ACQUITY Refractive Index Detector Overview and Maintenance Guide 715003547 / Revision C
Copyright © Waters Corporation 2014 All rights reserved
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General Information
Copyright notice © 2014 WATERS CORPORATION. PRINTED IN THE UNITED STATES OF AMERICA AND IN IRELAND. ALL RIGHTS RESERVED. THIS DOCUMENT OR PARTS THEREOF MAY NOT BE REPRODUCED IN ANY FORM WITHOUT THE WRITTEN PERMISSION OF THE PUBLISHER. The information in this document is subject to change without notice and should not be construed as a commitment by Waters Corporation. Waters Corporation assumes no responsibility for any errors 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 damages in connection with, or arising from, its use. For the most recent revision of this document, consult the Waters Web site (waters.com).
Trademarks ACQUITY, “THE SCIENCE OF WHAT’S POSSIBLE.”, and Waters are registered trademarks, and ACQUITY APC, ACQUITY Advanced Polymer Chromatography, and Empower are trademarks of Waters Corporation. Teflon is a registered trademarks of E. I. du Pont de Nemours and Company. Other registered trademarks or trademarks are the sole property of their owners.
Customer comments Waters’ Technical Communications department invites you to tell us of any errors you 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 usability. We seriously consider every customer comment we receive. You can reach us at
[email protected].
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Contacting Waters ®
Contact Waters with enhancement requests or technical questions regarding the use, transportation, removal, or disposal of any Waters product. You can reach us via the Internet, telephone, or conventional mail. Waters contact information: Contacting medium
Information
Internet
The Waters Web site includes contact information for Waters locations worldwide. Visit www.waters.com.
Telephone and fax
From the USA or Canada, phone 800 252 4752, or fax 508 872 1990. For other locations worldwide, phone and fax numbers appear in the Waters Web site.
Conventional mail
Waters Corporation 34 Maple Street Milford, MA 01757 USA
Safety considerations Some reagents and samples used with Waters instruments and devices can pose chemical, biological, or radiological hazards (or any combination thereof). You must know the potentially hazardous effects of all substances you work with. Always follow Good Laboratory Practice, and consult your organization’s safety representative for guidance.
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High voltage hazard Warning: To avoid electric shock, do not remove protective panels from ® the ACQUITY Refractive Index Detector. The components within are not user-serviceable.
FCC radiation emissions notice Changes or modifications not expressly approved by the party responsible for compliance, could void the users authority to operate the equipment. This device complies with Part 15 of the FCC Rules. Operation is subject to the following two conditions: (1) this device may not cause harmful interference, and (2) this device must accept any interference received, including interference that may cause undesired operation.
Canada spectrum management emissions notice This class A digital product apparatus complies with Canadian ICES-001. Cet appareil numérique de la classe A est conforme à la norme NMB-001.
Electrical power safety notice Do not position the instrument so that it is difficult to operate the disconnecting device.
Safety hazard symbol notice Documentation needs to be consulted in all cases where the symbol is used to find out the nature of the potential hazard and any actions which have to be taken.
Equipment misuse notice If the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired.
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Safety advisories Consult Appendix A for a comprehensive list of warning and caution advisories.
Operating this instrument When operating this instrument, follow standard quality-control (QC) procedures and the guidelines presented in this section.
Applicable symbols Symbol
Definition Manufacturer Authorized representative of the European Community Confirms that a manufactured product complies with all applicable European Community directives Australia C-Tick EMC compliant Confirms that a manufactured product complies with all applicable United States and Canadian safety requirements Consult instructions for use Electrical and electronic equipment with this symbol may contain hazardous substances and should not be disposed of as general waste. For compliance with the Waste Electrical and Electronic Equipment Directive (WEEE) 2012/19/EU, contact Waters Corporation for the correct disposal and recycling instructions.
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Audience and purpose This guide is intended for use by individuals who operate and maintain the ACQUITY refractive index detector.
Intended use of the ACQUITY refractive index detector Waters designed the ACQUITY Refractive Index Detector for use in ultra-performance liquid chromatography and advanced polymer chromatography applications. It provides sensitivity, stability, and reproducibility for the analysis of components, with limited or no UV absorption. The refractive index detector is for research use only and is not intended for use in diagnostic applications.
Calibrating To calibrate LC systems, follow acceptable calibration methods using at least five standards to generate a standard curve. The concentration range for standards should include the entire range of QC samples, typical specimens, and atypical specimens.
Quality-control Routinely run three QC samples that represent subnormal, 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 out of range might not be valid. Do not report these data until you are certain that the instrument performs satisfactorily.
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ISM classification ISM Classification: ISM Group 1 Class B This classification has been assigned in accordance with IEC CISPR 11 Industrial Scientific and Medical (ISM) instruments requirements. Group 1 products apply to intentionally generated and/or used conductively coupled radio-frequency energy that is necessary for 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 authorized representative
Waters Corporation Stamford Avenue Altrincham Road Wilmslow SK9 4AX UK
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Telephone:
+44-161-946-2400
Fax:
+44-161-946-2480
Contact:
Quality manager
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Table of Contents General Information .................................................................................... iii Copyright notice .................................................................................................. iii Trademarks ........................................................................................................... iii Customer comments ............................................................................................ iii Contacting Waters ............................................................................................... iv Safety considerations .......................................................................................... iv High voltage hazard............................................................................................. v FCC radiation emissions notice .......................................................................... v Canada spectrum management emissions notice .............................................. v Electrical power safety notice ............................................................................. v Safety hazard symbol notice................................................................................ v Equipment misuse notice .................................................................................... v Safety advisories ................................................................................................. vi Operating this instrument ................................................................................. vi Applicable symbols ............................................................................................. vi Audience and purpose....................................................................................... vii Intended use of the ACQUITY refractive index detector ............................... vii Calibrating ........................................................................................................ vii Quality-control .................................................................................................. vii ISM classification .............................................................................................. viii ISM Classification: ISM Group 1 Class B ...................................................... viii EC authorized representative ........................................................................ viii
1 The ACQUITY Refractive Index Detector ......................................... 13 Location of the refractive index detector in an example system ........... 15 Operating principles ......................................................................................... 15 Optical refraction ............................................................................................... 15 Differential refractometry ................................................................................. 20 October 13, 2014, 715003547 Rev. C
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Common refractive index detection problems ........................................... Environmental factors ....................................................................................... Inhomogeneities in solution .............................................................................. Range and attenuation ......................................................................................
23 23 23 24
Features ............................................................................................................... Fluid path components ...................................................................................... Flow path............................................................................................................ Purge mode......................................................................................................... Recycle mode ...................................................................................................... Countercurrent heat exchanger ........................................................................ Flow cell.............................................................................................................. Purge valve......................................................................................................... Pressure relief valve .......................................................................................... Recycle valve ...................................................................................................... Insulated sample inlet tubing ...........................................................................
24 25 25 27 29 30 30 30 30 31 31
Optics .................................................................................................................... 32 Selecting the appropriate sampling rate ..................................................... 33 Filtering noise ..................................................................................................... 34 Polarity ................................................................................................................. 35 Temperature control ......................................................................................... 36
2 Preparing the detector .......................................................................... 37 Stacking the modules ........................................................................................ 38 Installing the leak sensor ................................................................................. 39 Installation recommendations for fittings ................................................... 41 Connecting a column or second detector ..................................................... 42 Connecting to waste .......................................................................................... 43 Making the recycle connection ....................................................................... 44 Installing the multi-detector drip tray ......................................................... 45 Making the Ethernet connection ................................................................... 45 x
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Making signal connections .............................................................................. 45 Connecting to the electricity source ............................................................. 48 Typical solvent problems ................................................................................. 49 Selecting a solvent ............................................................................................. Solvent quality ................................................................................................... Preparation checklist......................................................................................... Water .................................................................................................................. Buffers ................................................................................................................ Tetrahydrofuran (THF) ..................................................................................... Refractive indices of common solvents .............................................................
49 49 50 50 50 51 51
Solvent degassing .............................................................................................. Gas solubility ..................................................................................................... Solvent degassing methods ............................................................................... Solvent degassing considerations .....................................................................
52 52 53 54
3 Using the detector ................................................................................... 57 Starting the detector ......................................................................................... 58 Monitoring detector LEDs ................................................................................. 59 About the detector control panel....................................................................... 60 Resolving leak sensor errors ........................................................................... 63 Shutting down the detector ............................................................................. 66 Removing buffered mobile phase ...................................................................... 67
4 Maintenance Procedures ...................................................................... 69 Maintaining the detector ................................................................................. Contacting Waters technical service................................................................. Maintenance schedule ....................................................................................... Configuring maintenance warnings .................................................................
70 70 71 72
Spare parts .......................................................................................................... 72 Troubleshooting with Connections INSIGHT ............................................. 72 Safety and handling .......................................................................................... 74
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Replacing the leak sensor ................................................................................ 75 Decontaminating the fluid path ..................................................................... 77 Cleaning the refractive index detector’s exterior ...................................... 79
A Safety Advisories .................................................................................... 81 Warning symbols ................................................................................................ 81 Task-specific hazard warnings.......................................................................... 81 Specific warnings ............................................................................................... 82 Caution advisory ................................................................................................ 84 Warnings that apply to all Waters instruments and devices ................... 85 Electrical and handling symbols .................................................................... 90 Electrical symbols .............................................................................................. 90 Handling symbols .............................................................................................. 91
B Specifications .......................................................................................... 93 Physical specifications ..................................................................................... 93 Environmental specifications ......................................................................... 94 Electrical specifications ................................................................................... 94 Input/output specifications ............................................................................. 95 Performance specifications ............................................................................. 95 Wetted materials of construction ................................................................... 97
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The ACQUITY Refractive Index Detector The ACQUITY refractive index detector is designed for ultra-performance liquid chromatography and advanced polymer chromatography applications. It operates as a component of Waters ® ACQUITY systems. Refer to Appendix B, for system specifications, and to Chapter 2, for solvent considerations. The major advantage of refractive index detectors lies in the universal nature of their response. They are well-suited to analyze compounds that are without strong UV chromophores, fluorophores, or electrochemical or ionic activity. Refractive index (RI) detectors are used to analyze carbohydrates, lipids, and polymers. RI detectors work by measuring changes in the bulk properties of the solvent and the solutes under investigation, exploiting the improbability that solvents and solutes would share the identical refractive index. RI detection is inherently less sensitive than other detection methods. It is not suitable to gradient analyses, and changes in solvent temperature and pressure can cause baseline instability. Also, the possibility exists that positive or negative peaks can appear during a single analysis.
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1 The ACQUITY Refractive Index Detector
Contents: Topic
Page
Location of the refractive index detector in an example system ......................................................................................... 15 Operating principles ........................................................................ 15 Common refractive index detection problems ................................ 23 Features............................................................................................ 24 Optics ................................................................................................ 32 Selecting the appropriate sampling rate ........................................ 33 Filtering noise .................................................................................. 34 Polarity ............................................................................................. 35 Temperature control ........................................................................ 36
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Location of the refractive index detector in an example system
Location of the refractive index detector in an example system The following diagram shows the location of a refractive index detector in a typical system.
Bottle tray Refractive index detector TP03471
Column heater Sample manager flow through needle
Quaternary solvent manager
Operating principles Optical refraction When a beam of light passes from one medium into another, it changes its speed. If the light enters the second medium at an angle that is not perpendicular to the medium’s surface, the light is bent (refracted).
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1 The ACQUITY Refractive Index Detector
The extent to which a medium refracts light is its refractive index (RI), calculated as the ratio of the velocity of light in a vacuum to the velocity of light in the medium. It is a physical property of the medium, with a dimensionless integer value represented by the letter n.
Factors that affect RI The refractive index of a medium depends solely on the speed of light through the medium, which is constant for a given wavelength of light at a specified temperature and pressure. Wavelength The refractive index of a medium has a specific value that changes with the wavelength of the incident light beam. The detector uses monochromatic light at a fixed wavelength, so the effect of different wavelengths of light on RI is not discussed in this guide. Density The density of the 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. These are the most important of the factors that affect the density of a medium are: •
Composition
•
Temperature
•
Pressure
The following figure illustrates the effect of density on the RI of two solutions. The refractive index of a sucrose solution changes linearly with concentration
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Operating principles
over this range of compositions, but a methanol solution exhibits a nonlinear region between concentrations of 45 and 55%. Effect of density on RI:
Refractive index
Weight percent sucrose in water
Density (g/mL)
Refractive index
Weight percent methanol in water
Density (g/mL)
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1 The ACQUITY Refractive Index Detector
Measuring refraction The extent to which a beam of light undergoes refraction when it enters a medium depends on these properties: •
The angle at which the light enters a changed medium (the angle of incidence)
•
The refractive indices of the old and new media
The following figure illustrates the relationship between the angle of incidence, angle of refraction, and refractive index. Refraction of light: Incoming light beam
Angle of incidence
θ1
Medium 1, RI - n1 Medium 2, RI - n2 Angle of refraction
θ2
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Refracted light beam
Operating principles
The relationship between the refractive indices of the two media and the angles of incidence and refraction is described by Snell’s law: n1(sin θ1) = n2(sin θ2) where θ1 = Angle of incidence θ2 = Angle of refraction n1 = RI of medium 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.
Using changes in RI for sample detection As the separated components of a sample pass through the refractometer flow cell, these events occur: •
The composition of the sample solution in the flow cell changes.
•
The RI of the solution changes.
•
The light beam passing through the solution is refracted.
The refractometer detects the position of the refracted light beam, creating a signal that differs from the baseline signal. The following figure shows how refraction by the sample in the flow cell changes the proportion of light on each element of the photodiode.
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1 The ACQUITY Refractive Index Detector
Presence of sample changes the photodiode signal:
Dual-element photodiode
Sample in sample side of flow cell
Collimating lens
Reference side of flow cell
Sample side of flow cell
Reference side of flow cell Incident light
By keeping wavelength, temperature, and pressure constant, the changes in RI measured by the refractometer are due only to changing sample concentration. A solution with a high concentration of solute refracts a beam of light more than a dilute solution does. Therefore, high concentrations of sample yield large peaks.
Differential refractometry The 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 referred to as Δn, expressed in refractive index units (RIU). The refractive index detector measures Δn values as small as 7 × 10–9 RIU by detecting the difference in the amount of light falling upon each of the elements of the dual-element photodiode (see the previous figure).
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Operating principles
External angle of deflection The ratio of light on the two photodiode elements, which arises from a positional change of an image cast onto the photodiode, is determined by the external angle of deflection (φ), as shown in the figure below. The external angle of deflection determines the magnitude of the shift (Δx) of a slit image cast on the photodiode by the light beam. The following figure illustrates the external angle of deflection and its dependence on the difference in RIs (Δn) between the reference and sample sides of the flow cell. How refraction changes the external angle of deflection: Y θ
n
φ Reference side of flow cell
n
Y θ
n + Δn Sample side of flow cell φ n
= Δx
Effect of refraction on the external angle of deflection As the beam of light moves along the light path to the photodiode, it encounters and is refracted by the air in the optics bench assembly, the fused
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1 The ACQUITY Refractive Index Detector
quartz walls of the flow cell, the solvent in the reference side of the flow cell, and the solution in the sample side of the flow cell. Of these refractive media, only the solution in the sample side of the flow cell changes over the course of a run. As a result, the external angle of deflection of the reference does not change until a change in the RI of the sample causes the light beam’s refraction from its zero position. The relationship between the external angle of deflection and the RI of the sample solution is expressed as Δn ≅ φ/tanθ where Δn = Difference in RI between the solvent and the solvent-sample solution φ = External angle of deflection (in radians) θ = Angle of incidence (in radians)
Effect of refraction on the photodiode signal The change in the external angle of deflection determines the shift (Δx) of the light beam on the photodiode. Because the detector uses a dual-pass optics bench assembly, the light beam passes through the flow cell twice before reaching the photodiode, doubling the image shift. The relationship between the image shift (Δx) at the refractive index detector photodiode and the change in RI of the solution is expressed as Δx = 2Y(tanθ) Δn where Δx = Distance of the image shift at the photodiode Y = Distance from the flow cell to the photodiode θ = Angle of incidence Δn = Difference in RI between solvent and sample solution The angle of incidence and the distance to the photodiode are fixed in the refractometer, so the equation becomes Δx = C Δn where C = A constant representing the fixed values 22
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Common refractive index detection problems
By detecting how far the image shifts (Δx), the refractometer measures the difference in RI (Δn) between the solvent-sample solution and the solvent alone. The shift in the ratio of the amount of the light beam striking each element of the dual-element photodiode results in a change in the output voltage from the refractive index detector. The data system registers the changes in output voltage as peaks in the chromatogram.
Common refractive index detection problems Changes in solution density caused by factors other than sample concentration are the most common source of problems in refractive index detection. Changes in solution density can be due to these causes: •
Environmental factors such as changes in temperature or pressure
•
Inhomogeneities in the solution
Environmental factors Even small changes in ambient temperature can cause baseline drift. Backpressure pulses from a dripping waste tube can cause short-term baseline cycling. Refer to the ACQUITY online Help for more information.
Inhomogeneities in solution The differential refractometer measures the difference in refraction between the reference solvent and the sample solution. Most common inhomogeneity problems are the result of improper solvent preparation. •
The mobile phase must be of constant composition.
•
Gradient separations are not recommended because the Δn from the mobile phase change can be larger than that from the analyte peak and can exceed the detection range (5 × 10–4 RIU) from the reference cell contents.
•
For maximum sensitivity, use the same solvent to prime all solvent lines on the binary solvent manager or quaternary solvent manager.
Because the refractive index detector is sensitive to contaminants, replacing tubing can often require long wash times. See Chapter 2 for more information.
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1 The ACQUITY Refractive Index Detector
Range and attenuation The total refractive index range of the detector is 1.00 to 1.75. However, for optimum performance, the usable solvent refractive index range is 1.24 to 1.60. The measurement range of the instrument is 7 × 10–9 to 5 × 10–4 refractive index units full scale (RIU mode).
Features Detector features:
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Feature
Description
Single channel/additional channel to monitor temperature
The ability to monitor refractive index and flow cell temperature.
Thermal stability
A countercurrent heat exchanger design and temperature-controlled, low-volume cell permit stable operation.
Single, programmable contact closure output
A configurable switch accommodates a maximum +30 V and 1 A. The switch can trigger fraction collectors and other external and it can actuate based on time and refractive index threshold criteria.
Refractive index units
The ability to provide measured refractive index signals to nano-RIU sensitivity.
Purge
Programmable, for purging the reference flow cell before performing a measurement. See also: For information about purging the detector, consult the ACQUITY Console online Help.
Long-life LED lamp
An 870-nm, long-life LED lamp.
Recycle valve
A preconfigured diverter valve recycles solvent and can be programmed to reduce solvent consumption. The valve can be set to the waste or recycle position via the console. See also: For information about recycling solvent, consult the ACQUITY Console online Help.
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Features
Detector features: (Continued) Feature
Description
Relief valve
Prevents overpressuring the flow cell and, consequently, possible flow cell damage.
Fluid path components The fluid path of the ACQUITY refractive index detector includes these components: •
Countercurrent heat exchanger
•
End-cap heat exchanger
•
Flow cell, with sample and reference sides
•
Purge valve
•
Pressure relief valve
•
Recycle valve
•
Inlet and outlet tubing
Flow path During an analysis, solvent flows as indicated in the following sequence: 1.
Enters through the inlet tubing port.
2.
Passes through the inlet 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.
Exits though the outlet tube of the countercurrent heat exchanger.
6.
Passes through the purge valve (and, optionally, the recycle valve) to the waste tubing.
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1 The ACQUITY Refractive Index Detector
Flow path during analysis: Flow cell
End cap heat exchanger
R
S
Fluid path for normal mode
Counter current heat exchanger
Relief valve (closed)
Purge valve (open) Sample in
Purge out
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Waste out
Features
Purge mode When you purge the detector, solvent flows as indicated in the following sequence: 1.
Enters through inlet tubing port.
2.
Passes through the inlet 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 cross fitting, bypassing the countercurrent heat exchanger.
6.
Flows through the reference side of the flow cell.
7.
Exits through the pressure-relief valve, and then either to waste or the recycle valve.
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1 The ACQUITY Refractive Index Detector
Flow path during purge: End cap heat exchanger
Flow cell R
Cross connection S
Fluid path for purge mode Counter current heat exchanger
Tee connection
Relief valve (open)
Purge valve (closed) Sample in
Purge out
Waste out
It is best to purge the flow cell before an analysis. In doing so, you pass fresh mobile phase into the reference side of the cell. No chromatographically significant data is available during a purge. An icon in the console indicates when the detector is undergoing a purge.
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Features
You can perform a purge via the console, the control panel, or an equilibration method with the purge parameter enabled. See also: For additional information about purging the detector, consult the ACQUITY Console online Help.
Recycle mode You engage the recycle mode via the console or control panel. A programmatically controlled recycle valve diverts the outlet fluid to one of two ports. An icon appearing in the console indicates when the unit is in recycle mode. The recycle valve’s ports and their corresponding outlet lines are labelled accordingly. See also: For additional information about recycling solvent, consult the ACQUITY Console online Help. ACQUITY refractive index detector external plumbing and valves: Purge valve
Pressure relief valve
Recycle valve
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1 The ACQUITY Refractive Index Detector
Countercurrent heat exchanger Achieving a stable baseline requires precise control of the temperature of the flow cell and the fluid entering it. The low-dispersion, countercurrent heat exchanger minimizes temperature fluctuations in the sample side of the flow cell. The device’s sample inlet and outlet lines are coaxial, which facilitates heat exchange between incoming and outgoing fluids. The refractive index of typical mobile phases used in liquid chromatography has a temperature sensitivity of about 3% per °C.
Flow cell The flow cell consists of two hollow prisms of fused quartz. Each prism has an inlet and outlet. One of the prisms constitutes the cell’s sample side through which a constant flow of eluent passes during analysis. The columns used in UPLC have smaller inner diameters (2.1 vs. 4.6 mm) and smaller particles (1.7 vs. 3.5 μm). Peaks generated by UPLC will have volumes which are 4 to 5 times smaller than those observed with HPLC. Consequently, the flow cell volume has been reduced to preserve this enhancement of peak resolution and sensitivity. The other prism constitutes the cell’s reference side. It is filled with fresh solvent when you purge the detector during equilibration. When you switch from purging to normal operation, the purge valve opens, and the pressure relief valve shuts, stopping the flow of solvent through the reference prism but leaving the cell filled with fresh solvent.
Purge valve During normal operation, the purge valve remains open. Fluid that passes through the sample side of the flow cell flows through the purge valve and out through the outlet tubing to the waste reservoir. When you purge the detector, the purge valve closes causing fluid passing through the sample side of the flow cell to exit through the reference side of the flow cell, through the relief valve, and then to waste.
Pressure relief valve During normal operation, the pressure relief valve remains closed. It opens when the pressure inside the flow cell, whose maximum pressure rating is 1000 kPa (10 bar, 145 psi), becomes too high for the pressure relief valve to
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Features
withstand, thus protecting the flow cell from exceeding the maximum pressure rating. The pressure rating of the relief valve is 206.8 kPa (2 bar, 30 psi). During purging, fluid moving through the sample and reference sides of the flow cell exits through the pressure relief valve and then to the waste reservoir. The figures on page 26 and page 28 indicate the paths of solvent and sample in the detector during normal operation and during a purge, respectively. The following table provides the inner diameters of the sample and fluid lines. Fluid line diameters: Fluid line
Inner diameter (inches)
Sample in
0.005
Sample out
0.040
Reference in
0.020
Reference out
0.020
Recycle in
0.040
Recycle out
0.040
Recycle valve During normal operation, the recycle valve remains closed. It opens only when you specify recycling from the console, control panel, or by running a method with the recycle valve parameter or timed events enabled. A closed valve diverts solvent to the second port, to which you can plumb fluid lines and thus return mobile phase to the main solvent reservoir during equilibration.
Insulated sample inlet tubing To ensure good thermal isolation, and reduce baseline instability, use insulated tubing to connect the temperature-controlled column to the detector’s sample inlet. ®
Note: The sample inlet tubing provided in the startup kit has Teflon insulation.
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1 The ACQUITY Refractive Index Detector
Optics The detector’s optics bench assembly consists of these components: •
Source lamp
•
Lamp lens mask
•
Lamp lens
•
Flow cell, with sample and reference sides
•
Mirror
•
Mirror mask
•
Collimating lens
•
Stray light mask
•
Dual-element photodiode
The following figure shows the path of the light beam as it passes through the components in the optics bench assembly. Optics bench assembly light path: Mirror Flow cell
Dual-element photodiode
Flow cell lens Mirror mask
32
Source lamp
Stray light mask
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Lamp mask Lamp lens
Selecting the appropriate sampling rate
The detector’s optics bench directs light as follows: •
Light from the source lamp is focused by the focusing lens through the aperture and collimating lens, forming 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 both sides of the flow cell and the collimating lens to the dual-element photodiode.
The difference in the amount of light striking the elements of the photodiode (because of sample refraction) results in a deflection from the baseline on the chromatogram.
Selecting the appropriate sampling rate A sufficient number of points must fall across a peak to define its shape. Thus, at very low sampling rates, the resolution between peaks is lost. Empower software uses the index of the data point closest to the end time, minus the index of the data point closest to the start time, to calculate the Points Across Peak value for each integrated peak in the chromatogram. Tip: The Points Across Peak value appears in the Peaks table, at the bottom of the Review Main window. If the Points Across Peak field is not visible, right-click anywhere in the table, and then click Table Properties. Click the Columns tab, and then scroll down to find the Points Across Peak field. Clear the check box, and then click OK. To maintain acceptable accuracy and precision, specify between 20 and 25 points across the narrowest peak. Increasing the sampling rate tends to increase baseline noise. For that reason, choose a sampling rate based on the signal-to-noise ratio (S/N) consistent with the precision requirements of the assay. For well behaved systems, the relative standard deviation (RSD), in percent, equals 50/(S/N). Thus for a signal-to-noise ratio of 100:1, the RSD would be approximately 0.5%.
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1 The ACQUITY Refractive Index Detector
Filtering noise The detector's digital, finite-impulse-response Hamming filter minimizes noise by degrading peak height and enhancing the filtering of high frequency noise. The filter’s performance depends on the filter time-constant you select. You can program a filter time to be fast, slow, normal, or other. If you select Fast, Slow, or Normal, you need not enter a value; the filter constant is determined by the sampling rate. If you select Other, you can enter a value. Note, however, that the value you enter is rounded up or down to a value based on the sampling rate. The filter time-constant adjusts the filter response time to achieve an optimal signal-to-noise ratio. Selecting Other and entering a value of 0.0 disables all filtering. Lower time-constant settings produce these effects: •
Remove less baseline noise
•
Produce narrow peaks, with minimal peak distortion and time delay
•
Make very small peaks harder to discern from baseline noise
Higher time-constant settings produce these effects: •
Greatly decrease baseline noise
•
Shorten and broaden peaks
The software includes fast or normal filtering constants at each sampling rate that are appropriate for high speed or high sensitivity applications, respectively.
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Polarity
The following figure shows the relationship between increased filter time-constant and absorbance.
Absorbance
Filter time-constant comparison
0 sec 1 sec 2 sec
Time (minutes)
Tip: Although the peak shape shows some distortion and the signal output is delayed with different time-constants, the peak area remains the same.
Polarity Detected peaks can be positive or negative. To obtain all positive peaks, you must configure and change the polarity of the detector signals through a timed event. Use the Polarity parameter to invert the sign of the RI data. A positive polarity leaves the data unaffected; a negative polarity essentially multiplies the value of each data point by –1, inverting the chromatogram. Polarity is specified in the instrument used for chromatographic runs. It can also be changed in the console or control panel but will be overridden by the method settings of the next run. Polarity can be thought of as a bimodal state (either positive or negative).
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1 The ACQUITY Refractive Index Detector
Temperature control The detector oven, which controls the temperature of the flow cell, has a temperature-setting range of 30 to 55 °C, settable to ±0.1 °C. The detector flow cell temperature reading is accessible via the console or control panel. The automatically resettable thermal limit switch protects the oven temperature from raising above the set point, cutting power to the heater when the thermal limit is exceeded, and displaying an error message. The switch resets when the oven temperature cools to a safe operating level. Note: A low ambient temperature can prevent the detector oven from attaining its set point.
Thermal equilibrium Allow the detector to reach thermal equilibrium before using it. Under typical operating conditions, the detector reaches equilibrium within a few hours, depending on the internal, column, and ambient temperatures. Recommendation: To avoid wasting solvent when equilibrating the detector, set the recycle valve to the recycle position. See also: For information about recycling solvent, consult the ACQUITY Console online Help.
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2
Preparing the detector Proper solvent selection and preparation are critical in differential refractometry to prevent baseline changes such as drift, noise, or an erratic baseline. Warning: To avoid back injuries, do not attempt to lift the detector without assistance. Contents: Topic
Page
Stacking the modules....................................................................... 38 Installing the leak sensor ................................................................ 39 Installation recommendations for fittings ...................................... 41 Connecting a column or second detector......................................... 42 Connecting to waste ......................................................................... 43 Making the recycle connection ........................................................ 44 Installing the multi-detector drip tray ........................................... 45 Making the Ethernet connection..................................................... 45 Making signal connections .............................................................. 45 Connecting to the electricity source ................................................ 48 Typical solvent problems ................................................................. 49 Selecting a solvent ........................................................................... 49 Solvent degassing............................................................................. 52
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2 Preparing the detector
Stacking the modules Warning: To avoid back injuries, do not attempt to lift the detector without assistance. To stack the modules: 1.
Place the rear feet of the detector atop the previously added module in the system stack, and slide it backward until its rear alignment pin rests in the rear alignment slot on the module.
Alignment pin (2)
Alignment slot (2)
38
2.
Lower the front of the detector so that its front alignment pin rests in the front alignment slot on the previously added module.
3.
Repeat step 1 and step 2 for the remaining system modules.
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Installing the leak sensor
Installing the leak sensor Warning: To avoid the harmful effects of personal contact with solvents, including inhalation, always wear chemical-resistant, powder-free gloves and observe Good Laboratory Practice when you handle them. See the Material Safety Data Sheets for the solvents you use. Warning: To avoid the harmful effects of personal contact with leaking solvents, flush the detector with an appropriate miscible solvent prior to performing this procedure. Warning: To avoid personal contamination with biohazards or compounds that are toxic, wear clean, chemical-resistant, powder-free gloves when performing this procedure.
Required materials •
Gloves: clean, powder-free, chemical-resistant
•
Leak sensor
To install the leak sensor: Caution: To avoid damaging the electronic components or circuitry of a system module, do not disconnect an electrical assembly from the module while the module remains connected to the ac supply source. Follow this procedure to completely interrupt power to the module: 1. Set the module’s power switch to Off. 2. Disconnect the module’s electrical supply cord from the ac source. Afterward, wait 10 seconds before disconnecting any assembly from the module. 1.
Power-off the detector.
2.
Open the detector door, gently pulling its right edge toward you.
3.
Carefully unpack the new leak sensor.
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2 Preparing the detector
4.
Align the leak sensor’s T-bar with the slot in the side of the leak sensor reservoir, and slide the leak sensor into place.
TP03559
T-bar Slot in leak sensor reservoir
5.
Plug the leak sensor connector into the port on the front of the detector. Leak sensor connector port on front of detector:
40
6.
Power-on the detector.
7.
In the console, select ACQUITY System from the system tree.
8.
Click Control > Leak sensors.
9.
Enable the detector leak sensor.
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Installation recommendations for fittings
Installation recommendations for fittings Warning: To avoid the harmful effects of personal contact with solvents, including inhalation, always wear chemical-resistant, powder-free gloves and observe Good Laboratory Practice when you handle them. See the Material Safety Data Sheets for the solvents you use. Warning: To avoid the harmful effects of personal contact with leaking solvents, flush the detector with an appropriate miscible solvent prior to installing or replacing fittings. Warning: To avoid personal contact with fittings contaminated with biohazards or toxic materials, wear clean, chemical-resistant, powder-free gloves when reinstalling the fittings. Note the diagram below for assembly orientation. Ferrule
Gold-plated compression screw
Tubing
Recommendations: •
To prevent bandspreading, ensure tubing fully bottoms in its fitting hole before tightening compression screws.
•
Perform dynamic leak test on the solvent manager whenever you replace or loosen fittings during maintenance (see the ACQUITY online Help).
•
Whenever you loosen fittings during maintenance, examine them for cracks, stripped threads, and deformations.
•
Do not reseat stainless steel ferrules more than six times.
Required material Gloves: clean, powder-free, chemical-resistant
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2 Preparing the detector
When tightening system fittings, consult the following table. Installation recommendations for detector fittings: Fitting
Recommended tightening
First use or reinstalled
Standard 1/16-inch fitting Gold-plated compression screw
Ferrule
Finger-tight, plus as much as an additional 1/4-turn 1/4-turn
Connecting a column or second detector Use only the insulating sample inlet tubing assembly supplied in the startup kit when connecting a column or second detector. This tubing assembly has been prepared with insulation sleeving to moderate the effect of ambient air temperature variations. Restriction: If a system includes more than one detector, you must connect the refractive index detector as the last detector in line. See page 45 for information about connecting the detector to the system via the detector’s signal cable. Required material Insulated sample inlet tubing assembly Required tool Open-end wrench, 5/16-inch
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Connecting to waste
To connect a column or other detector to the refractive index detector: 1.
Insert one end of the inlet tubing assembly into the inlet port of the refractive index detector. Important: Ensure the inlet tubing bottoms in the inlet port before tightening the gold-plated compression screw.
2.
Tighten the compression screw 1/4-turn past finger-tight.
3.
Repeat step 2, inserting the other end of the inlet tubing assembly into the outlet fitting of the column or another detector.
Connecting to waste Caution: To avoid damaging the flow cell, do not allow the maximum detector pressure to exceed 1000 kPa (10.0 bar, 145 psi). The detector’s flow cell is extremely sensitive to backpressure. Be sure to use the 0.030-inch ID waste tubing supplied, pre-installed, on the detector. Backpressure pulses from a dripping waste tube can cause short-term baseline cycling. To connect the detector to waste: 1.
Place the waste container lower than, or at the same level as, the detector.
2.
Place the free end of the waste tubing in the waste container.
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2 Preparing the detector
Location of waste tubing on recycle valve:
Location of waste tubing
Making the recycle connection To make the recycle connection: Place the free end of the recycle tubing in the solvent container. Note: If the recycle tubing was previously placed in the waste container, remove it from the waste container, and then place it in the solvent container.
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Installing the multi-detector drip tray
Location of recycle tubing on recycle valve:
Location of recycle tubing
Installing the multi-detector drip tray If your system has more than one detector, you must install the multi-detector drip tray. For information on how to install the multi-detector drip tray, refer to the instructions included in the multi-detector drip tray kit.
Making the Ethernet connection To make the Ethernet connection: Connect one end of one Ethernet cable to the detector, and then connect its other end to the network switch.
Making signal connections The rear panel of the detector includes a removable connector that holds the screw terminals for the optional I/O signal cables. This connector is keyed so that it can be inserted only one way. Refer to the signal connection location shown on the silk-screened label affixed to the rear panel of the detector.
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2 Preparing the detector
I/O signal connectors:
Inject Start + Inject Start Switch Switch Analog Out + Analog Out -
1 2 3 4 5 6
For electrical specifications, see Appendix B. Refractive index detector analog-out/event-in/event-out connections: Signal connection
Description
Inject Start
Indicates (with a contact closure output) that an injection has started.
Switch
Output switch to trigger external devices.
Analog Out
Analog data output.
Required materials •
Connector
•
Signal cable (optional, must be ordered separately)
Required tools
46
•
Nut driver, 9/32-inch
•
Flat-blade screwdriver
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Making signal connections
To make signal connections: 1.
Insert the connector into the connector port on the back of the detector. Connector port
Connector
2.
Using the flat-blade screwdriver, attach the positive and negative leads of the signal cable to the connector. Screw
Connector
Signal cable
3.
Fit the grounding cable’s fork terminal on the rear panel grounding stud, and secure the terminal with the locking nut.
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2 Preparing the detector
Tip: Use the 9/32-inch nut driver to tighten the locking nut until the fork terminal does not move. Fork terminal
Locking nut
Grounding stud
Connecting to the electricity source Each system module requires a separate, grounded power source. The ground connection in all power outlets must be common and physically close to the system. Warning: To avoid electric shock, observe these precautions, • use only the power cord provided when the system module was installed; • power-off and unplug the detector before performing any maintenance operation on it; • connect each system module to a common ground. To connect to the electricity source: Recommendation: Use a line conditioner and an uninterruptible power supply (UPS) for optimum, long-term, input voltage stability. 1.
48
Connect the female end of the power cord to the receptacle on the rear panel of the detector.
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Typical solvent problems
2.
Connect the male end of the power cord to a suitable wall outlet. Alternative: If the system includes the optional FlexCart, ensure the detector is powered off. Connect the female end of the cart's power supply cable (included in the startup kit) to the receptacle on the rear panel of the detector.
Typical solvent problems The ACQUITY refractive index (RI) detector measures changes in the RI of the solution flowing through the sample side of the flow cell. Yet conditions other than the presence of dissolved sample molecules can affect a solution’s RI: •
Changes in temperature
•
Changes in pressure
•
Contaminants
•
Separation of mixed solvents
•
Changes in dissolved gas content
Selecting a solvent An ideal solvent for an analysis demonstrates these characteristics: •
Good solubility characteristics for the intended application
•
Significantly different RI than the sample components
•
Satisfactory baseline noise performance
•
Optimum optical sensitivity characteristics
Solvent quality Use MS-grade solvents for the best possible results; the minimum requirement is HPLC-grade. Filter solvents through an appropriate membrane. Recommendation: Ensure solvent choices are consistent with the recommendations of the membrane filter manufacturer or supplier.
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2 Preparing the detector
A dirty or impure solvent can cause these problems: •
Baseline noise and drift
•
Plugged columns
•
Blockages in the fluid path
Preparation checklist The following solvent preparation guidelines help to ensure stable baselines and good resolution: •
Filtering solvents with a 0.22-μm filter.
•
Degassing the solvent.
•
Stirring the solvent.
•
Protecting solvents from drafts and shock.
Tip: For maximum sensitivity, use the same solvent to prime all solvent lines on the binary solvent manager or quaternary solvent manager.
Water Use water only from a high-quality water purification system. If the water system does not provide filtered water, filter it through a 0.22-μm membrane filter before use. Caution: To prevent microbial growth in systems using 100% water, change the water every third day.
Buffers When you use buffers, dissolve salts first, adjust the pH, and then filter to remove undissolved material.
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Selecting a solvent
Tetrahydrofuran (THF) When you use unstabilized THF, ensure that it is fresh. Previously opened containers of THF contain peroxide contaminants, which cause baseline drift. Warning: To avoid an explosion caused by unstable contaminants (peroxides) in THF, do not evaporate or otherwise concentrate THF to a state approaching dessication.
Refractive indices of common solvents The following table lists the refractive indices for some common chromatographic solvents. Consulting this table, verify that the solvent you intend to use for an analysis has an RI significantly different from the sample components. Refractive indices of common solvents: Solvent
RI
Solvent
RI
Fluoroalkanes
1.25
Tetrahydrofuran (THF)
1.408
Hexafluoroisopropanol (HFIP)
1.2752
Amyl alcohol
1.410
Methanol
1.329
Diisobutylene
1.411
Water
1.33
n-Decane
1.412
Acetonitrile
1.344
Amyl chloride
1.413
Ethyl ether
1.353
Dioxane
1.422
n-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)
1.428
Ethyl acetate
1.370
N,N-dimethyl acetamide 1.438 (DMAC)
1-Pentene
1.371
Ethyl sulfide
1.442
Acetic acid
1.372
Chloroform
1.443
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2 Preparing the detector
Refractive indices of common solvents: (Continued) Solvent
RI
Solvent
RI
Isopropyl chloride
1.378
Ethylene dichloride
1.445
Isopropanol
1.38
Carbon tetrachloride
1.466
n-Propanol
1.38
Dimethyl sulfoxide (DMSO)
1.477
Methylethylketone
1.381
Toluene
1.496
Diethyl amine
1.387
Xylene
~1.50
n-Propyl chloride
1.389
Benzene
1.501
Methylisobutylketone
1.394
Pyridine
1.510
Nitromethane
1.394
Chlorobenzene
1.525
1-Nitropropane
1.400
o-Chlorophenol
1.547
Isooctane
1.404
Aniline
1.586
Cyclopentane
1.406
Carbon disulfide
1.626
Solvent degassing Using degassed solvents is the most important step in solvent preparation. Degassing provides these benefits: •
Stable baselines and enhanced sensitivity
•
Reproducible retention times
•
Stable pump or solvent delivery system operation
Gas solubility The amount of gas that can dissolve in a given volume of liquid depends on these factors: •
The chemical affinity of the gas for the liquid
•
The temperature of the liquid
•
The pressure applied to the liquid
Changes in the composition, temperature, or pressure of the mobile phase can lead to changes in dissolved gas content.
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Solvent degassing
Effects of intermolecular forces Nonpolar gases (N2, O2, CO2, He) are more soluble in nonpolar solvents than in polar solvents. Generally, a gas is most soluble in a solvent with intermolecular attractive forces similar to those in the gas (“like dissolves like”).
Effects of temperature Temperature affects the solubility of gases. If the dissolution is exothermic, the solubility of the gas decreases when you heat the solvent. If the dissolution is endothermic, the solubility increases when you heat the solvent. For example, the solubility of He in H2O decreases with an increase in temperature, but the solubility of He in benzene increases with an increase in temperature.
Effects of partial pressure The mass of gas dissolved in a given volume of solvent is proportional to the partial pressure of the gas in the vapor phase of the solvent. If you decrease the partial pressure of the gas, the amount of that gas in solution also decreases.
Solvent degassing methods Solvent degassing helps you attain a stable baseline and also improves reproducibility and pump performance. There are two common methods used to degas solvents: •
Reducing pressure by vacuum
•
Sonication
You can use these methods individually or in combination.
Vacuum degassing To remove dissolved gasses from the solvent, the in-line vacuum degasser relies on the principle of Henry’s law, which states that the mole fraction of a gas dissolved in liquid is proportional to the partial pressure of that gas in the vapor phase above the liquid. If the partial pressure of a gas on the surface of the liquid is reduced, for example, by evacuation, then a proportional amount of that gas comes out of solution.
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Note: Vacuum degassing can possibly change the composition of mixed solvents.
Sonication Sonication with high-energy sound waves drives energy into the solvent and causes the submicron-sized “bubbles” of gas to aggregate. As the gas bubbles aggregate, they become large enough to float out of the solvent and dissipate. Sonication alone degasses 4 liters of solvent in approximately 20 minutes.
Solvent degassing considerations Select the most efficient degassing operation for the application.
Vacuum degassing The longer a solvent is exposed to vacuum, the more dissolved gases are removed. Two factors affect the amount of time the solvent is exposed to the vacuum. Factors affecting time solvent is exposed to the vacuum: Factor
Effect
Flow rate
At low flow rates, most of the dissolved gas is removed 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 membrane is fixed in each vacuum chamber. To increase the length of membrane, you can connect two or more vacuum chambers in series.
Sonication plus vacuum Sonication combined with vacuum degasses solvent very quickly. This technique is less likely to change the composition of mixed solvents because the mixed solvents are held under vacuum for only a short time (less than a minute is usually sufficient).
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Solvent degassing
Warning: To avoid injury from flying glass fragments, do not apply vacuum to the brown glass bottles in which solvent is shipped. Doing so creates a high risk of implosion. Use a thick-walled container designed for vacuum applications.
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3
Using the detector Contents: Topic
Page
Starting the detector........................................................................ 58 Resolving leak sensor errors............................................................ 63 Shutting down the detector ............................................................. 66
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3 Using the detector
Starting the detector Starting the ACQUITY refractive index detector entails powering-on the detector and each system module individually, as well as the ACQUITY workstation. It also entails starting the operating software (Empower). To start the detector: 1.
Power-on the workstation.
2.
Press the power switch on the top, left-hand side of the solvent manager door, sample manager door, column manager (if included in the system), and RI detector door. Result: Each system module “beeps” and runs a series of startup tests. The power and run LEDs change as follows:
3.
•
Each system module’s power LED shows green.
•
During initialization, each system module’s status (or run) LED flashes green.
•
After the modules are successfully powered-on, all LEDs show steady green. The solvent manager’s flow LED and the sample manager’s run LED remain unlit.
Start Empower software. Tip: You can monitor the ACQUITY console for messages and LED indications.
4.
Flush all flowpaths of the detector including the Purge and Recycle flowpaths. Tip: For maximum sensitivity, use the same solvent to prime all solvent lines on the binary solvent manager or quaternary solvent manager. See also: For information about purging the detector and recycling solvent, consult the ACQUITY Console online Help.
Note that it can take several hours for the optics bench to stabilize at a new temperature. Do not make a run until the temperature stabilizes. Changing temperature causes baseline drift and can necessitate lamp reoptimization. Note: A low ambient temperature can prevent the detector’s oven from attaining its set point.
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Recommendation: To avoid wasting solvent when equilibrating the detector, set the recycle valve to the recycle position.
Monitoring detector LEDs Light emitting diodes on the detector indicate its state of functioning.
Power LED The power LED, to the left-hand side of the detector’s front panel, indicates when the detector is powered-on or powered-off.
Run LED The run LED, to the right of the power LED, indicates the detector status. Run LED indications: LED mode and color
Description
Unlit
If both run and power LED are unlit, the detector is powered off. If run LED is unlit and power LED is constant green, the detector is in idle mode.
Blinking green
Detector is initializing or attempting to reach the flow cell set temperature.
Constant green
Detector is running and collecting data as part of a chromatography run.
Blinking red
Detector is in error mode.
Solid red
Detector is in error mode that requires service.
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3 Using the detector
About the detector control panel The detector’s control panel appears at the bottom of the Sample Set Editor page. Detector control panel: Run LED
Status
Recycle indicator Current flow cell temperature
Detector signal
Set flow cell temperature
The detector control panel displays the detector status, set and current flow cell temperatures, detector signal, polarity, and recycle status. You cannot edit detector parameters while the system is processing samples. The following table lists the items in the detector control panel. Modifiable detector control panel items:
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Control panel item
Description
Set flow cell temperature
Displays the set flow cell temperature.
Polarity
Displays the detector polarity.
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Starting the detector
Non-modifiable detector control panel items: Control panel item
Description
Status
Displays the status of the current operation. (Appears only if the detector is running.) Status can be: • Initializing • Getting Ready • Ready • Running • Purging • Error
Detector signal
Displays the detector signal measured in microrefractive index units (μRIU).
Current flow cell temperature
Displays the current flow cell temperature.
Run LED
Displays status of the run state (Initializing, Idle/Ready, Running) on the front panel of the detector.
Recycle icon
Appears whenever “Recycle” is enabled. Icon not visible when valve is in the “Waste” position.
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3 Using the detector
You can access additional functions by right-clicking anywhere in the detector control panel. Additional functions in the detector control panel:
62
Control panel function
Description
Auto zero
Sets the signal output to zero immediately.
Purge
Starts or ends the reference flow cell purging function. See also: For information about purging the detector, consult the ACQUITY Console online Help.
Set recycle valve
Starts or ends the solvent recycling function. See also: For information about recycling solvent, consult the ACQUITY Console online Help.
Reset RI
Resets the detector, when present, after an error condition.
Help
Displays the online Help for the console software.
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Resolving leak sensor errors
Resolving leak sensor errors After approximately 1.5 mL of liquid accumulates in the leak sensor reservoir, an alarm sounds indicating that the leak sensor detected a leak. Warning: To avoid the harmful effects of personal contact with solvents, including inhalation, always wear chemical-resistant, powder-free gloves and observe Good Laboratory Practice when you handle them. See the Material Safety Data Sheets for the solvents you use. Warning: To avoid the harmful effects of personal contact with leaking solvents, flush the detector with an appropriate miscible solvent prior to performing this procedure. Warning: To avoid personal contamination with biohazards or compounds that are toxic, wear clean, chemical-resistant, powder-free gloves when handling the leak sensor. To avoid spreading contamination, do not allow contaminated gloves to come in contact with uncontaminated surfaces, and discard gloves immediately on completing the procedure. Caution: To avoid scratching or damaging the leak sensor, • do not allow buffered solvents to accumulate and dry on it; • submerge only the prism in a cleaning bath.
Required materials •
Cotton swabs
•
Gloves: clean, powder-free, chemical-resistant
•
Nonabrasive, lint-free wipes
To resolve a leak sensor error: 1.
View the Leak Sensors dialog box in the ACQUITY Console to verify that a message stating “Leak Detected” appears, indicating that the leak sensor detected a leak.
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3 Using the detector
Caution: To avoid damaging the electronic components or circuitry of a system module, do not disconnect an electrical assembly from the module while the module remains connected to the ac supply source. Follow this procedure to completely interrupt power to the module: 1. Set the module’s power switch to Off. 2. Disconnect the module’s electrical supply cord from the ac source. Afterward, wait 10 seconds before disconnecting any assembly from the module. 2.
Power-off the refractive index detector.
3.
Open the refractive index detector’s door, gently pulling its right-hand edge toward you.
4.
Locate the source of the leak, if external to the unit, and make the repairs necessary to stop the leak.
5.
Remove the leak sensor from its reservoir, holding it by its serrations and pulling upward. Leak sensor:
Serrations
Tip: If you cannot easily manipulate the leak sensor after removing it from its reservoir, detach the connector from the front of the device (see page 76).
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Resolving leak sensor errors
6.
Use a nonabrasive, lint-free wipe to dry the leak sensor prism.
Prism Lint-free wipe TP03562
7.
Roll up a nonabrasive, lint-free wipe, and use it to absorb the liquid from the leak sensor reservoir and its surrounding area.
Rolled up lint-free wipe Leak sensor reservoir TP03561
8.
With a cotton swab, absorb any remaining liquid from the corners of the leak sensor reservoir and its surrounding area.
Cotton swab Leak sensor reservoir
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3 Using the detector
9.
Align the leak sensor’s T-bar with the slot in the side of the leak sensor reservoir, and slide the leak sensor into place.
TP03559
T-bar Slot in leak sensor reservoir
10. Plug the leak sensor connector into the port on the front of the detector. 11. If you detached the connector from the front of the detector, reattach it. Leak sensor connector port on front of detector:
12. Power-on the detector.
Shutting down the detector Recommendations:
66
•
Do not power-off the detector unless you are storing it.
•
If the detector will be idle for an extended period, remove water and buffered mobile phase from the fluid path, to prevent bacterial growth. Flush all flow paths with 100% organic solution.
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Shutting down the detector
If you are not running the detector for less than 24 hours, set the flow rate to 0.1 mL/min, and keep the solvent manager operating to minimize the amount of time the detector needs for reequilibration when you use it again. To shut down the detector for more than 24 hours: 1.
Flush all flow paths with 100% organic solution.
2.
Stop the solvent flow to the solvent manager.
3.
Power-off the detector.
Removing buffered mobile phase To remove mobile phase from the fluid path of the detector: 1.
Replace the buffered mobile phase with 100% HPLC-quality water and flush the system for 10 minutes at 2 mL/min. Important: If the storage solvent is incompatible with the column, remove the column before flushing.
2.
Replace the 100% water mobile phase with a 100% organic solution, and flush the system for 10 minutes at 2 mL/min.
Follow the recommended procedures for injector purging and priming for the pump used with the ACQUITY system. Power-off any peripheral devices before shutting down the detector. To power-off the detector, press the power switch on the top, left side of the detector door.
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4
Maintenance Procedures Keep to a maintenance schedule, and perform maintenance procedures as required and described in this chapter. Contents: Topic
Page
Maintaining the detector ................................................................. 70 Spare parts ....................................................................................... 72 Troubleshooting with Connections INSIGHT ................................ 72 Safety and handling ......................................................................... 74 Replacing the leak sensor ................................................................ 75 Decontaminating the fluid path ...................................................... 77 Cleaning the refractive index detector’s exterior ........................... 79
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4 Maintenance Procedures
Maintaining the detector Perform the procedures in this section when you discover a problem with a detector component or during routine maintenance. For information about isolating such problems, consult the ACQUITY Console online Help.
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). From elsewhere, phone the Waters corporate headquarters in Milford, Massachusetts (USA), or contact the local Waters subsidiary. The Waters web site includes phone numbers and e-mail addresses for Waters locations worldwide. Visit www.waters.com. When you contact Waters, be prepared to provide this information: •
Error message (if any)
•
Nature of the symptom
•
Serial number of the system module and its firmware version, if applicable
•
Flow rate
•
Operating pressure
•
Solvent(s)
•
Detector settings (flow cell temperatures, detector signal, polarity, and recycle status)
•
Type and serial number of column(s)
•
Sample type and diluent
•
Data software version and serial number
•
ACQUITY workstation model and operating system version
For complete information about reporting shipping damages and submitting claims, see Waters Licenses, Warranties, and Support Services documentation.
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Maintaining the detector
Locating system serial numbers The serial number on the system’s modules facilitates service and support. Serial numbers also provide a way to create single log entries for each module, so that you can review the usage history of a particular module. Be prepared to provide the serial numbers of the instruments or devices in the system when you contact Waters customer support. To view the information for a system module: 1.
In the ACQUITY Console, select a module from the system tree.
2.
Click Configure > View module information. Result: The Module Information dialog box displays this information: •
Serial number
•
Firmware version
•
Firmware checksum
•
Component software version
Alternatives: •
From the main window, place the pointer over the visual representation of the system module for which you want to view information.
•
Obtain the serial number from the printed labels affixed to the rear panels of system modules or inside their front doors.
Maintenance schedule Perform the following routine maintenance on the refractive index detector to ensure reliable operation and accurate results. When using the system throughout the day (and on nights and weekends), or when using aggressive solvents, such as buffers, perform the maintenance tasks more frequently.
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4 Maintenance Procedures
Recommended routine maintenance schedule: Maintenance procedure
Frequency
For information...
Replace the leak sensor
As needed
See page 75.
Decontaminating the fluid path
As needed
See page 77.
Clean the device’s exterior with a soft, lint-free cloth, or paper dampened with water
As needed
See page 79.
Configuring maintenance warnings Maintenance counters provide real-time usage status information that can help you determine when to schedule routine maintenance for specific components. You can set usage thresholds and maintenance warnings that alert you when a component reaches the designated threshold limit. By setting threshold limits and monitoring these usage counters regularly, you can minimize unexpected failures and unscheduled downtime during important work. For information on setting maintenance warnings, consult the ACQUITY Console online Help.
Spare parts ®
To ensure that a system operates as designed, use only Waters Quality Parts . Visit www.waters.com/wqp for information about Waters Quality Parts, including how to order them.
Troubleshooting with Connections INSIGHT ®
Connections INSIGHT is an “intelligent” device management (IDM) Web service that enables Waters to provide proactive service and support for the ACQUITY system. In a client/server system, you must also install the service agent, on the computer from which you control the system. The service agent software automatically and securely captures and sends information about the support needs of the system directly to Waters. If you encounter a performance issue when using the console software, you can manually submit a Connections INSIGHT request to Waters customer
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Troubleshooting with Connections INSIGHT
support. Alternatively, you can use Remote Desktop, a real-time collaboration option that controls the two-way connection with the ACQUITY system by enabling the Connections INSIGHT iAssist service level. Consult these sources for more information about Connections INSIGHT and Connections INSIGHT iAssist: •
http://www.waters.com
•
Connections INSIGHT Installation Guide (part number 715001399)
•
Connections INSIGHT User's Guide (part number 715001400)
•
Your sales representative
•
Your local Waters subsidiary
•
Waters Customer Support
To submit a Connections INSIGHT request: 1.
Select Troubleshoot > Submit Connections INSIGHT request.
2.
In the Connections INSIGHT Request dialog box, type your name, telephone number, e-mail address, and a description of the problem.
3.
Click Submit, and allow approximately 5 minutes to save the service profile. Result: A .zip file containing your Connections INSIGHT profile is forwarded to Waters customer support for review. Tip: Saving a service profile or plot file from the Instrument Console can require as much as 150 MB of file space.
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Safety and handling Bear in mind these advisories when you perform maintenance operations on the system. Warning: To avoid personal contamination with biohazards or compounds that are toxic, wear clean, chemical-resistant, powder-free gloves when handling components. Warning: To avoid the harmful effects of personal contact with solvents, including inhalation, always wear chemical-resistant, powder-free gloves and observe Good Laboratory Practice when you handle them. See the Material Safety Data Sheets for the solvents you use. Warning: To avoid electric shock, do not remove protective panels from the refractive index detector. The panels cover components that are serviceable only by Waters technicians. Caution: To avoid damaging the electronic components or circuitry of a system module, do not disconnect an electrical assembly from the module while the module remains connected to the ac supply source. Follow this procedure to completely interrupt power to the module: 1. Set the module’s power switch to Off. 2. Disconnect the module’s electrical supply cord from the ac source. Afterward, wait 10 seconds before disconnecting any assembly from the module. See Appendix A for safety advisory information.
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Replacing the leak sensor
Replacing the leak sensor Warning: To avoid the harmful effects of personal contact with solvents, including inhalation, always wear chemical-resistant, powder-free gloves and observe Good Laboratory Practice when you handle them. See the Material Safety Data Sheets for the solvents you use. Warning: To avoid the harmful effects of personal contact with leaking solvents, flush the detector with an appropriate miscible solvent prior to performing this procedure. Warning: To avoid personal contamination with biohazards or compounds that are toxic, wear clean, chemical-resistant, powder-free gloves when handling the leak sensor. To avoid spreading contamination, do not allow contaminated gloves to come in contact with uncontaminated surfaces, and discard gloves immediately on completing the procedure.
Required materials •
Gloves: clean, powder-free, chemical-resistant
•
Leak sensor
To replace the leak sensor: 1.
Power-off the refractive index detector.
2.
Open the refractive index detector’s door, gently pulling its right-hand edge toward you.
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4 Maintenance Procedures
Caution: To avoid damaging the electronic components or circuitry of a system module, do not disconnect an electrical assembly from the module while the module remains connected to the ac supply source. Follow this procedure to completely interrupt power to the module: 1. Set the module’s power switch to Off. 2. Disconnect the module’s electrical supply cord from the ac source. Afterward, wait 10 seconds before disconnecting any assembly from the module. 3.
Press down on the tab, to detach the leak sensor connector from the front of the device. Leak sensor connector
Press down on tab to release connector
4.
Remove the leak sensor from its reservoir, holding it by its serrations and pulling upward. Leak sensor:
Serrations
5.
76
Unpack the new leak sensor.
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Decontaminating the fluid path
6.
Align the leak sensor’s T-bar with the slot in the side of the leak sensor reservoir, and slide the leak sensor into place.
TP03559
T-bar Slot in leak sensor reservoir
7.
Plug the leak sensor connector into the port on the front of the detector. Leak sensor connector port on front of detector:
8.
Power-on the refractive index detector.
Decontaminating the fluid path 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, below, to decontaminate it. Required materials •
A wrench suitable for removing and replacing the column
•
A solvent miscible in both the mobile phase and water (methanol is commonly used)
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4 Maintenance Procedures
•
HPLC-grade water
•
A strong cleaning solvent suitable for the system and application (6N nitric acid is used frequently)
•
A separate waste container for acid waste
•
If you use an acid as a cleaning solvent, a means of measuring the pH of the acid effluent Caution: If you use 6N nitric acid and operate the detector at high sensitivities, flush the system extensively with water to remove all traces of the acid.
To decontaminate the fluid path: Note: Strictly adhere to the following procedure. 1.
Stop the solvent manager, and replace the column with a union.
2.
Replace the mobile phase with an intermediary solvent miscible in both the current solvent and water.
3.
Restart the solvent manager, and then set the flow rate to 1 mL/min, maintaining the purge for at least 10 minutes. See also: For information about purging the detector, consult the ACQUITY Console online Help.
4.
Set the detector to purge mode for approximately 10 minutes, and run for an additional 10 minutes in normal mode.
5.
Switch the solvent manager to HPLC-grade water, and flush the detector for 10 minutes. Recommendation: Provide a separate, clean, waste container for the cleaning solution. Do not allow organic waste to mix with acid waste.
78
6.
Switch the solvent manager to the cleaning solvent, and flush the detector for 10 minutes.
7.
Switch the solvent manager back to HPLC-grade water and flush until the pH of the waste effluent is neutral (a pH value of 6.0 to 7.0).
8.
Switch the solvent manager back to the water-miscible intermediate solvent, and flush for 10 minutes.
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Cleaning the refractive index detector’s exterior
9.
Switch the solvent manager back to the mobile phase, and flush for 5 minutes.
10. Take the detector out of purge mode and stop the pump or solvent delivery system. 11. Reattach the column and reequilibrate the detector.
Cleaning the refractive index detector’s exterior Clean surfaces of the detector using only a clean, soft, lint-free paper or clean cloth dampened with water. Warning: To avoid electric shock, observe these precautions: • Disconnect the device or instrument from the electrical supply. • When cleaning the surface of a device or instrument, apply water to a cloth, and then wipe the unit. Do not spray or otherwise directly apply water to any device surface. Warning: To avoid personal injury, use eye and hand protection during the cleaning process.
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4 Maintenance Procedures
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Warning symbols
A
Safety Advisories Waters instruments display hazard symbols designed to alert you to the hidden dangers of operating and maintaining the instruments. Their corresponding user guides 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 to the entire line of Waters products. Contents: Topic
Page
Warning symbols.............................................................................. 81 Caution advisory .............................................................................. 84 Warnings that apply to all Waters instruments and devices ........ 85 Electrical and handling symbols ..................................................... 90
Warning symbols Warning symbols alert you to the risk of death, injury, or seriously adverse physiological reactions associated with an instrument’s use or misuse. Heed all warnings when you install, repair, and operate Waters instruments. Waters assumes no liability for the failure of those who install, repair, or operate its instruments to comply with any safety precaution.
Task-specific hazard warnings The following warning symbols alert you to risks that can arise when you operate or maintain an instrument or instrument component. Such risks 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 specific risk and explains how to avoid it.
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A Safety Advisories
Warning: (General risk of danger. When this symbol appears on an instrument, consult the instrument’s user documentation for important safety-related information before you use the instrument.) Warning: (Risk of burn injury from contacting hot surfaces.) Warning: (Risk of electric shock.) Warning: (Risk of fire.) Warning: (Risk of sharp-point puncture injury.) Warning: (Risk of hand crush injury.) Warning: (Risk of injury caused by moving machinery.) 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.) Warning: (Risk of explosion.) Warning: (Risk of eye injury.)
Specific warnings The following warnings can appear in the user manuals of particular instruments and on labels affixed to them or their component parts.
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Warning symbols
Burst warning This warning applies to Waters instruments fitted with nonmetallic tubing. Warning: Pressurized nonmetallic, or polymer, tubing can burst. Observe these precautions when working around such tubing: • Wear eye protection. • 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 acids. • Be aware that some compounds, like methylene chloride and dimethyl sulfoxide, can cause nonmetallic tubing to swell, which significantly reduces the pressure at which the tubing can rupture.
Biohazard warning This warning applies to Waters instruments that can be used to process material that can contain biohazards: substances that contain biological agents capable of producing harmful effects in humans. Warning: Waters instruments and software can be used to analyze or process potentially infectious human-sourced products, inactivated microorganisms, and other biological materials. To avoid infection with these agents, assume that all biological fluids are infectious, observe Good Laboratory Practice, and consult your organization’s biohazard safety representative regarding their proper use and handling. Specific precautions appear in the latest edition of the US National Institutes of Health (NIH) publication, Biosafety in Microbiological and Biomedical Laboratories (BMBL).
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Chemical hazard warning This warning applies to Waters instruments that can process corrosive, toxic, flammable, or other types of hazardous material. Warning: Waters instruments can be used to analyze or process potentially hazardous substances. To avoid injury with any of these materials, familiarize yourself with the materials and their hazards, observe Good Laboratory Practice (GLP), and consult your organization’s safety representative regarding proper use and handling. Guidelines are provided in the latest edition of the National Research Council's publication, Prudent Practices in the Laboratory: Handling and Disposal of Chemicals.
Caution advisory Caution advisories appear where an instrument or device can be subject to use or misuse capable of damaging it or compromising a sample’s integrity. The exclamation point symbol and its associated statement alert you to such risk. Caution: To avoid damaging the instrument’s case, do not clean it with abrasives or solvents.
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Warnings that apply to all Waters instruments and devices
Warnings that apply to all Waters instruments and devices When operating this device, follow standard quality-control procedures and the equipment guidelines in this section. Attention: Changes or modifications to this unit not expressly approved by the party responsible for compliance could void the user’s authority to operate the equipment. Important: Toute modification sur cette unité n’ayant pas été expressément approuvée par l’autorité responsable de la conformité à la réglementation peut annuler le droit de l’utilisateur à exploiter l’équipement. Achtung: Jedwede Änderungen oder Modifikationen an dem Gerät ohne die ausdrückliche Genehmigung der für die ordnungsgemäße Funktionstüchtigkeit verantwortlichen Personen kann zum Entzug der Bedienungsbefugnis des Systems führen. Avvertenza: qualsiasi modifica o alterazione apportata a questa unità e non espressamente autorizzata dai responsabili per la conformità fa decadere il diritto all'utilizzo dell'apparecchiatura da parte dell'utente. Atencion: 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. 注意：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。 注意：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。 주의: 규정 준수를 책임지는 당사자의 명백한 승인 없이 이 장치를 개조 또는 변경할 경우, 이 장치를 운용할 수 있는 사용자 권한의 효력을 상실할 수 있습니다. 注意：規制機関から明確な承認を受けずに本装置の変更や改造を行うと、本装置のユー ザーとしての承認が無効になる可能性があります。
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A Safety Advisories
Warning: Use caution when working with any polymer tubing under pressure: • Always wear eye protection when near pressurized polymer tubing. • Extinguish all nearby flames. • Do not use tubing that has been severely stressed or kinked. • Do not use nonmetallic tubing with tetrahydrofuran (THF) or concentrated nitric or sulfuric acids. • Be aware that methylene chloride and dimethyl sulfoxide cause nonmetallic tubing to swell, which greatly reduces the rupture pressure of the tubing. Attention: Manipulez les tubes en polymère sous pression avec precaution: • Portez systématiquement des lunettes de protection lorsque vous vous trouvez à proximité de tubes en polymère pressurisés. • Eteignez toute flamme se trouvant à proximité de l’instrument. • Evitez d'utiliser des tubes sévèrement déformés ou endommagés. • Evitez d'utiliser des tubes non métalliques avec du tétrahydrofurane (THF) ou de l'acide sulfurique ou nitrique concentré. • Sachez que le chlorure de méthylène et le diméthylesulfoxyde entraînent le gonflement des tuyaux non métalliques, ce qui réduit considérablement leur pression de rupture. Vorsicht: 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. • Nichtmetallische Schläuche nicht für Tetrahydrofuran (THF) oder konzentrierte Salpeter- oder Schwefelsäure verwenden. • Durch Methylenchlorid und Dimethylsulfoxid können nichtmetallische Schläuche quellen; dadurch wird der Berstdruck des Schlauches erheblich reduziert.
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Warnings that apply to all Waters instruments and devices
Attenzione: fare attenzione quando si utilizzano tubi in materiale polimerico sotto pressione: • Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero pressurizzati. • Spegnere tutte le fiamme vive nell'ambiente circostante. • Non utilizzare tubi eccessivamente logorati o piegati. • Non utilizzare tubi non metallici con tetraidrofurano (THF) o acido solforico o nitrico concentrati. • Tenere presente che il cloruro di metilene e il dimetilsolfossido provocano rigonfiamenti nei tubi non metallici, riducendo notevolmente la pressione di rottura dei tubi stessi. Advertencia: se recomienda precaución cuando se trabaje con tubos de polímero sometidos a presión: • El usuario deberá protegerse siempre los ojos cuando trabaje cerca de tubos de polímero sometidos a presión. • Si hubiera alguna llama las proximidades. • No se debe trabajar con tubos que se hayan doblado o sometido a altas presiones. • Es necesario utilizar tubos de metal cuando se trabaje con tetrahidrofurano (THF) o ácidos nítrico o sulfúrico concentrados. • Hay que tener en cuenta que el cloruro de metileno y el sulfóxido de dimetilo dilatan los tubos no metálicos, lo que reduce la presión de ruptura de los tubos. 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。
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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。 경고: 가압 폴리머 튜브로 작업할 경우에는 주의하십시오. • 가압 폴리머 튜브 근처에서는 항상 보호 안경을 착용하십시오. • 근처의 화기를 모두 끄십시오. • 심하게 변형되거나 꼬인 튜브는 사용하지 마십시오. • 비금속(Nonmetallic) 튜브를 테트라히드로푸란(Tetrahydrofuran: THF) 또는 농축 질산 또는 황산과 함께 사용하지 마십시오. • 염화 메틸렌(Methylene chloride) 및 디메틸술폭시드(Dimethyl sulfoxide)는 비금속 튜브를 부풀려 튜브의 파열 압력을 크게 감소시킬 수 있으므로 유의하십시오. 警告：圧力のかかったポリマーチューブを扱うときは、注意してください。 • 加圧されたポリマーチューブの付近では、必ず保護メガネを着用してください。 • 近くにある火を消してください。 • 著しく変形した、または折れ曲がったチューブは使用しないでください。 • 非金属チューブには、テトラヒドロフラン(THF)や高濃度の硝酸または硫酸などを流 さないでください。 • 塩化メチレンやジメチルスルホキシドは、非金属チューブの膨張を引き起こす場合が あり、その場合、チューブは極めて低い圧力で破裂します。
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Warnings that apply to all Waters instruments and devices
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. Attention: 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. Vorsicht: Der Benutzer wird darauf aufmerksam gemacht, dass bei unsachgemäßer Verwenddung des Gerätes die eingebauten Sicherheitseinrichtungen unter Umständen nicht ordnungsgemäß funktionieren. Attenzione: si rende noto all'utente che l'eventuale utilizzo dell'apparecchiatura secondo modalità non previste dal produttore può compromettere la protezione offerta dall'apparecchiatura. Advertencia: el usuario deberá saber que si el equipo se utiliza de forma distinta a la especificada por el fabricante, las medidas de protección del equipo podrían ser insuficientes. 警告：使用者必須非常清楚如果設備不是按照製造廠商指定的方式使用，那麼該設備所提供 的保護將被消弱。 警告：使用者必须非常清楚如果设备不是按照制造厂商指定的方式使用，那么该设备所提供 的保护将被削弱。 경고: 제조업체가 명시하지 않은 방식으로 장비를 사용할 경우 장비가 제공하는 보호 수단이 제대로 작동하지 않을 수 있다는 점을 사용자에게 반드시 인식시켜야 합니다. 警告： ユーザーは、製造元により指定されていない方法で機器を使用すると、機器が提供 している保証が無効になる可能性があることに注意して下さい。
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Electrical and handling symbols Electrical symbols These 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
Frame, or chassis, terminal Fuse
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Electrical and handling symbols
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!
Fragile!
Use no hooks!
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Physical specifications
B
Specifications The specifications presented in this document depend on the conditions in individual laboratories. Refer to the site preparation guide or contact ® Waters Technical Service for more information on specifications. Contents: Topic
Page
Physical specifications ..................................................................... 93 Environmental specifications .......................................................... 94 Electrical specifications ................................................................... 94 Input/output specifications.............................................................. 95 Performance specifications .............................................................. 95 Wetted materials of construction .................................................... 97
Physical specifications Warning: To avoid back injuries, do not attempt to lift the detector without assistance. The following table lists the physical specifications for the ACQUITY refractive index detector. Physical specifications: Attribute
Specification
Height
20.8 cm (8.2 inches)
Width
34.3 cm (13.5 inches)
Depth
61.0 cm (24.0 inches)
Weight
15.4 kg (34.0 pounds)
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B Specifications
Environmental specifications The following table lists the environmental specifications for the ACQUITY refractive index detector. Environmental specifications: Attribute
Specification
Operating temperature
15 to 40 °C (59 to 104 °F)
Operating humidity
20 to 80%, noncondensing
Shipping and storage temperature
−30 to 60 °C (−40 to 140 °F)
Shipping and storage humidity
10 to 85%, noncondensing
Electrical specifications The following table lists the electrical specifications for the ACQUITY refractive index detector. Electrical specifications: Attribute
Specification
Protection classa
Class I b
Overvoltage category
II
Pollution degree
2
Moisture protectiond
Normal (IPXO)
c
Line voltages, nominal
Grounded ac
Voltage range
100 to 240 Vac
Frequency
50 to 60 Hz
Maximum power draw
145 VA
Fusing
3.15 A, fast acting
a. Protection Class I – The insulating scheme used in the instrument to protect from electrical shock. Class I identifies a single level of insulation between live parts (wires) and exposed conductive parts (metal panels), in which the exposed conductive parts are connected to a grounding system. In turn, this grounding system is connected to the third pin (ground pin) on the electrical power cord plug.
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Input/output specifications b. Overvoltage Category II – Pertains to instruments that receive their electrical power from a local level such as an electrical wall outlet. c. Pollution Degree 2 – A measure of pollution on electrical circuits that can produce a reduction of dielectric strength or surface resistivity. Degree 2 refers only to normally nonconductive pollution. Occasionally, however, expect a temporary conductivity caused by condensation. d. Moisture Protection – Normal (IPXO) – IPXO means that no Ingress Protection against any type of dripping or sprayed water exists. The “X” is a placeholder that identifies protection against dust, if applicable.
Input/output specifications The following table lists the input/output specifications for the ACQUITY refractive index detector. Input/output specifications: Attribute
Specification
Analog output
10, 20, 40, or 80 points/sec, 18 bit Range: -2.0 to 2.0 V
Input
Maximum input voltage: 30 VDC Logic “1”: >3.3 VDC Logic “0”:
