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WATERS CORPORATION ACQUITY Premier Overview And Maintenance Manual

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ACQUITY Premier TUV Detector
Overview and Maintenance Guide
715006903
Copyright © Waters Corporation 2021
Version 01
All rights reserved

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  • Page 1 ACQUITY Premier TUV Detector Overview and Maintenance Guide 715006903 Copyright © Waters Corporation 2021 Version 01 All rights reserved...

  • Page 2: General Information

    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 damages in connection with, or arising from, its use. For the most recent revision of this document, consult the Waters website (www.waters.com).

  • Page 3: Contacting Waters

    For other locations worldwide, phone and fax numbers appear in the Waters Local Offices information. Conventional mail Waters Corporation Global Support Services 34 Maple Street Milford, MA 01757 Safety considerations Some reagents and samples used with Waters instruments and devices can pose chemical, biological, or radiological hazards (or any combination thereof).

  • Page 4: Safety Hazard Symbol Notice

    Consult the documentation for important information about the hazard and the appropriate measures to prevent and control the hazard. Considerations specific to the ACQUITY Premier TUV detector Warning: To avoid electric shock, do not remove protective panels from the device.

  • Page 5: Applicable Symbols

    For compliance with the Waste Electrical and Electronic Equipment Directive (WEEE) 2012/19/EU, contact Waters Corporation for the correct disposal and recycling instructions For indoor use only October 21, 2021, 715006903 Ver. 01...

  • Page 6: Audience And Purpose

    This guide is intended for individuals who install, operate, or maintain the ACQUITY Premier TUV detector. It gives an overview of the technology and operation of the ACQUITY Premier TUV. To install the detector, you should generally know how to set up and operate laboratory instruments and computer-controlled devices and how to handle solvents.

  • Page 7: Quality Control

    Quality control Routinely run three QC samples that represent subnormal, normal, and above-normal levels of a compound. If sample trays are the same or very similar, vary the location of the QC samples in the trays. Ensure that QC sample results fall within an acceptable range, and evaluate precision from day to day and run to run.

  • Page 8: Table Of Contents

    Copyright notice............................ii Trademarks.............................ii Customer comments..........................ii Contacting Waters..........................iii Safety considerations..........................iii Safety hazard symbol notice......................iv Considerations specific to the ACQUITY Premier TUV detector.............iv FCC radiation emissions notice.......................iv Electrical power safety notice......................iv Equipment misuse notice........................ iv Safety advisories..........................iv Operating the device..........................iv Applicable symbols..........................
  • Page 9 2 Preparation and operation..................21 2.1 Installing the detector........................21 2.2 Plumbing the detector........................23 2.3 Installing the multi-detector drip tray....................26 2.4 Making Ethernet connections......................28 2.5 I/O signal connector........................28 2.6 Connecting to the electricity source....................29 2.7 Starting the detector........................30 2.7.1 Monitoring detector LEDs.....................
  • Page 10 4 Error messages......................56 4.1 Startup error messages........................56 4.2 Error messages preventing operation.................... 58 A Safety advisories.......................61 A.1 Warning symbols..........................61 A.1.1 Specific warnings........................62 A.2 Notices............................63 A.3 Bottles Prohibited symbol......................64 A.4 Required protection........................64 A.5 Warnings that apply to all Waters instruments and devices............64 A.6 Warnings that address the replacement of fuses................68 A.7 Electrical symbols..........................
  • Page 11 C.3.3 Wavelength selection for chromophore detection..............80 October 21, 2021, 715006903 Ver. 01 Page xi...

  • Page 12: Overview

    This guide focuses on the light-guiding, flow cell operating principles and maintenance procedures. The ACQUITY Premier TUV detector operates at wavelengths ranging from 190 to 700 nm. The detector can sample up to 80 data points per second.

  • Page 13: Detector Optics

    1.1 Detector optics The ACQUITY Premier TUV detector optics include these components: • High brightness deuterium (D ) lamp • Two mirrors: one off-axis, ellipsoidal mirror and one spherical mirror • Filter wheel • Shutter, wavelength calibration filter, and second-order filter •...

  • Page 14: Light-Guiding Flow Cell Operating Principles

    determined by the grating angle, onto the entrance of the flow cell. Light exiting the flow cell passes to the sample photodiode. 2. The beam splitter, located just ahead of the flow cell, diverts a portion of the light to a reference photodiode.
  • Page 15 In the ACQUITY Premier TUV detector, this angle is mechanically controlled by components external to the flow cell so that the variation in refractive index arising from different mobile phases does not materially influence the efficiency of the transmitted energy.

  • Page 16: Filtering Noise

    1.1.3 Filtering noise The detector provides a Hamming filter to minimize noise. The Hamming filter is a digital finite- impulse-response filter that creates peak height degradation and enhances the filtering of high- frequency noise. The behavior of the filter depends on the filter time-constant you select. You can program a filter time to be Fast, Slow, Normal, or Other.

  • Page 17: Wavelength Verification And Test

    Figure 1–4: Filter time-constant comparison Although the peak shape shows some distortion and the signal output is delayed with different time-constants, the peak area remains the same. 1.2 Wavelength verification and test Requirement: Always ensure that the front door is secured during startup verification. The detector’s deuterium arc lamp and integral erbium filter exhibit peaks in the transmission spectrum at known wavelengths.

  • Page 18: Operational Modes

    The detector wavelength verification procedures establish an approximate home position using a grating homing sensor. Once Home is established, the detector locates and references the 656.1- nm peak in the deuterium lamp emission spectrum. The integral erbium filter moves into the common light path ahead of the flow cell entrance slit, enabling the detector to locate three additional spectral features at these wavelengths: •...

  • Page 19: Dual-Wavelength Mode

    • Filter time-constant – Programs a filter time in seconds. Options are Fast, Slow, Normal, or Other. If you select Fast, Slow, or Normal, you need not specify a value. The filter constant is determined by the data rate. If you select Other, you can specify a value, but the value you specify is rounded up or down to a value based on the data rate.

  • Page 20: Ratioplot

    detector provides minimum and maximum ratio values that scale the ratio plot proportionally. In addition, a configurable minimum absorbance threshold activates ratio output scaling only when it reaches the absorbance at both wavelengths. (Dual mode only.) • Difference Plot (A-B) – This mode plots the arithmetic difference in absorbance for the two monitored wavelengths.

  • Page 21: Preparation And Operation

    2 Preparation and operation This section provides the preparation procedures necessary to set up and operate the ACQUITY Premier TUV detector. 2.1 Installing the detector To install the detector, you should generally know how to set up and operate laboratory instruments and computer-controlled devices and how to handle solvents.
  • Page 22 Figure 2–1: Proper placement for drip management system Indentations Drain routing hole for drip management system 2. Place the solvent tray module atop the detector. October 21, 2021, 715006903 Ver. 01 Page 22...

  • Page 23: Plumbing The Detector

    Figure 2–2: ACQUITY Premier TUV detector in an ACQUITY Premier System Bottle tray Detector Column heater Sample manager - flow through needle Quaternary solvent manager 2.2 Plumbing the detector Notice: To avoid causing severe damage to the instrument, use only compatible solvents.
  • Page 24 Requirement: If the ACQUITY Premier TUV detector is the last detector in the system, the back-pressure regulator is required for optimum performance. If a mass spectrometer or other detector is connected downstream of the detector, you should not install a back-pressure regulator.
  • Page 25 3. After the flange and rails are engaged, continue inserting the flow cell until the dowel pins on the detector engage the corresponding holes on the cell holder. 4. Continue to insert the flow cell until the three thumbscrews align with their holes in the bulkhead.

  • Page 26: Installing The Multi-Detector Drip Tray

    6. Remove the protective cover from the PEEK cell inlet tubing and connect the tubing to the flow cell inlet, confirming that the label on the tubing matches the type of detector and flow cell in your system. 7. Attach the short length of outlet tubing from the back-pressure regulator to the outlet of the flow cell.
  • Page 27 • Multi-detector drip tray kit To install the drip tray: 1. Turn the ACQUITY Premier TUV detector so that it is resting on its left-hand side. 2. Snap the extended plastic feet onto the bottom of the detector, and then snap the anti-skid pads onto the extended plastic feet.

  • Page 28: Making Ethernet Connections

    Figure 2–7: Installing the multi-detector drip tray (bottom view) Screws Plastic rivets Extended plastic feet 5. Return the ACQUITY Premier TUV detector to its original position atop the other detector. 2.4 Making Ethernet connections To make Ethernet connections: 1. Unpack and install the pre-configured workstation.

  • Page 29: Connecting To The Electricity Source

    Analog chart output 2.6 Connecting to the electricity source The ACQUITY Premier TUV detector requires a separate, grounded electricity source. The ground connection in the electrical outlet must be common and connected near the system. October 21, 2021, 715006903 Ver. 01...

  • Page 30: Starting The Detector

    Warning: To avoid electric shock, observe these precautions: • The power cord functions as the safety disconnect device. Position the equipment so that you can reach the power cord easily. • Use SVT-type power cords in the United States and HAR-type power cords, or better, in Europe.

  • Page 31: Monitoring Detector Leds

    If you must power-on the detector before the eluent is flowing, extinguish the lamp. You can do this in the Instrument Method Editor (Empower, MassLynx, or third-party) by specifying a Lamp On event in the Events table. You can also extinguish the lamp in one of these ways: •...

  • Page 32: About The Detector Control Panel

    Table 2–2: Lamp LED indications LED mode and color Description Unlit Indicates that the detector lamp is extinguished. Constant green Indicates that the detector lamp is ignited. Flashing green Indicates that the detector is initializing or calibrating. Flashing red Indicates that an error stopped the detector. You can find information regarding the error that caused the failure in the console.

  • Page 33: Shutting Down The Detector For Less Than 24 Hours

    The detector control panel displays the acquisition status (if the detector is running). You cannot edit detector parameters while the system is processing samples. The following table lists the items in the detector control panel. Table 2–3: Modifiable detector control panel items Control panel item Description Lamp On/Off LED...

  • Page 34: Shutting Down The Detector For More Than 24 Hours

    To shut down the detector for less than 24 hours: 1. Continue to pump the initial mobile phase mixture through the column. Doing so maintains the column equilibrium necessary for good retention time reproducibility. 2. To lengthen lamp life, extinguish the detector lamp by clicking the Lamp Off icon in the detector control panel.

  • Page 35: Maintenance Procedures

    3 Maintenance procedures This section provides the maintenance guidelines and procedures necessary to maintain the device's performance. Keep to a maintenance schedule, and perform maintenance as required and described in this section. 3.1 Contacting Waters Technical Service If you are located in the USA or Canada, report malfunctions or other problems to Waters Technical Service (800-252-4752).

  • Page 36: Safety And Handling

    3.2 Safety and handling Warning: Observe Good Laboratory Practice (GLP) at all times, particularly when working with hazardous materials. Consult the Safety Data Sheets regarding the solvents you use. Additionally, consult the safety representative for your organization regarding its protocols for handling such materials. Warning: To avoid electric shock, do not remove protective panels from the device.

  • Page 37: Flushing The Detector

    • If the light-guiding flow cell will not be used for a period of time, flush it with clean mobile phase, such as a water/acetonitrile or water/methanol mix, and either cap the flow ports or dry the flow cell with pure nitrogen or pure helium for 5 to 10 minutes. •...
  • Page 38 Required tools and materials • Chemical-resistant, powder-free gloves • Cotton swabs • Nonabrasive, lint-free wipes To resolve a detector leak sensor error: 1. View the Leak Sensors dialog box in the console to verify that the leak sensor detected a leak.
  • Page 39 Figure 3–2: Drying the leak sensor Prism Lint-free wipe 6. Roll up a nonabrasive, lint-free wipe and use it to absorb the liquid from the leak sensor reservoir and its surrounding area. Figure 3–3: Absorbing liquid from the leak sensor reservoir Rolled up lint-free wipes Leak sensor reservoir 7.
  • Page 40 Figure 3–4: Absorbing liquid from the leak sensor reservoir Cotton swab Leak sensor reservoir 8. Align the leak sensor T-bar with the slot on the leak sensor reservoir. Figure 3–5: Aligning the leak sensor T-bar with the slot on the leak sensor reservoir T-bar Slot on the leak sensor reservoir 9.

  • Page 41: Replacing The Detector's Leak Sensor

    Figure 3–6: Leak sensor installed in leak sensor reservoir Leak sensor installed 10. If you detached the leak sensor connector from the front of the instrument, reattach it. 11. In the console, select your detector from the system tree. 12. In the detector information window, click Control > Reset to reset the detector. 3.6.2 Replacing the detector's leak sensor Warning: To avoid personal contamination with biologically hazardous or toxic compounds,...
  • Page 42 Figure 3–7: Detaching the leak sensor Press down on the tab to release the connector Leak sensor connector 3. Remove the leak sensor from its reservoir by grasping it by its serrations and pulling upward on it. Figure 3–8: Removing the leak sensor Serrations 4.
  • Page 43 Figure 3–9: Align the leak sensor T-bar with the slot on the leak sensor reservoir T-bar Slot on the leak sensor reservoir 6. Slide the leak sensor into place. Figure 3–10: Leak sensor installed in leak sensor reservoir Leak sensor installed 7.

  • Page 44: Maintaining The Flow Cell

    3.7 Maintaining the flow cell Waters light-guiding flow cells transport light and sample via Teflon AF tubing. The tubing transmits energy through low-volume flow cells, resulting in heightened analytical sensitivity. Light efficiently transits tubing by means of a mechanism known as total internal reflection (TIR) in which the light remains within the fluid stream because the refractive index of the fluid exceeds that of the Teflon tubing material.

  • Page 45: Cleaning The Flow Cell

    Figure 3–13: Unwanted beam effects from a light-guiding cell The operational differences between the light-guiding method, where light is transmitted through interactions with the cell wall, and the conventional method, which avoids such interactions, underscores these practical measures for maintaining the liquid core flow cell: •...
  • Page 46 • Stainless steel unions (to replace the column during flushing) • Wrench suitable for removing and replacing the column To clean the flow cell: 1. In the detector control panel, click Lamp Off. 2. Stop the solvent flow and remove the column. 3.

  • Page 47: Performing A System Acid-Cleansing Flush

    Thumbscrews Inlet tubing Back-pressure regulator Leak sensor 5. Flush the detector with HPLC-grade water. Note: If the mobile phase is not compatible with water, flush with an intermediate solvent first. 6. Pump an acid wash composition of 1.0% formic acid in water or 90% water/10% organic mixture.
  • Page 48 a. Measure 700 mL of water in a graduated cylinder. b. In a separate graduated cylinder, measure 300 mL of phosphoric acid. c. Add phosphoric acid to water and mix for five minutes. 3. Fill a 1-L mobile phase reservoir with 100% water. 4.

  • Page 49: Replacing The Flow Cell

    14. Switch the solvent to 100% water, prime, and flow to ensure the 30:70 phosphoric acid/ water is out of the pump. 15. Reconnect the sample manager. 16. Repeat steps 1 through 8 using 100% water as the solvent. 17. Repeat steps 1 through 8 using 50:50 (v/v) methanol/water as the solvent. 18.
  • Page 50 Figure 3–15: Detector front door opened Lamp ID Lamp Outlet tubing Flow cell ID connector Flow cell assembly Flow cell handle Thumbscrews Inlet tubing Back-pressure regulator Leak sensor 5. Disconnect the flow cell ID connector (if present). 6. Remove the flow cell: a.
  • Page 51 Note: To avoid damaging the capillary tubing, do not touch it. 7. Unpack and inspect the new flow cell, ensuring that the flow-cell type is correct for your application. Note: When replacing the flow cell, replace the flow cell inlet tubing with the tubing included with the new flow cell.

  • Page 52: Replacing The Lamp

    To replace the lamp: 1. Power-off the lamp: a. To power-off the lamp manually, click ACQUITY Premier TUV Detector in the left- hand pane of the console, and then click Lamp Off. The green LED on the console darkens, as does the Lamp LED on the door.
  • Page 53 Figure 3–17: Detector front door opened Lamp ID Lamp Outlet tubing Flow cell ID connector Flow cell assembly Flow cell handle Thumbscrews Inlet tubing Back-pressure regulator Leak sensor 5. Loosen the two captive screws in the lamp base and gently withdraw the lamp from the lamp housing.

  • Page 54: Replacing The Fuse

    Warning: Lamp gas is under negative pressure. To avoid shattering the glass, use care when disposing of the lamp. Waters suggests that you adequately cushion the old lamp by containing it in the packaging of its replacement before you dispose of it. 6.

  • Page 55: Cleaning The Instrument's Exterior

    To replace the fuses: 1. Power-off the detector and disconnect the power cord from the power entry module. 2. Pinch the sides of the spring-loaded fuse holder, which is above the power entry module on the rear panel of the detector. With minimum pressure, withdraw the spring-loaded fuse holder.

  • Page 56: Error Messages

    4 Error messages The detector provides error messages to help troubleshoot system problems. 4.1 Startup error messages Startup diagnostic tests run automatically when you power-on the detector. They verify the proper operation of the detector electronics. If one or more of the tests fail, the detector beeps and displays an error message.
  • Page 57 Error message Description Corrective action Calibration unsuccessful: Peak Results of a calibration 1. Ensure that the front out of range n.nn nm operation differ by more than door is closed. 1.0 nm. Unit uses previously 2. Flush flow cell. stored calibration points. Flow cell memory device not Unable to electronically Connect flow cell identification...

  • Page 58: Error Messages Preventing Operation

    Error message Description Corrective action order filter and issues a warning message that any data collected for wavelengths above 370 nm may contain inaccuracies because of possible UV light interference (second- order effects). 4.2 Error messages preventing operation During initialization, calibration, and operation, the detector can display <Error> in the control panel, signifying a usually terminating malfunction and preventing further operation of the detector.
  • Page 59 Error message Description Corrective action Dark current too low: 0 Dark energy level equals 0. 1. Cycle power to the detector. 2. Contact Waters Technical Service. Electronic A/D failure Lamp optimization is adjusted 1. Cycle power to the at the minimum level. detector.
  • Page 60 Error message Description Corrective action Grating initialization failure: Backlash is the difference 1. Cycle power to the Backlash too high between the forward and detector. reverse peak positions of 2. Contact Waters deuterium at 656 nm. If this Technical Service. difference is greater than one step, the unit displays this message.

  • Page 61: A Safety Advisories

    A Safety advisories Waters products display safety symbols that identify hazards associated with the product’s operation and maintenance. The symbols also appear in product manuals with statements that describe the hazards and advise how to avoid them. This appendix presents all safety symbols and statements that apply to Waters’...

  • Page 62: Specific Warnings

    Warning: (Risk of exposure to ultraviolet radiation.) Warning: (Risk of contacting corrosive substances.) Warning: (Risk of exposure to a toxic substance.) Warning: (Risk of personal exposure to laser radiation.) Warning: (Risk of exposure to biological agents that can pose a serious health threat.) Warning: (Risk of tipping.)

  • Page 63: Notices

    A.1.1.2 Biohazard warning The following warning applies to Waters instruments and devices that can process biologically hazardous materials. Biologically hazardous materials are substances that contain biological agents capable of producing harmful effects in humans. Warning: To avoid infection from blood-borne pathogens, inactivated microorganisms, and other biological materials, assume that all biological fluids that you handle are infectious.

  • Page 64: Bottles Prohibited Symbol

    A.3 Bottles Prohibited symbol The Bottles Prohibited symbol alerts you to the risk of equipment damage caused by solvent spills. Prohibited: To avoid equipment damage caused by spilled solvent, do not place reservoir bottles directly atop an instrument or device or on its front ledge. Instead, place the bottles in the bottle tray, which serves as secondary containment in the event of spills.
  • Page 65 Advertencia: cualquier cambio o modificación efectuado en esta unidad que no haya sido expresamente aprobado por la parte responsable del cumplimiento puede anular la autorización del usuario para utilizar el equipo. 警告： 未经有关法规认证部门明确允许对本设备进行的改变或改装，可能会使使用者 丧失操作该设备的合法性。 警告： 未經有關法規認證部門允許對本設備進行的改變或修改,可能會使使用者喪失操 作該設備的權利。 경고 규정 준수를 책임지는 당사자의 명백한 승인 없이 이 장치를 개조 또는 변경할 경 우, 이...
  • Page 66 Warnung: Bei der Arbeit mit Polymerschläuchen unter Druck ist besondere Vorsicht angebracht: • In der Nähe von unter Druck stehenden Polymerschläuchen stets Schutzbrille tragen. • Alle offenen Flammen in der Nähe löschen. • Keine Schläuche verwenden, die stark geknickt oder überbeansprucht sind. •...
  • Page 67 警告： 当有压力的情况下使用管线时，小心注意以下几点： • 当接近有压力的聚合物管线时一定要戴防护眼镜。 • 熄灭附近所有的火焰。 • 不要使用已经被压瘪或严重弯曲的管线。 • 不要在非金属管线中使用四氢呋喃或浓硝酸或浓硫酸。 • 要了解使用二氯甲烷及二甲基亚枫会导致非金属管线膨胀，大大降低管线的耐压能 力。 警告： 當在有壓力的情況下使用聚合物管線時，小心注意以下幾點。 • 當接近有壓力的聚合物管線時一定要戴防護眼鏡。 • 熄滅附近所有的火焰。 • 不要使用已經被壓癟或嚴重彎曲管線。 • 不要在非金屬管線中使用四氫呋喃或濃硝酸或濃硫酸。 • 要了解使用二氯甲烷及二甲基亞楓會導致非金屬管線膨脹，大大降低管線的耐壓能 力。 경고 가압 폴리머 튜브로 작업할 경우에는 주의하십시오. • 가압 폴리머 튜브 근처에서는 항상 보호 안경을 착용하십시오. •...

  • Page 68: Warnings That Address The Replacement Of Fuses

    Warning: The user shall be made aware that if the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired. Avertissement : L’utilisateur doit être informé que si le matériel est utilisé d’une façon non spécifiée par le fabricant, la protection assurée par le matériel risque d’être défectueuses.
  • Page 69 Avertissement : pour éviter tout risque d'incendie, remplacez toujours les fusibles par d'autres du type et de la puissance indiqués sur le panneau à proximité du couvercle de la boite à fusible de l'instrument. Warnung: Zum Schutz gegen Feuer die Sicherungen nur mit Sicherungen ersetzen, deren Typ und Nennwert auf den Tafeln neben den Sicherungsabdeckungen des Geräts gedruckt sind.

  • Page 70: Electrical Symbols

    警告： 为了避免火灾，应更换“维护步骤”一章的“更换保险丝”一节中介绍的相同类型和 规格的保险丝。 警告： 為了避免火災，更換保險絲時，應使用「維護步驟」章節中「更換保險絲」所 指定之相同類型與規格的保險絲。 화재의 위험을 막으려면 유지관리 절차 단원의 “퓨즈 교체” 절에 설명된 것과 동일 경고 한 타입 및 정격의 제품으로 퓨즈를 교체하십시오. 警告 火災予防のために、ヒューズ交換ではメンテナンス項目の「ヒューズの交換」 に記載されているタイプおよび定格のヒューズをご使用ください。 A.7 Electrical symbols The following electrical symbols and their associated statements can appear in instrument manuals and on an instrument’s front or rear panels.

  • Page 71: Handling Symbols

    A.8 Handling symbols The following handling symbols and their associated statements can appear on labels affixed to the packaging in which instruments, devices, and component parts are shipped. Symbol Description Keep upright! Keep dry! Fragile! Use no hooks! Upper limit of temperature Lower limit of temperature Temperature limitation October 21, 2021, 715006903 Ver.

  • Page 72: B Specifications

    B Specifications This section lists individual operating specifications for the ACQUITY Premier TUV Detector, as follows: • Operational specifications • Optical component specifications • Environmental specifications • Electrical specifications • Dimensions B.1 Operational specifications Condition Specification Wavelength range 190 to 700 nm Bandwidth <5 nm...

  • Page 73: Optical Component Specifications

    Condition Specification Analog output 10, 20, 40, 80 Hz (channel A) data rates 10 Hz only (channel B) (single λ mode) B.2 Optical component specifications Condition Specification Lamp source 30-W High Brightness Deuterium lamp, 0.5 nm aperture, pre-aligned 2000-hour warranty, front accessible Photodiodes 2 silicon photodiodes (matched pair) Second-order filter...

  • Page 74: Electrical Specifications

    B.4 Electrical specifications Condition Specification Line frequency 50 to 60 Hz Line voltage 100 to 240 Vac Max VA input 200 VA Fuse ratings Two fuses: 100 to 240-Vac, 50 to 60 Hz F 3.15-A 250-V fast blo, 5 × 20 mm (IEC) Attenuated analog output channel: Attenuation range: 0.0001 to 4.000 AU 2 VFS...

  • Page 75: C Solvent Considerations

    C Solvent considerations Warning: Observe Good Laboratory Practice (GLP) at all times, particularly when working with hazardous materials. Consult the Safety Data Sheets regarding the solvents you use. Additionally, consult the safety representative for your organization regarding its protocols for handling such materials. C.1 Introduction Preventing contamination For more information on preventing contamination, refer to Controlling Contamination in LC/MS...

  • Page 76: Solvent Miscibility

    Using buffers Adjust the pH of aqueous buffers. Filter them to remove insoluble material, and then blend them with appropriate organic modifiers. After you use a buffer, flush it from the pump by running a wet prime with at least five system volumes of HPLC-grade distilled or deionized water. For shutdowns of more than a day, flush the pump with a 20% methanol/water solution to prevent microbial growth.
  • Page 77 Table C–1: Solvent miscibility (continued) Polarity Solvent Viscosity Boiling Miscibility λ Cutoff index CP, 20 °C point °C number (nm) (1 atm) Isopropyl ether 0.33 68.3 –– Toluene 0.59 100.6 P-xylene 0.70 138.0 Benzene 0.65 80.1 Benzyl ether 5.33 288.3 ––...

  • Page 78: How To Use Miscibility Numbers

    Table C–1: Solvent miscibility (continued) Polarity Solvent Viscosity Boiling Miscibility λ Cutoff index CP, 20 °C point °C number (nm) (1 atm) Formamide 3.76 210.5 –– Water 1.00 100.0 –– –– C.2.1 How to use miscibility numbers Use miscibility numbers (M-numbers) to predict the miscibility of a liquid with a standard solvent. To predict the miscibility of two liquids, subtract the smaller M-number value from the larger M- number value.

  • Page 79: Uv Cutoffs For Common Solvents

    C.3.1 UV cutoffs for common solvents The table below shows the UV cutoff (the wavelength at which the absorbance of the solvent is equal to 1 AU) for some common chromatographic solvents. Operating at a wavelength near or below the cutoff increases baseline noise because of the absorbance of the solvent. Table C–2: UV cutoff wavelengths for common chromatographic solvents Solvent UV cutoff...
  • Page 80 Table C–3: Wavelength cutoffs for different mobile phases Mobile phases UV cutoff Mobile phases UV cutoff (nm) (nm) Acetic acid, 1% Sodium chloride, 1 M Ammonium acetate, 10 mM Sodium citrate, 10 mM Ammonium bicarbonate, 10 Sodium dodecyl sulfate BRIJ 35, 0.1% Sodium formate, 10 mM CHAPS, 0.1% Triethyl amine, 1%...
  • Page 81 Table C–4: Electronic absorption bands of representative chromophores* Chromophore Chemical λmax εmax λmax εmax configuration (nm) (L/m/cm) (nm) (L/m/cm) Ether —O— 1000 Thioether —S— 4600 1600 Amine —NH 2800 Thiol —SH 1400 Disulfide —S—S— 5500 Bromide —Br Iodide —I Nitrile —C≡N —...
  • Page 82 Table C–4: Electronic absorption bands of representative chromophores* (continued) Chromophore Chemical λmax εmax λmax εmax configuration (nm) (L/m/cm) (nm) (L/m/cm) (alicyclic) 8000 Ethylenic/ C=C—C≡C 6,500 Acetylenic Ethylenic/ C=C—C=N 23,000 Amido Ethylenic/ C=C—C=O 210-250 10,000- Carbonyl 20,000 Ethylenic/ C=C—NO 9,500 Nitro *Willard, H.

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