline drift Flat baseline with no noise 125 125 Unable to autozero detector Low sensitivity Mirrored peaks 126 127 DP IP excessive baseline noise Viscometer Detector Problems 127 DP IP excessive baseline drift 127 Low sensitivity 128 Excessive DP Offset High IP Output 128 Low IP Output 128 Light Scattering Detector Problems 129 128 129 Excessive baseline noise 130 130 High baseline offset No signal outputs This chapter gives an overview about the troubleshooting and diagnostic features Apg Agilent Technologies 119 7 Troubleshooting and Diagnostics Troubleshooting If a problem is encountered Agilent Technologies advises that the troubleshooting section should be followed first to resolve the problem If there is an error or fault and you follow the recommended course of action and the result is not satisfactory then please direct the matter to Agilent Technologies or your local distributor Malfunctions within the MDS can arise from four general sources e the MDS itself is operating o
101. s in solution Any combination of the MDS detectors may be employed with the following combinations being the most common Agilent MDS User Manual 15 1 Introduction to the 1260 Infinity MDS G7800A Agilent 1260 Infinity GPC SEC MDS Conventional GPC The simplest offering is the MDS fitted with a refractive index RI detector This system can be used to collect conventional GPC data to allow molecular weight analysis via the use of a column calibration in the traditional GPC experiment GPC Viscometry Combining the MDS RI detector with the MDS Viscometer allows the GPC experiment to be expanded giving molecular weight information independent of the chemistry of the standards that are used to perform the calibration This approach increases the accuracy of molecular weights that are generated and allows the structure of the polymer molecules to be probed in detail GPC Light Scattering Combining the MDS RI detector with the MDS Light Scattering LS detector allows the determination of accurate molecular weights without the need for a column calibration Furthermore the size of the polymer molecules in solution can be determined by this method for high molecular weight materials Triple Detection The MDS may be configured for triple detection analysis employing the MDS RI Viscometer and LS detectors The most powerful form of the GPC experiment triple detection GPC allows accurate molecular weights to be obtained
102. s use with options of dual angle light scattering detector viscometer and dual angle light scattering with dynamic light scattering detector The key features include Ultra low dispersion Building on the Agilent 1200 Infinity Series UHPLC capabilities the 1260 Infinity MDS is minimizing dispersion in GPC SEC The light scattering flow cell has a market leading cell volume of just 10 uL The high backpressure RI cell is just 6 uL The viscometer is based on the latest advances in silica technology to create the ultimate balanced bridge Excellent baseline stability Each detector can be individually heated from 30 60 C to ensure stable baselines and excellent signal to noise performance Advanced optical design drastically reduces baseline spiking in LS traces commonly seen at low angles Adaptable and upgradable any combination of detector may be fitted within the system and the instrument may be expanded at any time allowing system capabilities to expand as budget allows The instrument offers the ability to collect digital detector outputs directly into Agilent GPC SEC software via a USB connection Output signals from external detectors can also be collected via the two independent analog input connections Agilent MDS User Manual Introduction to the 1260 Infinity MDS 1 With state of the art detector design and control interfaces built around ease of use the 1260 Infinity MDS is the solution to expanding GPC SEC bey
103. sages 146 Temperature Sensor Error 146 Unable to reach temperature set point 146 Heater Error 147 Laser Error 147 This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions 132 Agilent MDS User Manual Error Information 8 What Are Error Messages If an error occurs on the MDS it is indicated by the system alarming continuously with the display showing information about the error in the System Status Area There are two types of errors that can occur e System Errors Detector Errors For system errors the Home screen is displayed with the keypad locked The keypad cannot be unlocked manually The detector heaters are turned off and a pump stop command is sent via the auxiliary I O cable Pressing the CE key on the keypad once will stop the alarm Pressing it a second time will clear the error message If the error has not been rectified the error message will be displayed again within 5 s If the keypad has been inactive and no keys are pressed for a minute the alarm will sound again In all cases if it is not possible to resolve the error you should make a note of the error information displayed and contact your Agilent service representative for more information Agilent MDS User Manual 133 8 Error Information System Error Messages Upper Leak Sensor Failed Error ID SYSTEM 1010 The upper thermistor on the leak
104. sary to site the unit under an extraction hood or installed in a fume cupboard CAUTION Temperature stability impaired Locating the unit in a fume cupboard may compromise the temperature stability of the detector s gt Place instrument outside of fume cupboard and use an extraction hose to vent fumes to fume enclosure 32 Agilent MDS User Manual Site Requirements and Specifications 2 Physical Specifications Table 2 Physical Specifications Type Specification Comments Weight 10 kg Dual compartment Dimensions height x width x depth Line voltage Line frequency Power consumption Ambient operating temperature Ambient non operating temperature Humidity Operating altitude Non operating altitude Safety standards IEC CSA FDA 20 kg Quad Compartment 400 x 490 x 390 mm 15 8 x 19 2 x 15 4 inches 400 x 490 x 650 mm 15 8 x 19 2 x 25 6 inches 100 240 VAC 10 50 or 60 Hz 5 150 W 15 30 C 59 86 F 40 70 C 40 158 F lt 95 at 30 C 86 F Up to 2000 m 6562 ft Up to 4600 m 15091 ft Installation category Il Pollution degree 2 21CFR 1040 10 amp 1040 11 Dual compartment Quad compartment Wide ranging capability Maximum Non condensing For storing the module For indoor use only Agilent MDS User Manual 33 2 Site Requirements and Specifications Performance Specifications Table 3 Optional Refractive Index Detector
105. signal will be smoothed The signal time range and default value are shown below Range 0 1 5s Default 1s LED Gain This parameter is used to adjust the sensitivity of the RI detector in order to bring the peak response back on scale Adjustment of this parameter alters the brightness of the LED The LED gain range and default value are shown below Range 50 100 of full scale Default 100 Maxium sensitivity Signal Gain This parameter sets the factor by which the RI detector output signal is amplified The signal gain setting does not change the sensitivity of the detector but merely amplifies the captured signal by the inputted factor When setting the signal gain both the signal and noise are simply amplified by the value set so signal to noise ratios are unaffected The signal gain range and default value are shown below Range 0 1 5 0 Default 1 0 Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 Zero Offset This parameter is used to define the zero offset applied to the RI detector signal baseline after an autozero of the RI detector has been performed For example setting a zero offset value of 10 mV would mean the signal baseline is autozeroed to 10 mV The zero offset range and default value are shown below Range 500 500 mV Default 0 0 mV Sum Value This parameter is the current voltage sum value of the RI Detector in mV This is the voltage sum of the two light intensities 1
106. sily reached and unplugged gt Provide sufficient space behind the power socket of the instrument to unplug the cable Agilent MDS User Manual 29 2 Site Requirements and Specifications Power Cords Your detector is delivered with a power cord which matches the wall socket of your particular country or region The plug on the power cord which connects to the rear of the instrument is identical for all types of power cord 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 that Agilent Technologies supplies with this instrument for any other equipment 30 Agilent MDS User Manual Site Requirements and Specifications 2 Bench
107. t Figure 29 A Universal Calibration Plot Therefore for an unknown polymer sample the Universal Calibration is used to convert the intrinsic viscosity determined for each slice across the distribution from the viscometer to molecular weight Agilent MDS User Manual 165 11 Appendix 1 Theory of Operation Polymer Branching The determination of the degree of long chain branching has long occupied polymer chemists In polymer solutions the branching factor g is the starting point for many branching calculations In V 7 Where np is the intrinsic viscosity of the branched polymer and n is the intrinsic viscosity of the linear polymer of the same molecular weight is the structural model parameter which is user defined Four Capillary Viscometry Theory The MDS viscometer employs the fluid flow equivalent of the analogous Wheatstone bridge electrical circuit Solvent travels down a bridge of four capillaries of equal resistance arranged as shown in Figure 30 on page 166 IP IP Inlet pressure DP Differential pressure Specific viscosity 4DP IP 2DP From columns IV Specific viscosity Concentration In the limit as conc tends to zero Figure 30 Plumbing Diagram of the MDS Viscometer 166 Agilent MDS User Manual Appendix 1 Theory of Operation 11 The differential pressure transducer monitors the pressure drop across the bridge AP and the inlet pressure transducer measures
108. t in keypad and display status monitoring of each connected MDS detector PC control digital data acquisition into Agilent GPC SEC Software via the USB port receive and pass through a sample injection trigger for synchronized data acquisition two independent analog inputs for connecting signal outputs from external detectors eight analog outputs 1 V safety system service utility for debugging and firmware upgrading of the instrument Figure 2 MDS Control Unit Agilent MDS User Manual 13 1 introduction to the 1260 Infinity MDS MDS Detector Enclosures The 1260 Infinity MDS features two complementary detector enclosures which are designed to fix one on top of the other Each detector enclosure has two detector bays therefore for a single or dual detector system only the top enclosure is employed For a one or three detector system the remaining detector bay will be fitted with tidy draws for storing columns and other hardware Each enclosure has a door on the front that can be configured to open from the left or right Each door provides a storage area the top door for manuals and the bottom door for holding spanners Upgrading the 1260 Infinity MDS with additional detectors is simple Tidy draws are swapped out for detectors and if a triple system is required a bottom enclosure is added The inlets and outlets of each detector that is fitted are sited at the enclosure s front Connection between the
109. tamination However contamination from trapped particulates from precipitates or from thin films of residues can still occur If the instrument performance deteriorates we recommend cleaning the cell See Maintaining and Cleaning the RI Flow Cell on page 109 and Maintaining and Cleaning the LS Flow Cell on page 115 If cleaning the various detectors does not fix the problems contact your Agilent service representative Agilent MDS User Manual 105 6 Optimizing Performance Purging the Detectors 106 To ensure optimum performance of the 1260 Infinity MDS all detectors must be purged to ensure they have been fully flushed with mobile phase prior to use When flushing the detector between immiscible solvents initial flushing into an intermediate miscible solvent such as acetone or methanol is recommended before final transfer into the new solvent Purging the RI Detector The RI detector can be flushed with any miscible solvent 1 Introduce the solvent at a reduced flow of typically no higher than 0 5 mL min into the flow cell 2 Flush the sample cell for a minimum of 5 min Monitor the pressure during the flushing procedure to ensure that excessive pressure does not occur 3 Perform an RI Purge action with a 5 min purge time setting 4 Repeat step 2 and 3 if required Depending on the solvent choice some equilibration of the detector may be required This may last several hours Agilent MDS User
110. te bottle or into the internal detector within the LC assuming that you wish to use the existing detector system Data collection and analysis can be carried out using acquisition software capable of reading external analog signals and performing GPC type calculations Should you wish to use one or more existing detectors positioned within your LC system in conjunction with the MDS detector s and collect into Agilent GPC SEC Software the existing detectors will require analog output s The analog outputs from the detectors can be connected to the analog inputs on the MDS 44 Agilent MDS User Manual Installation 3 Installing the G7800 MDS WARNING eee When detectors are installed the MDS dual amp quad compartments weigh approx 20 kg 44 Ibs and 40 kg 88 Ibs respectively gt Carry the instrument with two people gt Bend your legs rather than your spine and care that your back is straight gt Ensure that the load is as close to your body as possible gt Ensure that you can handle the weight of the load CAUTION MDS drivers not installed The connection between the MDS and the PC can t be established if the MDS drivers are not installed gt Install the MDS driver before you connect the USB cable to the PC Place the module on the bench in a vertical position 2 Install the detector s into the appropriate bay 3 Install and configure the Agilent GPC SEC or Bio SEC Software on the PC
111. tector information and specific actions and parameters for the detector s connected The general structure follows Detector 1 Detector 2 Detector 3 Analog Input E a System Options gt Parameter 1 Parameter 2 Parameter N Back gt Action 1 Action 2 Action N Settings Back Figure 12 MDS Menu System Structure Agilent MDS User Manual of the Menu System is as gt Pass Number gt Service Settings 69 4 Controlling the 1260 Infinity MDS The Main Menu screen The Main Menu screen is the top level menu of the MDS Menu System from this menu options for each detector and system can be accessed This screen is dynamic and only shows options for the MDS detectors that are present in the detector compartments ee RI DETECTOR LS DETECTOR VS DETECTOR ANALOG INPUT Press SELECT or the ENTER key to access the RI DETECTOR menu SYSTEM OPTIONS BACK ace ea NOT READY Figure 13 The MDS Menu System The Main Menu screen consists of an Options menu an Options Information Area and a System Status Area lt Option Menu gt lt Option Information Area gt lt System Status Area gt a Figure 14 Layout of the MDS Main Menu Screen 70 Agilent MDS User Manual Controlling the 1260 Infinity MDS 4 The Options menu lists the detector and system menus available for your MDS The full list of menu options is shown below e RI
112. this source gt Do not look into the beam Eye damage by laser light Hazardous laser light can injure eyes gt Do not remove covers and interlocks gt Observe and note the laser warning signs carefully 152 Agilent MDS User Manual Maintenance 9 Electrical shock Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened gt Do not remove the cover of the module gt Only certified persons are authorized to carry out repairs inside the module Personal injury or damage to the product Agilent is not responsible for any damages caused in whole or in part by improper use of the products unauthorized alterations adjustments or modifications to the products failure to comply with procedures in Agilent product user guides or use of the products in violation of applicable laws rules or regulations gt Use your Agilent products only in the manner described in the Agilent product user guides CAUTION Safety standards for external equipment gt If you connect external equipment to the instrument make sure that you only use accessory units tested and approved according to the safety standards appropriate for the type of external equipment Agilent MDS User Manual 153 9 Maintenance Cleaning the Module The exterior of the instrument should be cleaned by wiping down with a soft cloth moistened with dilute detergent solution followed by wiping
113. thoroughly and repeat autozero 2 Zero glass assembly not connected to RI Please contact your Agilent service main board representative 3 Defective zero glass assembly Please contact your Agilent service representative 142 Agilent MDS User Manual Error Information 8 Viscometer Specific Error Messages Temperature Sensor Error Error ID VS 4110 Temperature sensor reading outside normal limits Probable cause Suggested actions 1 Defective temperature sensor Please contact your Agilent service representative 2 Defective main board in viscometer Please contact your Agilent service representative Unable to reach temperature set point Error ID VS 4120 The heater has timed out and is unable to reach set temperature Probable cause Suggested actions 1 Defective heater Please contact your Agilent service representative 2 Defective main board in viscometer Please contact your Agilent service representative Agilent MDS User Manual 143 Error Information Heater Error Error ID VS 4130 Heater has failed Probable cause 1 Defective heater 2 Defective main board in viscometer IP Purge Valve Error Error ID VS 4310 Purge valve failed to operate Probable cause 1 Purge valve is defective 2 Purge valve assembly not connected to viscometer main board 3 Defective main board in viscometer Suggested actions Please contact your Agilent service representative Please contact your Agilent service
114. to Determine Rh Rh the hydrodynamic radius of the compound of interest can be determined using the Stokes Einstein equation equation 11 11 ae ee 6 2 v D where k is Boltzman s constant T is the temperature of the eluent v is the viscosity of the sample D is the Diffusion coefficient calculated from the autocorrelation function Agilent MDS User Manual a Agilent MDS User Manual a ee 12 7 e Appendix 2 General Safety Information amp e General Safety Information Safety Symbols 182 General Safety Information Safety Standards 183 Operation 183 182 183 The Waste Electrical and Electronic Equipment Directive 185 Radio Interference 186 Agilent Technologies on Internet 187 This chapter provides additional information on safety legal and web a Agilent Technologies 181 12 Appendix 2 General Safety Information General Safety Information Safety Symbols Table 14 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to AN the instruction manual in order to protect risk of harm to the operator and to protect the apparatus against damage Indicates dangerous voltages Indicates a protected ground terminal The apparatus is marked with this symbol when hot surfaces are available A and the user should not touch it when heated up External Laser warning label located on rear of LS and DLS detector Internal Laser
115. to noise and low levels of drift and is fitted with a low dispersion cell to maintain peak shapes throughout the sample injection The heated cell environment means that excellent temperature stability is maintained giving ultra stable baselines Measurement Principle and Light Path A light beam emitted from an LED crosses the sample and the reference cell of the RI detector twice When both cells contain pure solvent the system is calibrated to zero by means of a parallel zero plate that positions the beam on the two detector diodes 1 and 2 in such a manner that the measured light intensities 1 and I gt of the two diodes are virtually identical When the sample cell contains a solution with a different refractive index to that of the solvent the light beam is geometrically proportionally deflected depending on the relative change of the refractive index according to Snell s refraction law Agilent MDS User Manual Appendix 1 Theory of Operation 11 Light source LED Concave mirror Measurement cell Zeroplate Figure 27 Optical Diagram of the Refractive Index Detector This results in a change of the light intensities I and I gt proportional to concentration and refractive index of the sample solution From these intensity changes the signal value is calculated and indicated on the output display The built in measurement cell of the RI detector operates with a measuring angle of 45 Measurements ar
116. to the wavelength of the incident light the intensity of the light can be defined by equation 3 2 3 _ a a My sin dn dey 1 5 2 4 2 N ASR where I is the intensity of the radiated light S I is the intensity of the incident light 0 is the wavelength of light in a vacuum 0 D as defined in Figure 34 on page 172 and R Radius of molecule in solution If we collect light from a volume V of a solution with a concentration c gm mL the intensity of scattered light can be found by multiplying equation 3 by the number of molecules in the volume V The number of molecules can be expressed by ee My Now if we solve for Mw we obtain equation 4 M IN AR r 7 4 2 M sin c dn dc lIV 174 Agilent MDS User Manual Appendix 1 Theory of Operation 11 Collecting all the constants and instrumental parameters into an overall instrumental constant A we obtain equation 5 Vs i M A c dni dc I WwW Equation 5 can be used to measure the molecular weight Mw of small molecules at any scattering angle O It should be noted however that larger molecules scatter less light at high values of than at low angles because of interference effects caused by the fact that light scattered from one part of the molecule travels a different distance from another part of the molecule and is not in phase with light scattered This phenomenon can be quantified by defining the light scattering form
117. tory according to these instructions before the system can be installed If you have misplaced your copy you can obtain a replacement from your local Agilent office Alternatively download a PDF from the Agilent web site www Agilent com chem 28 Agilent MDS User Manual Site Requirements and Specifications 2 Site Requirements A suitable environment is important to ensure optimal performance of the instrument please refer to the Site Preparation Checklist for more details Laser Safety When the Agilent LSD or LS DLS detector is installed the 1260 Infinity MDS is classified as a Laser Class 1 product EC825 1 CFR1040 10 amp 1040 11 During normal operation of the Agilent 1260 Infinity MDS no laser light is accessible to the user Eye damage by laser light Hazardous laser light can injure eyes gt Do not remove covers and interlocks gt Observe and note the laser warning signs carefully Power Considerations Check the operating voltage of your instrument on the IEC inlet fuse holder on rear of unit 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 from the power line at any time gt Make sure the power connector of the instrument can be ea
118. tream such as that found in gel permeation chromatography GPC In flowing streams measurements are made on each elution slice using a unique light scattering design and very fast digital signal processors Agilent MDS User Manual 171 11 Appendix 1 Theory of Operation 172 The Physical Basis Of Light Scattering Light consists of perpendicular electric and magnetic fields that oscillate in a direction that is perpendicular to the direction of propagation of the light as shown in Figure 34 on page 172 When light strikes a molecule the electrons will experience a force due to the electric field and will move slightly This movement will induce an oscillating dipole moment that will radiate light in all directions at the oscillating frequency This radiated light is the scattered light that is detected and processed as described below scattered light incident light Y Molecule Figure 34 Light Scattered by a Molecule Figure 34 on page 172 describes the spatial arrangement of the incident light and scattered light in the light scattering experiment The light is polarized in the vertical direction thus the electric field will oscillate in the Z direction and the magnetic field will oscillate in the X direction A diode laser which is a monochromatic source of light that can be focused to a very small point in the centre of the sample cell is used in the light scattering system Typical sources include a semiconductor lase
119. uggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative Communication in Control unit has failed Probable cause 1 Main control firmware corrupt 2 Defective main board in control unit Suggested actions Restart the instrument Please contact your Agilent service representative Agilent MDS User Manual Error Information 8 RI Detector Specific Error Messages Heated Block exceeded lower limit Error ID RI 3110 The sample cell block thermistor is reading too low Probable cause Suggested actions 1 Defective RI block assembly Please contact your Agilent service representative Heated Block exceeded upper limit Error ID RI 3120 The sample cell block thermistor reading too high Probable cause Suggested actions 1 Defective RI block assembly Please contact your Agilent service representative LED Light Source Error Error ID RI 3210 The LED light source has failed Probable cause Suggested actions 1 LED Light source not connected to the RI Please contact your Agilent service main board representative 2 Defective LED Light source Please contact your Agilent service representative Agilent MDS User Manual 141 8 Error Information Autozero Error Error ID RI 3410 The autozero action has timed out Probable cause Suggested actions 1 Detector at false zero Purge RI detector
120. ut maintenance inside the unit There are no user serviceable parts inside the instrument Unauthorized access to the instrument will invalidate the instrument warranty 150 Agilent MDS User Manual Maintenance 9 Information for Service Personnel Please note that this instrument is double fused The following fuses are fitted e 2x 250 H 2 A T 20x5 mm WARNING Fire and damage to the module Wrong fuses gt Make sure that only fuses with the required rated current and of the specified type super fast fast time delay etc are used for replacement gt The use of repaired fuses and the short circuiting of fuse holders must be avoided Agilent MDS User Manual 151 9 Maintenance Warnings and Cautions Toxic flammable and hazardous solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks gt When working with these substances observe appropriate safety procedures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice gt The volume of substances should be reduced to the minimum required for the analysis gt Do not operate the instrument in an explosive atmosphere Eye Discomfort The light source in the RI detector is a class 1 LED product Temporary discomfort may result from directly viewing the light produced by
121. utside specification e the MDS detector s installed can be dirty or operating outside specification e the LC system can have a broken dirty or non optimally operating component but the problem is manifesting itself in the MDS detector s installed e a mobile phase and or column problem which by its very nature is spread throughout the LC system but appears as a malfunction of the MDS detector s installed To troubleshoot the MDS detector s installed you must be able to separate the MDS detector s performance within the LC system from its performance outside the LC system This section begins with guidelines for testing the MDS including the installed detector s as a stand alone Section System Problems on page 122 lists the observed problems with the detectors along with possible causes and the suggested solutions 120 Agilent MDS User Manual Troubleshooting and Diagnostics 7 Troubleshooting an LC System Standard practice is to add one component at a time back into the LC system so that the component causing the problem is easily identified if when the condition reoccurs Begin troubleshooting by adding the pump to the MDS first and finish by adding the column last If the MDS has more than one detector installed or there is another type of detector available use them to aid in troubleshooting For example if the MDS has a MDS RI and a MDS LS detector installed and only the MDS RI Detector has a noisy baseli
122. warning label located on inner box of LS and DLS detector WARNING haat alerts you to situations that could cause physical injury or death gt Do not proceed beyond a warning until you have fully understood and met the indicated conditions CAUTION A CAUTION alerts you to situations that could cause loss of data or damage of equipment gt Do not proceed beyond a caution until you have fully understood and met the indicated conditions 182 Agilent MDS User Manual Appendix 2 General Safety Information 12 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 Safety Standards This is a Safety Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards Operation Before applying power comply with the installation se
123. without the need for a column calibration and gives detailed information about the structure and solution behavior of the polymer molecules 16 Agilent MDS User Manual Introduction to the 1260 Infinity MDS 1 G7805A Agilent 1260 Infinity Bio SEC MDS For the 1260 Infinity Bio SEC MDS Agilent Technologies uses highest quality materials in the flow path also referred to as wetted parts which are widely accepted by life scientists as they are known for optimum inertness to biological samples Explicitly the complete flow path is free of stainless steel and other alloys containing metals such as iron nickel cobalt chromium molybdenum or copper which can interfere with biological samples The G7805A detector options require a concentration detector such as the 1260 Infinity Bio inert DAD SEC Dual Angle Light Scattering Combining the MDS Light Scattering LS detector with a concentration detector allows the determination of accurate molecular weights without the need for a column calibration Furthermore this technique is excellent for the detection of aggregates SEC Dynamic Light Scattering Complementing the MDS Light Scattering LS detector DLS provides hydrodynamic size information for biomolecules Agilent MDS User Manual 17 1 18 Introduction to the 1260 Infinity MDS Data Collection and Analysis The 1260 Infinity MDS provides on board digital data acquisition allowing data to be collected from the
124. y Hold Up Columns 113 Optimizing Light Scattering Performance 115 Maintaining and Cleaning the LS Flow Cell 115 Aqueous Eluents 115 Shutting down the Instrument 118 This chapter gives hints on how to optimize the performance or use additional devices oh Agilent Technologies 103 6 Optimizing Performance Location of the 1260 Infinity MDS Place the detector conveniently near your HPLC system The modular design of the MDS 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 detector inlet should be kept to a minimum 104 Agilent MDS User Manual Optimizing Performance 6 Routine Maintenance of the MDS System A contaminated MDS can lead to noise and drift problems that are often mistakenly attributed to other areas of the system Many cases of performance degradation in sensitive instruments with flow through cells are traceable to cell contamination The high sensitivity of the instrument makes it imperative that a high standard of solvent purity and general system cleanliness be maintained To insure this and to decrease the amount of cleaning required use e filtered solvents with solvent reservoir filters e an in line filter between the pump and detector a pre column to protect the cell from con

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