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June 11, 2015, 715004754 Rev. A

Page 34

1.3.8.2

Thermal equilibrium

Under typical operating conditions the detector reaches equilibrium within a few

hours, depending on internal temperature and column temperature.

1.3.9 Startup diagnostics tests

On startup, the 2414 RI detector runs a series of automated diagnostic tests. An error

message appears if any of the tests fail. These startup diagnostic tests include:

•

Central processing unit (CPU)

•

Serial communication interface (SCI)

•

Electrically erasable programmable read-only memory (EEProm)

•

RAM

•

Display test pattern

•

Application program checksum verification (2414 code)

•

LED verification

•

Photodiode

•

Purge valve verification

1.3.10 Bootloader program

The 2414 Bootloader program is a special type of program that resides permanently

in the CPU flash memory. It is responsible for CPU hardware initialization and

application-independent communications (such as Ethernet). It is also responsible for

starting the detector’s software.

Содержание 2414

Страница 2: ...June 11 2015 715004754 Rev A Page ii...

Страница 3: ...nnection with or arising from its use For the most recent revision of this document consult the Waters Web site waters com Trademarks Alliance Empower MassLynx THE SCIENCE OF WHAT S POSSIBLE and Water...

Страница 4: ...is used to find out the nature of the potential hazard and any actions which have to be taken Considerations specific to the 2414 Refractive Index Detector Power cord replacement hazard Waters contac...

Страница 5: ...into the drain located on the underside of the device Tubing connected to this drain directs the flow to an appropriate waste container Equipment repair or disposal Direct questions regarding repair o...

Страница 6: ...Confirms that a manufactured product complies with all applicable European Community directives or Australia EMC compliant Confirms that a manufactured product complies with all applicable United Stat...

Страница 7: ...ard curve The concentration range for standards must include the entire range of QC samples typical specimens and atypical specimens Quality control Routinely run three QC samples that represent subno...

Страница 8: ...r the internal functioning of the equipment Class B products are suitable for use in both commercial and residential locations and can be directly connected to a low voltage power supply network EC au...

Страница 9: ...nd purpose vii Intended use of the 2414 Refractive Index Detector vii Calibrating vii Quality control vii EMC considerations vii Canada spectrum management emissions notice vii ISM Classification ISM...

Страница 10: ...40 2 6 4 Connect the valve pack drip tray 41 3 Connecting Signal Cables 43 3 1 Component connection overview 43 3 1 1 Supported IEEE 488 and Ethernet configurations 44 3 2 Ethernet signal cable connec...

Страница 11: ...cs failure at startup 64 5 1 3 Using online Help 64 5 1 4 Using the keypad 64 5 1 5 Navigating the user interface 68 5 2 Operating in RIU mode 69 5 2 1 Using the display in RIU mode 69 5 2 2 Navigatin...

Страница 12: ...r Messages Diagnostic Functions and Troubleshooting 97 7 1 Error messages 97 7 1 1 Startup error messages 97 7 1 2 Operational error messages 98 7 2 Performing diagnostic functions 98 7 2 1 Accessing...

Страница 13: ...and devices 118 A 6 Warnings that address the replacing of fuses 121 A 7 Electrical and handling symbols 123 A 7 1 Electrical symbols 123 A 7 2 Handling symbols 124 B Specifications 127 B 1 Physical...

Страница 14: ...June 11 2015 715004754 Rev A Page xiv...

Страница 15: ...ulk properties of the solvent and the solutes under investigation exploiting the improbability that solvents and solutes would share an identical refractive index 1 2 Operating principles 1 2 1 Optica...

Страница 16: ...he medium also affects its RI At a fixed wavelength the relationship between the density of a medium and its RI is generally but not necessarily linear The most important of the factors that affect th...

Страница 17: ...a medium depends on these properties Angle at which the light enters the new medium the angle of incidence Refractive indices of the old and new media The angle of a refracted light beam through the...

Страница 18: ...1 n2 RI of medium 2 You can use Snell s Law to calculate the RI of a sample solution from the angle of incidence the RI of the solvent and the angle of refraction 1 2 1 3 Using changes in RI for samp...

Страница 19: ...try The 2414 RI detector can measure extremely small changes in refractive index to detect the presence of sample The small difference in RI between a reference solution and a sample solution is refer...

Страница 20: ...he reference side of the flow cell and the solution in the sample side of the flow cell Of these refractors only the solution in the sample side of the flow cell changes over the course of a run As a...

Страница 21: ...constant representing the fixed values By detecting how far the image shifts x the refractometer measures the difference in RI n between the solvent sample solution and the solvent alone The shift in...

Страница 22: ...mation 1 3 Detector description The detector is designed for high performance liquid chromatography applications It can operate as a standalone unit with an integrator or with a Waters system controll...

Страница 23: ...provides measured refractive index signals to nano RIU sensitivity Purge mode Before performing a measurement the 2414 RI detector can be programmed automatically or by using the front panel keypad t...

Страница 24: ...ecycle on keypad panel active Auto Zero on inject on keypad panel active Auto Zero delay from 0 to 30 seconds Chart mark on keypad panel active Auto Zero on keypad panel active 1 3 3 2 410 emulation m...

Страница 25: ...configuration for flow allows mobile phase to pass through the sample flow cell and then to waste or to the recycle valve During analysis the solvent sample takes this path 1 Enters through the inlet...

Страница 26: ...et tubing port 2 Passes through the sample in tube of the countercurrent heat exchanger 3 Flows through the end cap heat exchanger 4 Flows through the sample side of the flow cell 5 Flows out to the c...

Страница 27: ...ystem where you can define a duration 1 3 4 2 Recycle mode You engage the recycle mode via the detector s front panel or remote control interface like a data system or controller A programmatically co...

Страница 28: ...lines are coaxial which facilitates heat exchange between incoming and outgoing fluids 1 3 5 2 Flow cell The flow cell consists of two fused quartz hollow prisms Each cell has an inlet and outlet One...

Страница 29: ...moving through the sample and reference sides of the flow cell goes out through the pressure relief valve to the waste reservoir The figures on page 26 and page 27 indicate the flow paths during norma...

Страница 30: ...sing lens through the aperture and collimating lens to form a beam The light beam passes through the sample and reference sides of the flow cell to the mirror The light beam is reflected back through...

Страница 31: ...r dc power supply The power source for the detector the dc power supply provides voltage for the analog and digital circuitry 1 3 7 1 Filter noise The 2414 RI detector uses a Hamming filter and RC fil...

Страница 32: ...bance Figure 1 10 Filter time constant comparison 1 3 7 1 2 RC filter A finite impulse response filter which simulates a first order resistor and capacitor filter This filter is available in 410 mode...

Страница 33: ...If an event occurs to change Polarity while Polarity 2 is TRUE an appropriate error message appears For instance a front panel key press causes a warning message to appear on the front panel display a...

Страница 34: ...diagnostic tests include Central processing unit CPU Serial communication interface SCI Electrically erasable programmable read only memory EEProm RAM Display test pattern Application program checksu...

Страница 35: ...ctor ensure that the required components are present none of the shipping containers or unpacked items are damaged 2 2 Unpacking and inspecting The detector s shipping carton contains besides the dete...

Страница 36: ...ses Warranties and Support Services Note Ensure that the serial number on the detector s rear panel nameplate or inside the front left hand panel matches the number on its validation certificate 2 3 S...

Страница 37: ...re 2 1 Aligning pins with slots 3 Lower the front of the module that you are adding so that its front alignment pin rests in the front alignment slot on the previously added module 4 Repeats steps 1 a...

Страница 38: ...to a suitable wall outlet 3 Press the power switch on the front door to power on the detector Result The detector runs a series of startup diagnostic tests while the lamp LED blinks green The lamp LED...

Страница 39: ...detector to the detector This tubing assembly has been Warning To avoid the harmful effects of personal contact with solvents including inhalation always wear chemical resistant powder free gloves and...

Страница 40: ...nto the outlet fitting of the column or another detector 2 6 2 Connect to waste The detector s flow cell is extremely sensitive to backpressure Be sure to use the correct ID waste tubing supplied pre...

Страница 41: ...the tubing into the waste container 2 6 4 Connect the valve pack drip tray A factory installed drip tray lies beneath the three valves of the valve pack Be sure to direct the drip tray tube to a suit...

Страница 42: ...June 11 2015 715004754 Rev A Page 42...

Страница 43: ...or MassLynx software connected via the Ethernet network Tip The Ethernet port also supports the Waters PC based Autoloader utility for installing firmware see the Waters 2414 Refractive Index Detecto...

Страница 44: ...n operate a 2414 RI detector controlled by a data control system in one of these configurations Where all system modules including the detector communicate with the data system via an IEEE 488 bus int...

Страница 45: ...operation and for firmware upgrades via the Waters Autoloader utility see the Waters 2414 Refractive Index Detector release notes Requirements You cannot use the detector s Ethernet port while you are...

Страница 46: ...connections needed to support these configurations Figure 3 3 Alliance HPLC system with the detector under Empower software control via the IEEE 488 bus interface You use the data control software to...

Страница 47: ...om the detector s rear panel connector to the injector as shown in the table below For information on injection trigger signals from a manual injector see Connecting injection trigger signals on page...

Страница 48: ...control you can make the following signal connections using the 2414 RI detector s analog out event in connectors Autozero on inject Chart mark on inject Both chart mark and autozero on inject Inject...

Страница 49: ...dule and the 2414 RI detector 3 4 1 2 Generating a chart mark on injecting To generate a chart mark on the detector at the start of an injection from the Alliance e2695 separations module make the con...

Страница 50: ...Inject Start Pin 9 Chart Mark Pin 2 Inject Start Pin 10 Chart Mark Table 3 6 Detector connections to an Alliance e2695 separations module Alliance e2695 separations module connector B Detector connec...

Страница 51: ...2414 RI detector to chromatography data software through a two channel eSAT IN Module make the connections shown in the table and figure below Table 3 7 Analog output connections to the eSAT IN modul...

Страница 52: ...each injection Inject start signal from a contact closure signal with each injection Each time the detector receives a signal from a manual injector it performs the corresponding autozero inject star...

Страница 53: ...tors Pin 2 Autozero black Table 3 9 Chart mark connections to a manual injector Detector connector A Manual injector connector Pin 9 Chart Mark red Two spade lug terminal connectors both cables can be...

Страница 54: ...tor connector A Manual injector 1 Inject Start 2 Inject Start 3 Ground 4 Purge 5 Purge 6 Polarity 7 Polarity 8 Ground 9 Chart Mark 10 Chart Mark 11 Ground 12 Switch 13 Switch Detector connector A Manu...

Страница 55: ...thod setting When Polarity Enable is closed connected to an instrument polarity determines peak polarity Polarity open disconnected generates negative polarity Polarity closed connected generates posi...

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Страница 57: ...of mixed solvents Outgassing of dissolved gases 4 2 Selecting a solvent An ideal solvent for your analysis has these characteristics Good solubility characteristics for your application Significantly...

Страница 58: ...a high quality water purification system If the water system does not provide filtered water filter it through a 0 22 m membrane filter before use 4 2 4 Buffers When you use buffers dissolve salts fir...

Страница 59: ...Pentane 1 358 Ethyl bromide 1 424 Acetone 1 359 Methylene chloride 1 424 Ethanol 1 361 Cyclohexane 1 427 Methyl acetate 1 362 Ethylene glycol 1 427 Isopropyl ether 1 368 N N dimethyl formamide DMF 1...

Страница 60: ...ncrease in temperature but the solubility of He in benzene increases with an increase in temperature 4 3 1 3 Effects of partial pressure The mass of gas dissolved in a given volume of solvent is propo...

Страница 61: ...as the solvent passes through the vacuum chamber At higher flow rates lesser amounts of gas per unit volume of solvent are removed Surface area of the degassing membrane The length of the degassing m...

Страница 62: ...June 11 2015 715004754 Rev A Page 62...

Страница 63: ...rtup diagnostic tests If the detector passes all tests the initial home RIU or 410 mode screen appears Figure 5 1 Initial home screen RIU mode Figure 5 2 Initial home screen 410 mode Note The 2414 RI...

Страница 64: ...etector provides limited context sensitive help When you press Shift HOME from a point in the program associated with an online Help screen the Help screen appears Figure 5 3 Example of an online Help...

Страница 65: ...ing to the desired item and then press Enter For the number 10 select 0 and then press Enter To go to the end of a choice list select For entries numbered 11 or 12 scroll to the desired item on the ch...

Страница 66: ...or down toward the end Other screens can have special instructions for the use of the s and t keys for example the Display Contrast screen Next Displays a screen with additional options related to the...

Страница 67: ...0 9 above Recycle Activate the recycle or diverter valve Recycle is a toggle function The current recycle state is indicated by icon 4 See 0 9 above System Info Displays system information including s...

Страница 68: ...hen press Enter Note The s and t keys do not increment or decrement numerical field entries Instead use the numerical keypad Enters a decimal point Also positions the cursor at the last entry in a lis...

Страница 69: ...g the HOME key At the first use of the detector the home screen shows the factory set defaults After the first use the home screen shows the settings displayed before the detector was last powered off...

Страница 70: ...sterisk that indicates current conditions are not stored as a method Remote IEEE address If the detector is controlled by a data system or other control device over the IEEE 488 bus it displays a remo...

Страница 71: ...e screen press Next These are the secondary functions in RIU mode RIU FS Filter type Time constant Voltage offset RIU offset Enable disable keypad entries The settings that you specify in the secondar...

Страница 72: ...ult is 500 The RIU Full Scale setting is a parameter used to generate an analog output voltage detector output with the appropriate scaling factor The value expressed in RIU corresponds to the RI valu...

Страница 73: ...zero is requested via the front panel You can disable this parameter by pressing any numerical key to deselect this box Enable keypad chart mark Selected by default this parameter results in a chart m...

Страница 74: ...the secondary function screens 5 2 4 Programming timed events threshold events and methods Note Programmed methods are available in RIU mode only You can store and retrieve up to 10 methods The detect...

Страница 75: ...event list is sorted automatically when you press Next The 2414 RI detector allows programming of the timed events shown in the following table To program a new timed event 1 On the keypad press the...

Страница 76: ...o return to the method choice list to store the method 11 Press Reset to reset the run clock to 0 If the 2414 RI detector is configured with another external device the inject start event programmed f...

Страница 77: ...itial Threshold value as a timed event 3 Press Enter to advance to the next Switch field or press the s or t key to move among the five fields on the threshold events screen 4 When the Switch field is...

Страница 78: ...HOD Shift Temp C 2 Press 3 Retrieve a method Result The last method number stored or retrieved is displayed in the method number box 3 Enter the number of the method you want to retrieve and press Ent...

Страница 79: ...ou press Enter the following conditions occur All timed events are deleted All threshold events are disabled All other operating parameters of the method RIU FS Filter Time Constant etc are set to def...

Страница 80: ...displaying the Full Scale value used by the Waters 410 and 2410 Detectors and driving the Detector Out signal on the 2414 RI detector output To switch the detector from RIU mode to 410 mode press the...

Страница 81: ...ld Icon field name Function Home1 status Home2 entry Sensitivity Shows the current sensitivity setting Home1 status Temp C entry Detector Temperature Shows the current temperature of detector oven Num...

Страница 82: ...ctions of the 410 mode home screen From the home screen you can access the following functions either from the home screen or by pressing the Next key Sensitivity The Waters 410 compatible Integrator...

Страница 83: ...ta system The offset is added after any polarity has been applied to the output default is 0 mV Voltage offset range is 0 to 2000 mV Autozero on inject The Autozero On Inject Enable enables an autozer...

Страница 84: ...software connected to the detector via the Ethernet connector A data control system running Empower software connected to the detector via the IEEE 488 bus see Connecting to a Waters data control sys...

Страница 85: ...t run when contact closure changes from On closed to Off open Ignore Do not respond to Inject start input This is the default setting Use the Enter key and the numeric keypad or the s and t keys to se...

Страница 86: ...the recycle input to turn on diverter valve High If the contact closure is open Recycle mode is engaged If the contact closure is closed Recycle mode is disengaged Low If the contact closure is closed...

Страница 87: ...n adjust the noise level peak height peak direction and the temperatures of the internal oven and column heaters to optimize the performance of the detector 5 6 1 Attenuation and sensitivity guideline...

Страница 88: ...1 1 Temperature These screens control the internal detector oven and if configured Waters column heater module These screens are the same for RIU and 410 modes Figure 5 20 Temperature screen 1 Figure...

Страница 89: ...el is controlled by the software The signal source for the channel is user programmable When the Detector Oven Temperature channel output type is selected the channel will output a 0 to 2 V signal on...

Страница 90: ...efractive index change trace For RIU1 and RIU2 press CE to reset to auto T1 represents the left side of the trace or ending time to be displayed default is 30 T2 represents the right side of the trace...

Страница 91: ...ty water and flush the system for 10 minutes at 2 mL min 2 Replace the 100 water mobile phase with a solution of 90 methanol 10 water and flush the system for 10 minutes at 2 mL min 3 Cap the flow por...

Страница 92: ...June 11 2015 715004754 Rev A Page 92...

Страница 93: ...A contaminated fluid path can cause baseline noise drift inaccurate sample refraction and other operational problems If you suspect the detector s fluid path is contaminated follow the procedure belo...

Страница 94: ...Set the detector to purge mode for approximately 5 minutes and operate it for an additional 5 minutes in normal mode 4 Restart the pump or solvent delivery system and then set the flow rate to 5 mL mi...

Страница 95: ...e not visible In those cases you must remove the fuse and test it for electrical continuity For information on detecting the cause of a blown fuse refer to Hardware troubleshooting on page 105 To repl...

Страница 96: ...d for your requirement 6 Insert the new fuse into the fuse holder 7 Insert the fuse holder into its receptacle in the detector s rear panel and gently push on the fuse until it locks into position War...

Страница 97: ...cle power and then contact Waters Technical Service if the error persists see Accessing the diagnostic functions on page 98 Most errors in this category are encountered on startup Messages requiring y...

Страница 98: ...it any diagnostic test when it has ended press DIAG to return to the diagnostics choice list or HOME to return to the Home screen 7 2 1 Accessing the diagnostic functions You can use several diagnosti...

Страница 99: ...stic tests affects results To clear changes to the voltage output select 1 Reset diagnostics from the diagnostics choice list or cycle power to the detector The following table lists the diagnostics t...

Страница 100: ...ze LED screen 7 2 3 Using the input and output diagnostic functions Use the input and output diagnostic functions to perform these tasks Fix that is specify voltage Monitor event out switch and eight...

Страница 101: ...closure inputs A solid filled in circle indicates the contact closure is closed On High An open empty circle indicates the contact closure is open Off Low 2 For the outputs SW1 perform these steps a...

Страница 102: ...lumn Heater Displays the internal oven and if any the column heater status Simulate peak Specifies the generation of test peaks to calibrate your integrator or data system Valve Monitors the status of...

Страница 103: ...of peak repetition 3 Enter a period for repeating the peaks in seconds from 1 to 99 4 Press the Run key Result The generation of the peaks is indicated by the real time display of the change in peak...

Страница 104: ...or serial number Problem symptom s RIU FS or measurement range in RIU mode or sensitivity setting in 410 mode Internal oven temperature Flow rate Filter setting Type of column column temperature setti...

Страница 105: ...el fuse No power at outlet Confirm that the ac outlet is energized by connecting another electrical unit known to be in working order and determining whether it operates front panel display fails to i...

Страница 106: ...many possible causes of baseline noise by identifying the rate at which the baseline is changing and purging the flow cell with the proper solvent Cycling If the baseline is cycling determine the per...

Страница 107: ...e in Decontaminating the fluid path on page 93 Flow fluctuations rapid or slow drift Correct pump problems replace pump seals ensure that valves are operating properly Improper ambient environment Ver...

Страница 108: ...erm cycling Disconnect other instruments on the electrical circuit use a different wall outlet determine the suitability of the line voltage use power conditioner Radio frequency noise short or long t...

Страница 109: ...end to become constant or within range within 4 minutes which can indicate that the column was not equilibrated or that the solvent is not properly degassed Baseline noise random Flow cell can contain...

Страница 110: ...ion times Incorrect flow rate Verify flow rate Incorrect solvent composition Change solvent composition Column heater module not on Power on column heater module Column not equilibrated Equilibrate co...

Страница 111: ...dening or loss of column efficiency can be the cause If only one peak in a chromatogram is badly shaped the peak component can be interacting with the column through a chemical mechanism that does not...

Страница 112: ...Improper connection between detector and recorder Autozero detector baseline Inspect cabling between unit and recorder Solvent and sample have similar refractive indices Select a different solvent Sen...

Страница 113: ...efficiency Clean or replace column Change in mobile phase composition Correct mobile phase pH or ionic composition Incorrect flow rate Change flow rate Dirty flow cell Electronic noise Clean the fluid...

Страница 114: ...June 11 2015 715004754 Rev A Page 114...

Страница 115: ...he failure of individuals to comply with any safety precaution when installing repairing or operating any of its instruments or devices The following symbols warn of risks that can arise when you oper...

Страница 116: ...a serious health threat Warning Risk of tipping Warning Risk of explosion Warning Risk of high pressure gas release Warning To avoid injury from bursting nonmetallic tubing heed these precautions whe...

Страница 117: ...luids that you handle are infectious Specific precautions appear in the latest edition of the US National Institutes of Health NIH publication Biosafety in Microbiological and Biomedical Laboratories...

Страница 118: ...condary containment in the event of spills Requirement Use eye protection when refilling or replacing solvent bottles Requirement Wear clean chemical resistant powder free gloves when handling samples...

Страница 119: ...otection lorsque vous vous trouvez proximit de tubes en polym re pressuris s Eteignez toute flamme se trouvant proximit de l instrument Evitez d utiliser des tubes s v rement d form s ou endommag s Ev...

Страница 120: ...ici riducendo notevolmente la pressione di rottura dei tubi stessi Advertencia se recomienda precauci n cuando se trabaje con tubos de pol mero sometidos a presi n El usuario deber protegerse siempre...

Страница 121: ...inform que si le mat riel est utilis d une fa on non sp cifi e par le fabricant la protection assur e par le mat riel risque d tre d fectueuses Vorsicht Der Benutzer wird darauf aufmerksam gemacht das...

Страница 122: ...one per garantire protezione contro gli incendi so8stituire i fusibili con altri dello stesso tipo aventi le caratteristiche indicate sui pannelli adiacenti alla copertura fusibili dello strumento Adv...

Страница 123: ...incendi sostituire i fusibili con altri dello stesso tipo aventi le caratteristiche indicate nel paragrafo Sostituzione dei fusibili del capitolo Procedure di manutenzione Advertencia Para evitar ince...

Страница 124: ...ymbols and their associated statements can appear on labels affixed to the packaging in which instruments devices and component parts are shipped Functional ground Input Output Symbol Description Keep...

Страница 125: ...June 11 2015 715004754 Rev A Page 125 Lower limit of temperature Temperature limitation Symbol Description...

Страница 126: ...June 11 2015 715004754 Rev A Page 126...

Страница 127: ...le lists the environmental specifications for the 2414 RI detector Table B 1 Physical specifications Attribute Specification Width 34 3 cm 13 5 inches Height 20 8 cm 8 2 inches Depth 61 0 cm 24 0 inch...

Страница 128: ...tains to instruments that receive their electrical power from a local level such as an electrical wall outlet II Pollution degree 3 3 Pollution Degree 2 A measure of pollution on electrical circuits w...

Страница 129: ...0 H2O 3 0 10 9 RIU in 410 2410 emulation mode 1 s FTC RC filter 1 0 mL min 100 water Drift 1 2 0 10 7 RIU hr RIU FS settings RIU mode 1 0 10 6 to 5 0 10 4 RIU Sensitivity settings 410 mode 1 2 4 8 16...

Страница 130: ...June 11 2015 715004754 Rev A Page 130...

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