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Solvent degassing

6-7

Solvent degassing

Using degassed solvents is one of the most important steps in solvent

preparation. Degassing provides

•

stable baselines and enhanced sensitivity

•

reproducible retention times

•

stable pump or solvent delivery system operation

This section presents information on the solubility of gases, solvent degassing

methods, and solvent degassing considerations.

Solvent degassing methods

Solvent degassing helps you attain a stable baseline and also improves

reproducibility and pump performance.
Three common methods used to degas solvents are

•

sparging with helium

•

reducing pressure by vacuum

•

using sonication

These methods may be used individually or in combination.

Vacuum-ultrasound followed by sparging is the most effective technique for

most solvents.

Sparging

Sparging removes gases from solution by displacing dissolved gases in the

solvent with a less soluble gas, usually helium. Well-sparged solvent improves

pump performance. Helium sparging brings the solvent to a state of

equilibrium, which may be maintained by slow sparging or by keeping a

blanket of helium over the solvent. Blanketing inhibits reabsorption of

atmospheric gases.

Tip:

Sparging may change the composition of mixed solvents.

Vacuum degassing

The inline vacuum degasser operates on the principle of Henry’s law to

remove dissolved gases from the solvent. Henry’s law states that the mole

fraction of a gas dissolved in liquid is proportional to the partial pressure of

Содержание 2424

Страница 2: ...rs that may appear in this document This document is believed to be complete and accurate at the time of publication In no event shall Waters Corporation be liable for incidental or consequential dama...

Страница 3: ...encounter in this document or to suggest ideas for otherwise improving it Please help us better understand what you expect from our documentation so that we can continuously improve its accuracy and u...

Страница 4: ...esentative for guidance When you develop methods follow the Protocol for the Adoption of Analytical Methods in the Clinical Chemistry Laboratory American Journal of Medical Technology 44 1 pages 30 37...

Страница 5: ...rs Intended use of the 2424 ELS detector Waters designed the 2424 ELS detector to analyze and monitor many compounds Symbol Definition Confirms that a manufactured product complies with all applicable...

Страница 6: ...mal normal and above normal levels of a compound Ensure that QC sample results fall within an acceptable range and evaluate precision from day to day and run to run Data collected when QC samples are...

Страница 7: ...vii EC Authorized Representative Waters Corporation Micromass UK Ltd Floats Road Wythenshawe Manchester M23 9LZ United Kingdom Telephone 44 161 946 2400 Fax 44 161 946 2480 Contact Quality manager...

Страница 8: ...viii...

Страница 9: ...i ISM classification vi ISM Classification ISM Group 1 Class B vi EC Authorized Representative vii 1 2424 ELS Detector Optics Principles 1 1 Principles of evaporative light scattering detection 1 2 Ov...

Страница 10: ...sions 2 5 Power requirements 2 6 Gas requirements 2 7 Making the gas supply connection 2 7 Venting the exhaust hose 2 8 Connecting to the electricity source 2 11 Installing the nebulizer assembly 2 12...

Страница 11: ...ng to start a run 3 15 Primary and secondary functions 3 15 Setting up a run 3 17 Setting the nebulizer and drift tube temperature 3 18 Setting the gain and gas pressure 3 19 Setting the column heater...

Страница 12: ...method 3 39 Viewing events within a method 3 39 Resetting a method 3 39 Clearing events 3 40 Conserving lamp life 3 41 Changing chromatographic conditions 3 43 Shutting down the detector 3 44 Periodi...

Страница 13: ...eypad diagnostic functions 5 8 Gas and temperature control diagnostic functions 5 10 Sample and reference energy diagnostic function 5 12 Generate Test Peaks diagnostic function 5 13 General troublesh...

Страница 14: ...Drift tube temperature 6 10 Selecting the optimum temperature 6 10 A Safety Advisories A 1 Warning symbols A 2 Task specific hazard warnings A 2 Specific warnings A 3 Caution symbol A 5 Warnings that...

Страница 15: ...he 2424 ELS detector effectively you must understand the principles that underlie operation of the detector s optics and electronics Contents Topic Page Principles of evaporative light scattering dete...

Страница 16: ...molecules natural product extracts and libraries food products and related materials For detecting compounds that exhibit little to no UV Vis response and do not ionize well for mass spectrometry the...

Страница 17: ...heat to evaporate the solvent Conversely low gas flow produces large droplets requiring more heat to evaporate the solvent Desolvation In the desolvation region the mobile phase evaporates leaving dri...

Страница 18: ...sizes exhibit different angular distributions of the scattered light and particles whose sizes and shapes vary have different light scattering cross sections In general larger particles scatter more...

Страница 19: ...ng type depends on the size of the particles going through the light beam The ratio of particle diameter D to the incident wavelength or defines the type of scattering that results Rayleigh scattering...

Страница 20: ...cks linearity over wide concentration ranges When you use the detector for assays you may need to experiment with a variety of best fits using linear quadratic and log log responses for the compounds...

Страница 21: ...Detector description The detection of a sample peak occurs as follows 1 Eluent from the column flows into the nebulizer where a steady supply of gas converts it into a fine aerosol Carefully controll...

Страница 22: ...g gaseous effluent is vented Signal processing and noise calculations Power source fluctuations can introduce noise in the detector output and be a major source of noise at high signal levels To offse...

Страница 23: ...oard It also interfaces between the Preamplifier board and the CPU board CPU board Contains the microprocessor serial RS232 and Ethernet communications battery backed nonvolatile RAM in which the user...

Страница 24: ...can interact The chamber contains these components Two light traps Reference photodiode To prevent the solvent and analyte from condensing on the chamber walls or optical surfaces the chamber is heat...

Страница 25: ...tile samples Drift Tube You can set the drift tube heater up to 100 C to evaporate any residual solvent RTD resistance temperature detector sensors provide temperature feedback to the heater control t...

Страница 26: ...s response varies with energy throughput If the lamp energy is degraded peak response degrades accordingly If lamp intensity diminishes peak response decreases and noise increases During normal operat...

Страница 27: ...Contemporary Instrumental Analysis Simon Schuster Prentice Hall Inc New Jersey 2000 G D Christian Analytical Chemistry Sixth Edition John Wiley Sons Inc New York 2003 TP02730 EXHAUST 15cm 6 inch CLEAR...

Страница 28: ...hromatography Edited by E Yeung J Wiley Sons New York 1986 B A Bidlingmeyer Practical HPLC Methodology and Applications Wiley Sons NY 1992 U Neue HPLC Columns Theory Technology and Practice Wiley VCH...

Страница 29: ...Guiochon Use of light scattering as a detector principle in liquid chromatography J Chromatogr 265 1 1983 G Guiochon A Moysan and C Holley Influence of various parameters on the response factors of t...

Страница 30: ...1 16 2424 ELS Detector Optics Principles...

Страница 31: ...y 2 3 Making the gas supply connection 2 7 Venting the exhaust hose 2 8 Connecting to the electricity source 2 11 Installing the nebulizer assembly 2 12 Connecting the siphon drain tubing 2 14 Connect...

Страница 32: ...ate laboratory instruments and computer controlled devices and also how to handle solvents Make Signal Connections to Start installation procedure Installation complete Select appropriate site Unpack...

Страница 33: ...the shipping cartons for future transport or shipment If you discover any damage or discrepancy when you inspect the contents of the cartons immediately contact the shipping agent and your local Wate...

Страница 34: ...ector the amount of weight stacked on top of it should not exceed 18 kg 40 pounds Installation site requirements Parameter Requirement Operating temperature range 4 to 30 C 39 2 to 86 F avoid direct e...

Страница 35: ...nnections are located Gas supply 450 to 690 kPa 4 5 to 6 9 bar 65 to 100 psi at the regulator of dry oil free filtered nitrogen or zero grade oil free filtered air Ventilation Locate near fume hood or...

Страница 36: ...s distributor Power off and unplug the detector before performing any maintenance on the instrument Connect all components of the HPLC system to a common ground Warning For continued protection agains...

Страница 37: ...the gas supply connection 1 Cut the 6 mm tubing squarely that is perpendicular to the tubing s horizontal axis Warning Do not use gases that are not inert In particular avoid those that would allow th...

Страница 38: ...vided in the startup kit If you are using the system with an external filter first connect the gas source to the filter and then connect the filter to the back of the unit Venting the exhaust hose To...

Страница 39: ...se to an evacuation source but do not apply a vacuum Caution Failure to use the vapor trap could result in too strong a vacuum which could adversely affect the vapor flow through the drift tube This c...

Страница 40: ...ings on the vapor trap bottle Vapor trap bottle and exhaust hose Warning Inhalation risk Do not allow detector exhaust to enter the laboratory atmosphere Caution To avoid excessive electronic noise do...

Страница 41: ...2 kPa 0 bar 0 03 psi between the detector and the laboratory exhaust system Exhaust system flow example Connecting to the electricity source The 2424 ELS detector requires a separate grounded electri...

Страница 42: ...ord to a suitable wall outlet 4 Do not turn the detector on at this time Installing the nebulizer assembly Waters offers two nebulizers for the 2424 ELS detector a low flow for flow rates from 50 to 5...

Страница 43: ...the nebulization chamber The quick disconnect tubing fitting will be at the twelve o clock position Installing the nebulizer 6 Push the nebulizer into the nebulization chamber and turn it clockwise u...

Страница 44: ...ase Omitting this step delays satisfactory detector performance Routing the siphon drain tubing down the front of the detector Required materials Front siphon drain tubing in startup kit Hose clamp to...

Страница 45: ...the end of the tubing is not immersed in the collected liquid Routing the siphon drain tubing to the rear of the detector Tip The rear siphon drain tubing is intended for use with the optional Waters...

Страница 46: ...he hole in the siphon drain tubing bracket and align the screw and bracket with the hole that you removed the cover screw from 3 Using a Phillips screwdriver secure the bracket to the front left side...

Страница 47: ...6 Route the other end of the rear siphon drain tubing through the opening in the rear left corner of the detector tray 7 Attach the convoluted tubing to the rear siphon drain tubing using the plastic...

Страница 48: ...f the unit in the event of a leak Required materials Tubing not supplied Sharp knife not supplied To connect the drip tray 1 Cut a length of tubing sufficient to reach between the drip tray and the wa...

Страница 49: ...d exhausts it as gas vapor Do not allow solvent flow to continue if no gas flow is present Required materials Sample inlet tubing assembly 5 16 inch open end wrench To connect a column or second detec...

Страница 50: ...king signal connections Tip Connect the detector to other HPLC system components through an Ethernet connection The figure on page 2 6 shows the rear panel locations of the connectors used to operate...

Страница 51: ...or or chart recorder Yes Yes Install Ethernet cable No Connect to Ethernet bus Start signal connection Signal connection complete Install event and I O cable s No Connect event inputs or outputs Insta...

Страница 52: ...Ethernet cable This cable is contained in the startup kit Single Waters instrument connection Multiple Waters instrument connections In a system configuration with many Waters Ethernet instruments an...

Страница 53: ...se a network switch for multiple Ethernet instruments Use of a network hub in place of a network switch is not supported Multiple Waters Ethernet instrument connections Connecting to a Waters MassLynx...

Страница 54: ...ent system configurations Tip For pinout connections to the detector see page 2 26 Detector inject start connections Inject start output source Inject start input connection on the 2424 ELS detector c...

Страница 55: ...the detector to other instruments use the two analog out event in I O connectors and their corresponding pin outs on the rear panel This section describes signal connections between the detector s re...

Страница 56: ...time clock to start Lamp on Enables and disables the lamp When the input is active the lamp is on Chart mark in Adds a chart mark at 10 of full scale to either or both analog output channels Signal Ou...

Страница 57: ...e column heater temperature or gas pressure and is programmable Output voltage range 0 1 to 2 1 VDC fixed maximum data rate is 10 Hz Stop flow Stops the flow to the chromatographic system when a low i...

Страница 58: ...shown in the following table and figure Warning Fire and explosion hazard Failure to connect the stop flow output could cause the detector to flood 1 2 3 4 5 6 7 8 9 10 Inject Start In Inject Start In...

Страница 59: ...lliance separations module Alliance separations module connector B 2424 ELS detector connector I Pin 4 stop flow red Pin 6 stop flow red Pin 5 stop flow black Pin 7 stop flow black 1 2 3 4 5 6 7 8 9 1...

Страница 60: ...output connections to a chart recorder Chart recorder connectors 2424 ELS detector connector I Pen 1 Pin 1 signal out red Pen 1 Pin 2 signal out black Tip For this connection do not use the cable shie...

Страница 61: ...injector Inject start signal from a contact closure signal with each injection Auto zero signal to adjust the zero offset of the detector each time the injector makes an injection Each time the detec...

Страница 62: ...ctor Inject start connections to an injector pulse duration 0 to 10 seconds 2424 ELS detector connector II Injector connector Pin 1 inject start in red Two spade lug terminal connectors both cables ma...

Страница 63: ...Connecting the Waters column heater module The detector can control one Waters column heater module through the EXT port on the rear panel of the detector The port is a standard 9 pin D type connecto...

Страница 64: ...2 34 Setting up the Detector...

Страница 65: ...igating the user interface 3 13 Preparing to start a run 3 15 Setting up a run 3 17 Configuring the detector 3 26 Operating the detector 3 30 Programming methods and events 3 34 Conserving lamp life 3...

Страница 66: ...As part of a MassLynx System Use the detector configured with a MassLynx system To configure the detector with a MassLynx system follow the instructions in the MassLynx documentation to set the param...

Страница 67: ...ts are coded for use only by Waters Service Engineers for troubleshooting When initialization is complete the detector displays the Home screen see page 3 7 and page 3 13 Detector Home screen Tip For...

Страница 68: ...ge 5 14 for hardware related causes of confidence tests failure during startup and their corrective actions Using the display The detector employs a 128 64 bitmap graphic display and a 24 key membrane...

Страница 69: ...following table Detector Home and Message screen icons Icon or field Icon field name Function Gain Selects the gain setting Regular field PSI Gas pressure Displays the current gas pressure and allows...

Страница 70: ...asterisk which indicates current conditions are not stored as a method Remote control Indicates that the detector is controlled by a data system and displays a remote control icon 0 00 Run time Displ...

Страница 71: ...Configure DIAG Diagnostics and TRACE Primary function keys Chart Mark Auto Zero Run Stop and Next Primary function keys take effect immediately with no further entry required Secondary function keys R...

Страница 72: ...sired item then press Enter For the number 10 select 0 and then press Enter To go to the end of a choice list press For entries numbered 11 or 12 press the or key to scroll to the desired item on the...

Страница 73: ...p Starts or stops pauses the run clock The elapsed time appears near the lower right hand corner of the Home screen Reset Resets the detector run clock to zero minutes and returns the detector to init...

Страница 74: ...Displays the list of options for creating and clearing timed and threshold events and storing retrieving and resetting methods DIAG Displays the list of diagnostic routines CONFIG Displays the first C...

Страница 75: ...te of the lamp is indicated by an icon on the Home screen 4 See 0 9 above System Info Displays system information including software version checksum and instrument serial number 5 See 0 9 above Lock...

Страница 76: ...ctive field CE Clears an editing change and returns the contents of a field to its previous value Sets the value to a unique word for some fields For example in the voltage offset diagnostic you may e...

Страница 77: ...through the list and then press Enter Tips If you know the number corresponding to the desired choice you can press that number without pressing Enter first The and keys do not increase or decrease nu...

Страница 78: ...3 of 5 4 of 5 and 5 of 5 Secondary functions of the Home screen Auto zero on inject and gain enable keypad and event in for auto zero and chart mark Light scattering Home screen Data rate and time con...

Страница 79: ...the gain factor from 1 to 1000 Each gain setting has a linear relationship with the actual light scattering signal Gas pressure Gas pressure is controlled at the nebulizer by a pressure regulator Thi...

Страница 80: ...Baseline Maintain Baseline Nebulizer heater level Heating Cool Off Heater level 0 to 100 or Cool Cool Drift tube heater set temp C Off 5 to 100 C Off Drift tube heater alarm band C 5 to 25 C 20 C Col...

Страница 81: ...o program several other parameters depending on the functions you want to perform during a run See page 3 15 for function descriptions fields screen number type of function display units allowable ran...

Страница 82: ...eheating of the sample solution to the set heater power level via a resistive heat wrap that surrounds the nebulizer tube From the Nebulizer and Drift Tube Temperature Control Home screen you control...

Страница 83: ...scale sensitivity of the detector by defining the gain factor from 1 to 1000 Each gain setting relates linearly with the actual light scattering signal The gas pressure setting monitors the condition...

Страница 84: ...Home screen appears Gain and Gas Pressure Home screen 2 Enter the gain amount in the Gain field Once you enter a gain amount the photomultiplier tube PMT is activated 3 To turn off the PMT enter 0 in...

Страница 85: ...view any changes in the current field Resetting the stop flow output switch A dedicated switch stop flow becomes active when a heater gas flow or lamp failure occurs Once the cause of the error is co...

Страница 86: ...n on a particular section of the trace To display the Scale parameters 1 Press Scale 2 Press Next to display T2 starting time The default is 0 3 Press Next again to display LSU1 starting or low light...

Страница 87: ...0 screen shown above T1 is changed to 5 T2 is changed to 0 LSU1 and LSU2 remain as auto scaled Scaled trace for 5 minutes changing T1 to 5 The following screen shows a 30 minute scaled trace similar t...

Страница 88: ...r 80 Hz To set the data rate 1 From the Home screen press Next The data rate and time constant function screen appears Data rate and time constant function screen 2 Use Enter and the numeric keypad or...

Страница 89: ...t full scale value defines the maximum output voltage value that will be used to represent the units full scale value For example using the default values the units full scale value of 2000 is represe...

Страница 90: ...he On Inject check box at the start of a run the detector either evaluates the auto zero adjustment based on no signal zero or it resets the auto zero adjustment to zero Configuring the detector Press...

Страница 91: ...to select the appropriate entry Chart mark You can specify the input to create a chart mark on signal output To determine the response of the channel use the chart mark function High Create chart mar...

Страница 92: ...configuration screen When the active state is Off the stop flow output is normally On until a stop flow error condition occurs At that point the stop flow output is changed to the Off state Requireme...

Страница 93: ...cting the type of nebulizer You use the fourth configuration screen to select the appropriate nebulizer for your flow rate range High flow 0 3 to 3 mL minute Low flow 05 to 5 mL minute Setting the dis...

Страница 94: ...ng help The detector offers limited context sensitive Help When you press press Shift HOME from a point in the program with which a Help screen is associated the screen appears If Help is unavailable...

Страница 95: ...rt of the ideal gain values appears on screen The report is based on a computation that maximizes use of one half the range of the electronics so a 2 margin accommodates any variations in signal inten...

Страница 96: ...optimization Gain optimized chromatograph Recommended method development approach You should use a method with two timed event changes to optimize this chromatogram The first gain setting change could...

Страница 97: ...ctor s Instrument Method Editor Under Empower control the method is downloaded to the detector when you make an injection or if the method is set up Once you program the method into the detector or Em...

Страница 98: ...Separations Module When the run is completed press Run Stop Reset The detector displays a recommended LSU FS value and a table of gain values Programming methods and events Overview of methods The det...

Страница 99: ...are deactivated when power is restored On startup you always see an asterisk inside the method icon on the Home screen When the detector is operating under remote control the remote icon appears Prog...

Страница 100: ...enter the time To advance to the set field Events choice list press 5 Press Enter again to display the choice list or if you know the event number press the number for the event you are programming 6...

Страница 101: ...ied threshold the switch is set as shown in the table below You can program the switch parameters listed in the table To define the pulse period or the frequency of a wave see page 3 26 To program a t...

Страница 102: ...arameter you are programming Storing a method A method consists of all programmable parameters on the Home and associated screens as well as timed and threshold events You can store the current method...

Страница 103: ...Method choice list the method number you specified appears within the method number icon Viewing events within a method To view timed and threshold events that make up a stored method 1 Retrieve the m...

Страница 104: ...s Tip To prevent losing the current conditions before you clear the method store them in one of the available storage slots When you clear the storage slots you can restore the previous conditions 4 P...

Страница 105: ...h it while allowing the detector to remain powered on You can do this in three ways Manually By programming a timed event By programming the lamp itself via the external contact closure Tip If you are...

Страница 106: ...front panel 1 Press Lamp press Shift 1 The lamp control screen displays this information The amount of time in hours and minutes the lamp has been ignited since the most recent startup The total time...

Страница 107: ...on using a timed event See page 3 27 for more information on programming the lamp through the external contact closure Changing chromatographic conditions Requirement When the detector is plumbed to t...

Страница 108: ...tes to drain the evaporation tube and detection chamber 5 Stop the gas flow 6 Power off the power to the detector Tips The last set of selected parameters is retained in memory and becomes the default...

Страница 109: ...aintenance Tip To avoid damaging the column remove it before you remove the mobile phase from the fluid path 1 Set the drift tube temperature at the appropriate desolvation temperature setting Tip 50...

Страница 110: ...3 46 Operating the Detector...

Страница 111: ...hnical service 4 2 Maintenance considerations 4 2 Replacing the lamp cartridge 4 3 Replacing the nebulizer 4 6 Cleaning the nebulizer ultrasonically 4 9 Cleaning the drift tube 4 12 Servicing the vapo...

Страница 112: ...Problem symptom s Nebulizer and drift tube temperatures Heater set points and levels Flow rate Filter setting System operating pressure Gas pressure Solvent s System configuration other components Fo...

Страница 113: ...To prevent injury always observe Good Laboratory Practices when you handle solvents change tubing or operate the system Know the physical and chemical properties of the solvents you use See the Materi...

Страница 114: ...s with the fan running and then remove the left front panel cover 3 Using a Phillips screwdriver completely loosen the two captive screws and pull the assembly out slightly to relieve stress on the la...

Страница 115: ...nplug the detector before detaching the lamp power connector from the detector Caution To avoid damaging the detector s electronics power off and unplug the detector before detaching the lamp power co...

Страница 116: ...t the power cable from the rear panel 3 Remove the left hand front panel cover Warning To avoid burn injuries do not touch the nebulizer until its temperature cools to less than 30 C as displayed on t...

Страница 117: ...zer as follows a Use a 5 16 inch wrench to loosen the compression screw that holds the inlet tubing in place b Remove the solvent inlet tubing from nebulizer 5 Push in the quick disconnect tubing fitt...

Страница 118: ...nect tubing fitting is at the twelve o clock position Then remove it from the nebulization chamber 7 Remove the packing ring from the old nebulizer and slide it onto the new nebulizer If the old packi...

Страница 119: ...Push the nebulizer into the nebulization chamber and turn it clockwise until it snaps into place 10 Insert the gas inlet tubing into the quick disconnect tubing fitting on the right side of the nebul...

Страница 120: ...n screw that holds the inlet tubing in place b Remove the solvent inlet tubing from the nebulizer Warning To avoid burn injuries do not touch the nebulizer until its temperature cools to less than 30...

Страница 121: ...n and turn the nebulizer counterclockwise so that the quick disconnect tubing fitting is at the twelve o clock position Then remove it from the nebulization chamber 7 Remove the packing ring from the...

Страница 122: ...the gas inlet tubing into the quick disconnect tubing fitting on the right side of the nebulizer and place the nebulizer in a dry beaker so that it stands up 14 Run gas at 410 kPa 4 1 bar 60 psi for 5...

Страница 123: ...semble the detector for operation 6 Reset the system to operating conditions and evaluate chromatography Servicing the vapor trap To service the vapor trap 1 Unscrew the vapor trap bottle from the cov...

Страница 124: ...ng loaded fuse holder which fits above the power entry module on the rear panel of the detector With minimum pressure withdraw the spring loaded fuse holder 3 Remove and discard the fuses 4 Make sure...

Страница 125: ...leaning the instrument s exterior 4 15 5 Reconnect the power cord to the power entry module Cleaning the instrument s exterior Use a soft cloth dampened with water to clean the outside of the detector...

Страница 126: ...4 16 Maintaining the Detector...

Страница 127: ...pparent detector problem may actually originate with the chromatography or other system instruments If you isolate a general chromatography problem see Chromatography troubleshooting on page 5 21 If y...

Страница 128: ...essage screen Errors described on this screen can be catastrophic in nature preventing further operation of the detector suspending the light scattering display and halting output The error messages c...

Страница 129: ...to the number on the detector keypad Menu items that display further choices are accompanied by Diagnostic functions Diagnostic function Description Reset flow diags Resets all diagnostic functions to...

Страница 130: ...ings You can disable all active sticky diagnostics by pressing DIAG 1 Reset Flow Diags If no sticky diagnostics are active the wrench icon does not appear in the home screen Lamp display keypad Lists...

Страница 131: ...ice personnel can access service diagnostics To exit any diagnostic when completed press DIAG to return to the diagnostics menu or HOME to return to the Home screen Running the Auto Gain diagnostic fu...

Страница 132: ...Auto Gain diagnostic press Enter Input and output diagnostic functions Use the input and output diagnostic functions for these purposes To view and reset the sample signal s auto zero value To fix es...

Страница 133: ...fixed but the values can be set independently The valid range of voltages is 2000 mV for both channels The voltage is driven on the selected channel Detector Out or Auxiliary Out Monitoring contact cl...

Страница 134: ...e lamp display and keypad diagnostic functions press DIAG 5 Change Lamp diagnostic function Use the Change Lamp diagnostic function to enter the serial number and installation date of a new lamp To us...

Страница 135: ...p use information To use the Lamp History function From the Lamp display keypad menu press 2 Lamp history The Lamp History diagnostic screen appears Lamp History diagnostic screen Test Keypad diagnost...

Страница 136: ...To use the Test Display function 1 From the Lamp display keypad menu press 4 Test display The display fills from top to bottom and right to left It then returns to the Lamp display keypad menu If the...

Страница 137: ...nostic function you can control the gas pressure regulator and gas solenoid valve independently The diagnostic screen displays the state of the gas pressure switch and the value of the pressure transd...

Страница 138: ...r 0 in the set point field Sample and reference energy diagnostic function With the sample and reference energy diagnostic function you view raw sample signal and reference energy information and you...

Страница 139: ...g This section suggests possible causes of errors and recommends troubleshooting actions Keep in mind that the source of apparent detector problems can actually be the chromatography or it can involve...

Страница 140: ...n heater module to detector Detector inoperative Fuse blown Check that the front panel display is operational if it is not check or replace the AC rear panel fuse No power at outlet Check the outlet b...

Страница 141: ...tray Properly attach and route the waste tube Keypad not functioning Keypad defective 1 Power off and then power on the detector 2 Run the keypad diagnostic see page 5 9 3 If the problem persists cal...

Страница 142: ...ilure sample ADC Lamp or PMT signal too low Weak lamp or bad alignment 1 Replace the lamp see page 5 8 2 Power the detector off and then on 3 If the problem persists call Waters Technical Service see...

Страница 143: ...leak in bench Light entering optics bench 1 Power off and then power on the detector 2 If the problem persists call Waters Technical Service see page 4 2 System not normalized Run diagnostic Memory wa...

Страница 144: ...ter failure short circuit Cable or connector short Problem with personality board 1 Power off and then power on the detector 2 If the problem persists call Waters Technical Service see page 4 2 Column...

Страница 145: ...Heater failure short circuit Cable or connector short Problem with personality board 1 Power off and then power on the detector 2 If the problem persists call Waters Technical Service see page 4 2 Dr...

Страница 146: ...d then power on the detector 2 If the problem persists call Waters Technical Service see page 4 2 Nebulizer heater temperature probe failure The heater s temperature probe is not connected or has a lo...

Страница 147: ...exhibits symptoms not addressed in one of the tables refer to General troubleshooting on page 5 13 If you need further help contact Waters Technical Service Optics heater rose above its set temperatur...

Страница 148: ...hase mixing problem causing improper evaporation Correct mobile phase composition Use high quality HPLC water and organic solvents Drift tube temperature not optimized correctly Recalculate temperatur...

Страница 149: ...aust trap Check for kinks in exhaust line or empty condensate flask Column leaking silica or packing material Replace column and flush it thoroughly before connecting it to the detector Air trapped in...

Страница 150: ...ctor is making a gurgling sound Detector exhaust too strong Move exhaust hose further away from vacuum See the figure Exhaust system flow example on page 2 11 Drift tube not heating Tube temperature n...

Страница 151: ...ix the error then restart the pump Flow interrupted or obstructed Check mobile phase level in reservoirs Check flow throughout system Make sure mobile phase inlet filter is clean Leak Check system for...

Страница 152: ...ase Peak should be seen immediately Detector output signal not zeroed Press the Auto Zero key No gain set Set gain see page 3 19 Detector exhaust too strong Move exhaust hose further away from vacuum...

Страница 153: ...phase is degrading or that the column is contaminated Change early in a series of runs and tend to become constant or fall within range after a few minutes which can indicate that the column was not...

Страница 154: ...ed retention times Air bubble in pump head Prime pump to remove bubble Malfunctioning pump check valve s Clean replace or rebuild pump check valve s Broken pump plunger Replace the plunger Reduced ret...

Страница 155: ...cy is poor throughout the chromatogram post column band broadening or loss of column efficiency can be the cause If only one peak in a chromatogram is badly shaped the peak component may be interactin...

Страница 156: ...connection between the detector and the recorder Auto zero detector baseline Check cables between unit and recorder No sample injected Check injector Leak in solvent path Check fittings and drip tray...

Страница 157: ...ults troubleshooting Symptom Possible cause Corrective action Decreased peak height Leak in injector Troubleshoot injector Degraded contaminated or improperly prepared sample Use fresh sample Column c...

Страница 158: ...too low Increase drift tube temperature see page 3 18 Drift tube temperature too high Decrease drift tube temperature see page 3 18 Nebulizer temperature too high Decrease nebulizer power level see p...

Страница 159: ...is chapter presents information on detector performance common solvent problems solvent selection degassing a solvent Warning To avoid chemical hazards always observe safe laboratory practices when ha...

Страница 160: ...atment If the sample contains any particulate matter filter it through a 0 2 m or 0 45 m filter before injection Column treatment The chromatographic column contains microparticles to separate the com...

Страница 161: ...ilter before use The total organic carbon reading should be as low as possible 5 ppb Buffer compatibility The detector cannot be used with nonvolatile solvents such as salt buffer solutions Volatile m...

Страница 162: ...solvents The following table lists the properties for some common chromatographic solvents Warning THF contaminants peroxides can explode when concentrated or evaporated to dryness Warning Do not use...

Страница 163: ...alcohol 32 4 at 20 C 82 26 12 Isopropyl myristate 1 at 20 C 192 6 164 Methanol 97 at 20 C 64 7 11 Methyl t butyl ether 240 at 20 C 55 2 28 Methyl ethyl ketone 74 at 20 C 79 64 9 Methyl isobutyl keton...

Страница 164: ...H range Boiling Point C Acids Acetic Acid 4 75 9 25 116 00 Carbonic Acid 6 37 7 63 Formic Acid 3 75 10 25 100 70 Trifuoroacetic Acid 0 30 13 70 71 80 Bases Ammonia 9 25 4 75 33 35 Ethylamine 10 81 3 1...

Страница 165: ...n These methods may be used individually or in combination Vacuum ultrasound followed by sparging is the most effective technique for most solvents Sparging Sparging removes gases from solution by dis...

Страница 166: ...o remove dissolved gas quickly consider the following Vacuum degassing The longer a solvent is exposed to the vacuum the more dissolved gases are removed Two factors affect the amount of time the solv...

Страница 167: ...ause less gas is consumed and a better sensitivity is achieved However at some point this benefit is offset by an increase in baseline noise from the inefficient nebulization of the eluent resulting i...

Страница 168: ...izer gas flow rate However the evaporator temperature must be high enough to evaporate the solvent and sufficiently dry the particle plume without adversely affecting the sample If the evaporator temp...

Страница 169: ...des also include the hazard symbols with accompanying text statements describing the hazards and telling you how to avoid them This appendix presents all the safety symbols and statements that apply t...

Страница 170: ...ks include burn injuries electric shocks ultraviolet radiation exposures and others When the following symbols appear in a manual s narratives or procedures their accompanying text identifies the spec...

Страница 171: ...ction Extinguish all nearby flames Do not use tubing that is or has been stressed or kinked Do not expose nonmetallic tubing to incompatible compounds like tetrahydrofuran THF and nitric or sulfuric a...

Страница 172: ...al surfaces of the mass spectrometer when the instrument is in Operate mode To avoid non lethal electric shock make sure the instrument is in Standby mode before touching areas marked with this high v...

Страница 173: ...When operating this device follow standard quality control procedures and the equipment guidelines in this section Warning Waters instruments can be used to analyze or process potentially hazardous s...

Страница 174: ...er Modifikationen an dem Ger t ohne die ausdr ckliche Genehmigung der f r die ordnungsgem e Funktionst chtigkeit verantwortlichen Personen kann zum Entzug der Bedienungsbefugnis des Systems f hren Avv...

Страница 175: ...e trouvant proximit de l instrument Evitez d utiliser des tubes s v rement d form s ou endommag s Evitez d utiliser des tubes non m talliques avec du t trahydrofurane THF ou de l acide sulfurique ou n...

Страница 176: ...iamenti nei tubi non metallici 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 usuari...

Страница 177: ...Warnings that apply to all Waters instruments A 9 Nonmetallic Tetrahydrofuran THF Methylene chloride Dimethyl sulfoxide THF...

Страница 178: ...tueuses Vorsicht Der Benutzer wird darauf aufmerksam gemacht dass bei unsachgem er Verwenddung des Ger tes die eingebauten Sicherheitseinrichtungen unter Umst nden nicht ordnungsgem funktionieren Atte...

Страница 179: ...l instrument Vorsicht Zum Schutz gegen Feuer die Sicherungen nur mit Sicherungen ersetzen deren Typ und Nennwert auf den Tafeln neben den Sicherungsabdeckungen des Ger ts gedruckt sind Attenzione per...

Страница 180: ...e can appear in instrument user manuals and on the instrument s front or rear panels Electrical power on Electrical power off Standby Direct current Alternating current Protective conductor terminal F...

Страница 181: ...ng symbols A 13 Handling symbols These handling symbols and their associated text can appear on labels affixed to the outer packaging of Waters instrument and component shipments Keep upright Keep dry...

Страница 182: ...A 14 Safety Advisories...

Страница 183: ...ght 14 7 kg 32 5 pounds Environmental specifications Attribute Specification Operating temperature 4 to 30 C 39 2 to 86 F Operating humidity 20 to 95 noncondensing Shipping and storage temperature 30...

Страница 184: ...outlet c Pollution Degree 2 A measure of pollution on electrical circuits which may produce a reduction of dielectric strength or surface resistivity Degree 2 refers only to normally nonconductive pol...

Страница 185: ...5 A Current carry 1 2 A Temperature control Nebulizer heater power 0 to 100 Nebulizer cooler Cooling Off Drift tube heater Ambient to 100 C 212 F a Signal and Auxiliary b Inject Start Lamp On Chart M...

Страница 186: ...B 4 Specifications...

Страница 187: ...biohazard warning A 4 burst warning A 3 C calibration photomultiplier tube 1 8 PMT 1 8 Cancel key 3 12 caution symbol A 5 CE key 3 12 changing contrast 3 11 data rate 3 13 filter time constant 3 13 sc...

Страница 188: ...sting 3 29 changing 3 11 function 3 29 key 3 11 controller board 1 9 controlling from Empower system 3 2 from MassLynx system 3 2 CPU board 1 9 current method conditions 3 13 3 34 3 40 D damage report...

Страница 189: ...6 event inputs auto zero 3 27 chart mark 3 27 configuring 3 27 default 3 28 inject start 3 27 lamp 3 28 exhaust venting requirements 2 9 external analog data collection device connecting 2 30 F failu...

Страница 190: ...7 inject start connection 2 24 generating 2 27 signal 2 24 injection trigger signals connecting 2 31 input and output connectors 2 26 installing fuses 2 6 major steps 2 2 network guidelines 2 23 proce...

Страница 191: ...maintenance considerations 4 2 mass spectrometer shock hazard A 4 MassLynx system control 3 2 maximum voltage outputs function 3 13 method active 3 39 choice list 3 10 current conditions 3 13 initial...

Страница 192: ...ed event 3 35 threshold timed event 3 35 peak identification 5 31 resolution 5 29 troubleshooting 5 30 photomultiplier tube calibration 1 8 physical specifications B 1 plus minus key 3 12 PMT calibrat...

Страница 193: ...te 3 24 drift tube temperature 3 18 filter time constant 3 24 gain 3 19 gas pressure 3 19 nebulizer temperature 3 18 pulse periods 3 28 switch output 3 25 setting up a run 3 17 shift icon 3 5 Shift ke...

Страница 194: ...s 3 34 3 41 auxiliary switch parameters 3 35 clearing 3 40 deleting 3 36 description 3 35 gas pressure parameters 3 35 lamp parameters 3 35 parameters auto zero 3 35 chart mark 3 35 programming 3 34 3...

Страница 195: ...22 V vacuum degassing 6 7 6 8 vapor trap servicing 4 13 viewing events within a method 3 39 voltage offset function 3 13 W warm up time 3 3 warning symbols A 2 A 5 Waters Technical Service contacting...

Страница 196: ...Index 10...

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