SpectraSYSTEM RI-150 Refractive Index Detector Reference ......Italy: Strada Rivoltana • I-20090 Rodano (Milano) • [39] (02) 95059 226 Japan: C-2F • 3-9, Moriya-cho, Kanagawa-ku

$Page 1: SpectraSYSTEM RI-150 Refractive Index Detector Reference ......Italy: Strada Rivoltana • I-20090 Rodano (Milano) • [39] (02) 95059 226 Japan: C-2F • 3-9, Moriya-cho, Kanagawa-ku$
Finnigan™

SpectraSYSTEM™ RI-150

Refractive Index DetectorReference Manual

A0099-060 Revision A May 2004

Technical information contained in this publication is for reference purposes only and is subject to change without notice. Every effort has been made to supply complete and accurate information; however, Thermo Electron Corporation assumes no responsibility and will not be liable for any errors, omissions, damage, or loss that might result from any use of this manual or the information contained therein (even if this information is properly followed and problems still arise).

This publication is not part of the Agreement of Sale between Thermo Electron Corporation and the purchaser of an LC system. In the event of any conflict between the provisions of this document and those contained in Thermo Electron Corporation’s Terms and Conditions, the provisions of the Terms and Conditions shall govern.

System Configurations and Specifications supersede all previous information and are subject to changewithout notice.

The products of Thermo Electron San Jose are produced under ISO 9001 accredited quality management systems.

Australia: P.O. Box 239 Rydalmere • Unit 14, 38 – 46 South Street • Rydalmere, N.S.W. 2116 • [61] (02) 9898-9000Austria: Wehlistrasse 27b • A-1200 Wien • [43] (01) 333 50 34-0Belgium: Technologiestraat 47 • B-1082 Brussels • [32] (02) 482 30 30Canada: 5716 Coopers Avenue, Unit 1 • Mississauga, Ontario • L4Z 2E8 • [1] (905) 712-2258France: 16 Avenue du Québec • Silic 765 • Z.A. de Courtaboeuf • F-91963 Les Ulis Cédex • [33] (01) 60 92 48 00Germany: Im Steingrund 4-6 • D-63303 Dreieich • [49] (06103) 408 0Italy: Strada Rivoltana • I-20090 Rodano (Milano) • [39] (02) 95059 226Japan: C-2F • 3-9, Moriya-cho, Kanagawa-ku • Yokohama, Kanagawa • 221-0022 • [81] (45) 453 9100Japan: Esaka Grand Building • 2-3-1 Esaka-cho, Suita City • Osaka 564-0063 • [81] (06) 6387-6681Netherlands: Takkebijsters 1 • NL-4817 BL Breda • [31] (076) 5878 722P.R. China: Room 901, Ping-an Mansion • No. 23, Jin Rong Street • Xi Cheng District • Beijing 100032 • [86] (010) 6621 0839Spain: Sepulveda 7 A • ES-28108 Alcobendas (Madrid) • [34] (091) 657 4930Spain: Acer 30 – 32 • Edificio Sertram – Planta 2, Modulo 3 • ES-08038 Barcelona • [34] (093) 223 0918Sweden: Pyramidbacken 3 • S-141 75 Kungens Kurva (Stockholm) • [46] (08) 556 468 00United Kingdom: Stafford House • 1 Boundary Park • Boundary Way • Hemel Hempstead • Hertfordshire HP2 7GE • [44] (01442) 233 555U.S.A.: 355 River Oaks Parkway • San Jose, CA 95134-1991 • [1] (408) 965-6000

Notes: The country code is enclosed in square brackets [ ]. The city code or area code is enclosed in parenthesis ( ). For countries other than the U.S.A., when you are dialing from within the specified country, dial the 0 of the city code. For countries other than Italy, when you are dialing from outside the country, do not dial the 0 of the city code.

Finnigan™, PushLoop™, and SpectraSYSTEM™ are trademarks of Thermo Electron Corporation.

This manual and the instruments to which it applies have satisfied the requirements for CSA, FCC, the EMC, and Low Voltage Directives. Use of non-approved components and repair methods may reduce or invalidate the built-in protection that is required to meet the above certifications.

Printing History: Revision A printed in May 2004

Published by Technical Publications, Thermo Electron Corporation, San Jose, California.Copyright© 2004 Thermo Electron Corporation. All rights reserved. Printed in the United States of America.

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05/2004 Thermo Electron i

Contents

Customer Support............................................................................................................................................. iii

Startup Checklist .............................................................................................................................................. vii

Getting Started................................................................................................................................................. 1-1 Features ............................................................................................................................................... 1-1 Front Panel........................................................................................................................................... 1-2 Back Panel ........................................................................................................................................... 1-4 Side Panel ............................................................................................................................................ 1-5 Bottom Panel ....................................................................................................................................... 1-6 LCD Display (User Screens).............................................................................................................. 1-7 Error Messages ................................................................................................................................. 1-11

Installation ........................................................................................................................................................ 2-1 Unpacking ............................................................................................................................................ 2-1 Standard Accessories......................................................................................................................... 2-1 Installing the Detector ......................................................................................................................... 2-3

Operation........................................................................................................................................................... 3-1 Before You Begin ................................................................................................................................ 3-1 Operating Instructions (General)....................................................................................................... 3-1 Suggestions ......................................................................................................................................... 3-2 Validation Test ..................................................................................................................................... 3-3 QuickStart............................................................................................................................................. 3-4

Theory of Operation........................................................................................................................................ 4-1 Optical System..................................................................................................................................... 4-1 Purging the Flowcell............................................................................................................................ 4-4 Electrical System ................................................................................................................................. 4-6

Troubleshooting .............................................................................................................................................. 5-1 Common Problems ............................................................................................................................. 5-1 Troubleshooting Table........................................................................................................................ 5-2

Service and Preventive Maintenance ......................................................................................................... 6-1 Service .................................................................................................................................................. 6-1 Preventive Maintenance ..................................................................................................................... 6-1

Specifications.................................................................................................................................................. A-1

Accessories and Replacement Parts .........................................................................................................B-1

ii Thermo Electron 05/2004

Figures Figure 1-1 Front panel.......................................................................................................................................1-2

Figure 1-2 Back panel........................................................................................................................................1-4

Figure 1-3 Side panel .........................................................................................................................................1-5

Figure 1-4 Bottom panel....................................................................................................................................1-6

Figure 2-1 Loosening locking screws................................................................................................................2-3

Figure 2-2 Integrator connections ....................................................................................................................2-4

Figure 2-3 Recorder connections......................................................................................................................2-5

Figure 2-4 Terminal block connections............................................................................................................2-5

Figure 4-1 Deflection type refractive index detector ......................................................................................4-2

Figure 4-2 Optical system..................................................................................................................................4-3

Figure 4-3 Movement of the image on the photodiode ...................................................................................4-4

Figure 4-4 Solvent path schematic....................................................................................................................4-5

Figure 4-5 Electrical system..............................................................................................................................4-6

Figure 6-1 Fuses .................................................................................................................................................6-3

Tables Table 1-1 Front Panel ........................................................................................................................................1-2

Table 1-2 Back panel .........................................................................................................................................1-3

Table 1-3 Side panel...........................................................................................................................................1-5

Table 1-4 Parameters for SpectraSYSTEM RI-150 refractive index detector.............................................1-8

Table 2-1 Standard accessories.........................................................................................................................2-2

Table 3-1 Chromatography conditions for Quick Start ................................................................................3-4

Table 4-1 Deflection type refractive index detector ........................................................................................4-2

Table 4-2 Optical system ...................................................................................................................................4-3

Table 4-3 Movement of the image on the photodiode .....................................................................................4-4

Table 4-4 Solvent Path.......................................................................................................................................4-5

Table 4-5 Electrical System...............................................................................................................................4-7

Table B-1 Accessories and replacement parts ................................................................................................B-1

05/2004 Thermo Electron iii

Customer Support Thermo Electron San Jose products are supported by Thermo Electron San Jose Customer Service Engineers with customer support available in North America, in Europe, and in Australasia and Asia.

IN NORTH AMERICA

In North America, Thermo Electron San Jose Customer Service Engineers are available from the following offices:

Northeastern Region Phone [1] (732) 627-0220 Fax [1] (732) 627-0260

Southern Region Phone [1] (770) 516-5589 Fax [1] (770) 516-6916

Central Region Phone [1] (847) 310-0140 Fax [1] (847) 310-0145

Western Region Phone [1] (408) 965-6000 Fax [1] (408) 965-6123

Canada Phone [1] (905) 712-2258 Fax [1] (905) 712-4203

iv Thermo Electron 05/2004

REPLACEABLE PARTS

Contact Customer Service Operations to order replaceable parts. The location and telephone and fax numbers for North America are as follows:

North America Customer Service Operations 1400 Northpoint Parkway, Suite 10 West Palm Beach, FL 33407 Phone [1] (800) 532-4752 Fax [1] (561) 688-8731 E-mail: [email protected]

TECHNICAL SUPPORT

You can contact Technical Support at the following location, telephone and fax numbers, and e-mail address:

North America Technical Support Operations 1400 Northpoint Parkway, Suite 10 West Palm Beach, FL 33407 Phone [1] (800) 685-9535 Fax [1] (561) 688-8736

E-mail: [email protected]

05/2004 Thermo Electron v

IN EUROPE

In Europe, customer support, replaceable parts, and technical support are available from each of the following offices.

Technical support is also available from North America Technical Support Operations at the following phone number and e-mail address:

Phone [1] (561) 688-8700 E-mail [email protected]

Wien (Vienna), Austria Phone [43] (01) 333 50 34-0 Fax [43] (01) 333 50 34-26

Brussels, Belgium Phone [32] (02) 482 30 30 Fax [32] (02) 482 30 31

Les Ulis Cédex, France Phone [33] (01) 60 92 48 00 Fax [33] (01) 60 92 49 00

Dreieich, Germany Phone [49] (06103) 408 0 Fax [49] (06103) 408 1222

Milano, Italy Phone [39] (02) 95 059 226 Fax [39] (02) 95 320 370

Breda, Netherlands Phone [31] (076) 587 8722 Fax [31] (076) 571 4171

Madrid, Spain Phone [34] (091) 657 4930 Fax [34] (091) 657 4937

Barcelona, Spain Phone [34] (093) 223 0918 Fax [34] (093) 223 0982

Stockholm, Sweden Phone [46] (08) 556 468 00 Fax [46] (08) 556 468 08

Hemel Hempstead, United Kingdom Phone [44] (01442) 233 555 Fax [44] (01442) 233 667

For all other countries, contact your local Thermo Electron San Jose products dealer.

vi Thermo Electron 05/2004

IN AUSTRALASIA AND ASIA

In Australasia and Asia, customer support, replaceable parts, and technical support are available from each of the following offices.

Technical support is also available form North America Technical Support Operations at the following phone number and e-mail address:

Phone [1] (561) 688-8700 E-mail [email protected]

Rydalmere, N.S.W., Australia Phone [61] (02) 9898-9000 Fax [61] (02) 9898-9800

Yokohama, Japan Phone [81] (45) 453-9100 Fax [81] (06) 453-9110

Osaka, Japan Phone [81] (06) 6387-6681 Fax [81] (06) 6387-6641

Beijing, P.R. China Phone [86] (010) 6621 0839 Fax [86] (010) 6621 0851 For all other countries, contact your local Thermo Electron San Jose products dealer.

05/2004 Thermo Electron vii

Startup Checklist This is a brief summary of the steps for installation of your SpectraSYSTEM™ RI-150 Refractive Index Detector. Complete installation information can be found in Chapter 2.

Unpack and inspect your instrument.

Position the detector appropriately.

Loosen the locking screws on the bottom of the detector.

Ensure that you are using the appropriate power cord for your power source. Then, connect the power cord.

Make rear panel connections.

Connect the flowcell.

Turn on the instrument.

Check initial response to power-on.

Verify operation with the Quick Start procedure that begins on page 3-4.

This detector was installed by:

______________________________ ____________ (Name) (Date)


05/2004 Thermo Electron 1-1

1 Getting Started

Introduction This chapter provides general information about your Thermo Electron, FinniganTM SpectraSYSTEMTM RI-150 Detector.

Features The RI-150 is a highly sensitive refractive index detector with the following features:

• The refractive index operating range is 1.00 to 1.75 RIU. A broad selection of mobile phases can be used, making the detector suitable for a variety of applications.

• An automatic intensity adjustment compensates for deterioration of the sensitivity due to flowcell contamination or reduced light levels.

• Microprocessor controlled high-resolution automatic zeroing, offset adjustment for output signal, and push-button reference liquid purge functions provide easy and prompt operation.

• Electrical design improvements provide low noise and high operational stability.

• A low volume (8 µL) flowcell and modified inlet tubing significantly reduce band broadening.

• The solenoid valve is operated at half of its rated voltage and the tungsten lamp is operated at reduced voltage to maximize component life.

• A discharge channel (drain port) on the side of the instrument directs solvent out of the detector to keep electronic and optical components dry in the unlikely event of leakage within the detector.

• A variety of input and output terminals, which are located on the back panel of the detector, makes it easy to automate a liquid chromatography system.

1-2 Thermo Electron 05/2004

Front Panel

C LPURGE

ESC

A/Z

MARKER

POWER

LEAK

ENT

[1]

[2]

[3] [4] [5] [6] [7] [8]

[9]

[10]

RI-150SYSTEMSpECTRA

Figure 1-1. Front panel

Table 1-1. Front Panel

Item No.

Description Function

1 POWER key Press the POWER key once to turn the unit On or Off. Tungsten lamp lights automatically when switch is in the ON position

2 LCD Display Displays the following screens: Status, Parameters, Validation Information, and Validation Execute. Displays the refractive index value in 1 × 10-6 RIU units in the upper portion of the Status screen. Display range is from -999 to 999. No figures are displayed when the refractive index value goes out of range.

3 ESC key Pressing the ESC key returns you to the Status screen.

4 PURGE key Press the PURGE key to purge air out of the flowcell or to flush the reference compartment of the flowcell with fresh solvent.


Table 1-1. Front Panel, continued

Item No.


5 LEAK LED The LEAK LED Illuminates when a solvent leak is detected.

6 A/Z key Pressing the A/Z key automatically zeroes the detector. Zero the detector every time you change the REC. RANGE value. As the detector is autozeroing, the LED above the A / Z key is illuminated and the message “AUTO ZERO” appears on the lower line of the Status screen.

7 MARKER key Outputs a pulse (≥5% full scale) to the MARKER OUT terminals on the back panel. This marker is most commonly used to indicate the start of a run.

8 Arrow keys The arrows keys allow you to move from screen to screen. They also allow you to edit parameter settings.

9 CL key Press the CL (Cancel) key to cancel your entries.

10 ENT key Press the ENT (Enter) key to confirm entries.


Back Panel

+_

+_

~LINE

This Equipment complies with therequirements in Part 15 of FCC Rules fora Class A computing device. Operation ofthis equipment in a residential area maycause unacceptable interference to radioand TV reception requiring the operatorto take whatever steps are necessary tocorrect the interference.

! WARNINGDANGEROUS VOLTAGES

EXPOSED WHENCOVER IS REMOVED

UNPLUG POWER CORD

! WARNINGFOR CONTINUED

PROTECTIONREPLACE ONLY

WITH SAMEFUSE TYPE

AND RATING

SEE MANUAL

T3, 15A100-240V

150VA50-60Hz

(250V)~LINE

POWER MAX.FREQUENCY

COM

PURGEIN

ZEROIN

MARKERIN

READYOUT

LEAKOUT

ERROROUT

!

INTEG OUT

FG

RECOUT

[11][12][13]

[14][15] [16]

[17]

[18]

[19]

[20]

[21]

[22]

SERIAL NO.

MODEL NO.

054/27768RI150

Figure 1-2. Back panel

Table 1-2. Back Panel of RI-150 refractive index detector

Item No.

Function Description

11 MARKER IN terminal External Signal In (Event Marker) 12 ZERO IN External Signal In (Auto Zero) 13 PURGE IN External Signal In (Purge On) 14 READY OUT Signal Out Ready 15 LEAK OUT Signal Out (Solvent leak) 16 ERROR OUT Signal Out (Error). 17 INTEG OUT Integrator out 18 FG Ground for signal cable 19 REC. OUT Recorder out 20 COM RS-232 port 21 Ground terminal Refer to page 2-4. 22 Power inlet Connect to line power


Side Panel

OUT IN

[23] [24] [25]

Figure 1-3. Side panel

Table 1-3. Side panel

Item No.


23 Outlet Port Solvent exits the flowcell through the OUT port.

24 Inlet Port Solvent enters the flowcell through the IN port.

25 Drain Port In the case of an internal solvent leak, solvent is expelled through the drain port on the side of the detector.


Bottom Panel There are two locking screws on the bottom panel of the detector. These screws lock the position of the optical bench in order to prevent damage to the instrument during shipment. During installation of the detector, you must loosen these screws. Refer to Locking Screws on page 2-3 for information on loosening these screws.

Drain Port Locking

Screws

Figure 1-4. Bottom panel of RI-150 detector


LCD Display (User Screens) The RI-150 refractive index detector has an LCD display on the front panel as shown in Figure 1-1. The display consists of following four screens: Status, Parameter Setting, Validation Information, and Validation Execute.

STARTUP SCREENS

After you press the Power key, the following start-up screens appear.

The first screen that appears displays the model name on the first line and the version number on the second line.

The second screen that appears displays the message “INITIALIZING” as the detector initializes itself.

After the detector completes its initialization process, the message “TEMP. UNSTABILIZED” is displayed in the second line of the display until the detector reaches its default temperature setting of 35°C.

When the unit reaches the default temperature setting, the “TEMP. UNSTABILIZED” message disappears and the “RD” message appears at the end of the first line.

FOUR SCREENS

The display consists of the following four screens: Status, Parameter Setting, Validation Information, and Validation Execute. Pressing the right and left arrows allows you to move from screen to screen as shown below.

Status Screen

RI−150 Ver. RA06E01

INITIALIZING

-0.0 µRIU 35 °C TEMP. UNSTABILIZED

-0.0 µRIU 35 °C RD

VALIDATION INFORMATION

PARAMETER SETTING

VALIDATION EXECUTE

-0.0 µRIU 35 °C RD


PARAMETER SETTING SCREENS

From the Status screen, press the Right arrow key to access the Parameter Setting screen. From the Parameter Setting screen, you can set the values for the parameters listed in Table 1-4.

Table 1-4. Parameters for SpectraSYSTEM RI-150 refractive index detector

Parameter Default Available Range

Recorder Range 512 µRIU 512, 256, 128, 64, 32, 16, 8, 4, 2, 1, 0.5, or 0.25 µRIU

Integrator Range 500 µRIU 500 or 125 µRIU

Temperature 35 °C 30 °C to 50 °C (in increments of 1°C ) or OFF

Time Constant 3 seconds 6, 3, 2, 1.5, 1, 0.5, 0.25, or 0.1 seconds

Polarity positive (+) positive (+) or negative (−)

Baseline Shift 0 µRIU 0 to 50 (in increments of 1)

To move from parameter to parameter, do the following: 1. Press the Up arrow or the Down arrow. 2. To access the available settings in a parameter screen, press the

ENT key. A flashing cursor appears indicating the parameter setting is selectable.

3. Select a setting by using the Up and Down arrow keys. 4. Then, press the ENT key to confirm the selection.

From the Parameter Setting screen, press the Down arrow screen to access the next screen.

The RECORDER RANGE screen allows you to set the range of your recording device. Press the ENT key. A flashing cursor appears indicating that the Recorder Range setting is selectable. Select 512, 256, 128, 64, 32, 16, 8, 4, 2, 1, 0.5, or 0.25 by using the Up and Down arrow keys. Then, press the ENT key to confirm the selection.

Press the Down arrow key to access the next screen.

The INTEGRATOR RANGE screen allows you to set the range of your integrator. Press the ENT key. A flashing cursor appears indicating that the Integrator Range setting is selectable. Select 500 or 125 by using the Up and Down arrow keys. Then, press the ENT key to confirm the selection.


The TEMPERATURE screen allows you to set the operating temperature of the detector. Press the ENT key. A flashing cursor appears indicating that the Temperature setting is selectable. Select a

PARAMETER REC. RANGE 512 µRIU

PARAMETER TEMPERATUE 35 °C

PARAMETER INTEG. RANGE 500

PARAMETER SETTING


temperature setting from 30 °C to 50 °C or select OFF by using the Up and Down arrow keys. Then, press the ENT key to confirm the selection.


The TIME CONSTANT screen allows you to select the time constant of the detector’s response. Press the ENT key. A flashing cursor appears indicating that the Time Constant setting is selectable. Select 6, 3, 2, 1.5, 1, 0.5, 0.25, or 0.1 seconds by using the Up and Down arrow keys. Then, press the ENT key to confirm the selection.


The POLARITY screen allows you to select the polarity of your analysis. Press the ENT key. A flashing cursor appears indicating that the Polarity setting is selectable. Select + or - by using the Up and Down arrow keys. Then, press the ENT key to confirm the selection.


The BASELINE SHIFT screen allows you to select the offset of your baseline. Press the ENT key. A flashing cursor appears indicating that the Baseline Shift setting is selectable. Select a value from 0 to 50 by using the Up and Down arrow keys. Then, press the ENT key to confirm the selection.


The SELECT DEFAULT screen allows you to reset the parameter settings to their defaults. If you want to reset all of the parameter settings to their defaults, press the ENT key. A flashing cursor appears. Select “YES” by using the Up and Down arrow keys. Then, press the ENT key to confirm the selection. Select “NO” if you do not want to erase your settings.

After pressing the ENT key to confirm that you want to reset the detector to its default settings, the message “Erase Current Setting?” appears. Leave the setting at “NO” if you do not want to erase your parameter settings. Select “YES” if you want to erase your entries. If you select “Yes”, the parameter settings are returned to their defaults, the detector beeps, and LCD display goes back to the Status Screen.

If you selected “NO” above, press the Down arrow to access the next parameter setting screen.

The LCD CONTRAST screen allows you to adjust the contrast of the detector’s LCD screen. Press the ENT key. A cursor appears to indicating that you can change the contrast of the LCD. Select a

PARAMETER TIME CONSTANT 1.5SEC

PARAMETER POLARITY +

PARAMETER BASELINE SHIFT 0

PARAMETER SELECT DEFAULT

ERASE CURRENT SETTING? NO

PARAMETER LCD CONTRAST 4


contrast between 1 and 7 by using the Up and Down arrow keys. Then, press the ENT key to confirm the selection.

VALIDATION INFORMATION SCREENS

The Validation Information screens allow you to access information about the performance of the RI-150 refractive index detector. To access the Validation Information screen from the Status screen, press the Right arrow key.


The LAST VALIDATION DATE screen displays the date of the most recent validation of the RI-150 refractive index detector. This screen does not display a date until you execute your first validation and enter a date in the INPUT DATE screen.


The LAMP VOLTAGE screen displays the lamp voltage detected during the last validation of the detector. If the lamp voltage exceeds 4.5 V, purge the flowcell with fresh solvent. The applied lamp voltage increases automatically as the light intensity from the flowcell drops. The reduction in light intensity can be due to either a dirty flowcell or an aging light source. Refer to page 6-2 for instructions on cleaning the flowcell. The typical lifespan of the tungsten lamp is 40,000 hours. Call service for lamp replacement.


The SPAN screen displays the difference in the refractive index between the reference solvent (typically deionized water) and a standard solution (typically a solution of sucrose) from the last validation of the detector. The span function is a validation of the detector’s response to a defined standardized solution.

VALIDATION EXECUTE SCREENS

The Validation Execute feature allows you to execute a validation routine to verify the accuracy of your RI-150 detector.

From the VALIDATION INFORMATION screen, press the Right arrow to access the VALIDATION EXECUTE screen.

To execute the Validation routine, press the ENT key once.

LAST VALIDATION DATE . .

VALIDATION INFORMATION

LAMP VOLTAGE 3.75 V

SPAN 512µRIU

ENT

VALIDATION EXECUTE


The INPUT DATE screen allows you to enter a date for the validation. Press the ENT key. A cursor appears indicating that you can edit the date. Use the Up and Down arrow keys to edit the date. Then, press the ENT key to confirm your entry.


The ZERO MEASUREMENT screen allows you to re-zero the detector’s baseline. Ensure that the detector’s temperature is stabilized and that you are pumping the appropriate mobile phase through both the reference and sample compartments of the detector’s flowcell. Then, press the A/Z key to autozero the baseline. When “0.0” appears, press the ENT key.

The SAMPLE MEASUREMENT screen allows you to validate the accuracy of your detector. With the purge valve closed, pump an appropriate standard solution through the system to verify the accuracy of the detector’s response. Press the ENT key to confirm the value that appears. This value will be reported in the SPAN screen.

Error Messages To alert you about a condition that might damage your instrument or compromise your analysis, the RI-150 refractive index detector displays the following error messages in the second line of the Status screen: Home Position Error, Leakage Error, Overheat Error, Optical Balance Error, and Parameter Error.

The “HOME POSITION ERROR” message indicates that the null glass does not come back to its home position. If this message appears when you attempt to autozero the detector from an external control device, try purging the flowcell. If this message appears during instrument startup, power off the detector and contact your local Thermo Electron representative.

The “OPT. BALANCE ERROR” message indicates that Auto-Zero was not successful. Insufficient solvent exchange of the reference flow path might cause this. Try purging the flowcell to fill the reference compartment with fresh solvent. If purging the flowcell does not correct this problem, power off the detector and contact your local Thermo Electron representative.

The “LEAKAGE ERROR” message indicates a solvent leak inside the chassis of the detector.

CAUTION! If the “LEAKAGE ERROR” message appears, power off the detector at once.

INPUT DATE . .

ZERO MEASUREMENT PUSH ENTER 0.0

SAMPLE MEASUREMENT PUSH ENTER 512.5

600.0 µRIU 35 °C HOME POSITION ERROR

600.0 µRIU 35 °C OPT. BALANCE ERROR

600.0 µRIU 35 °C LEAKAGE ERROR


The “PARAMETER ERROR” message indicates that the detector has failed to store data.

The “OVERHEAT ERROR” message indicates overheating of the detector’s optical block. If this message appears, power off the detector and contact your local Thermo Electron representative.

MISCELLANEOUS MESSAGES

In addition to the error messages listed above, there are several other messages that might be displayed as follows: Intensity, Temp. Unstabilized, Purge, and Autozero.

The “INTENSITY” message indicates inadequate light intensity. There are several possible causes for this condition:

1. The reference side of the flowcell might contain an inappropriate solvent. Set the LC pump to deliver an appropriate solvent. Then, press the PURGE key to fill the reference side of the flowcell with fresh solvent. Purge the flowcell for 5 minutes at a flow rate of 1 mL/min to refill the reference compartment with fresh solvent. Then, press the PURGE key a second time to return to normal operation.

CAUTION! Leaving the purge valve in the On position for excessive periods of time will shorten its lifespan. At a flow rate of 1 mL/min, 5 minutes is typically sufficient to flush the flowcell.

2. There are air bubbles in the flowcell. Press the PURGE key on and off a few times to remove air bubbles from both the reference and sample sides of the flowcell.

3. The optical axis is off center. Press the A/Z key to autozero the detector.

The “UNSTABILIZED TEMPERATURE” message indicates that the temperature of the optical system has not met the preset temperature.

The “PURGE” message indicates that the purge valve is open. When the purge valve is open, solvent flows through both the reference and the sample sides of the detector’s flowcell. See Figure 4-4 on page 4-5.

The “AUTOZERO” message indicates that the detector is zeroing its intensity readout.

600.0 µRIU 35 °C PARAMETER ERROR

600.0 µRIU 35 °C OVERHEAT ERROR

0.0 µRIU 35 °C INTENSITY

0.0 µRIU 35 °C TEMP. UNSTABILIZED

0.0 µRIU 35 °C PURGE

0.0 µRIU 35 °C AUTOZERO


2 Installation

Introduction This chapter covers the initial installation of your RI-150 detector, including connection to other chromatographic instrumentation. As you go through unpacking and installation, you may want to use the Start-up Checklist located at the beginning of this manual. The checklist is an abbreviated version of this chapter and is supplied as a quick reference of how to conduct a successful installation.

Unpacking Carefully remove the detector from the shipping container and inspect both the detector and packing for any signs of damage. If you find any damage, immediately contact the shipping company.

CAUTION! The RI-150 refractive index detector weighs 13 kgs (27 lbs). Use proper lifting techniques to avoid potential injuries.

Standard Accessories The shipping container should contain the detector and the standard accessory kit. Carefully check to make sure you have received all the items listed in Table 2-1. If any items are missing, contact your Thermo Electron representative immediately.

Place the detector on a vibration-free bench top as close as possible to the chromatographic column outlet (thus minimizing the length of tubing necessary for connection to the flowcell inlet). Refractive index detectors are very sensitive to changes in temperature and airflow, which can cause a drifting baseline. Therefore, be sure to place the detector in a draft-free location away from an open window, air conditioner vents, or other circulating air source. Allow at least 13 cm (5 inches) of clear space between the rear panel of the detector and any wall or obstructions to provide access to the rear-panel connectors.


Table 2-1. Standard accessories

Item No.

Item Quantity

1 Power cord for 120 V line power source and power cord appropriate for shipping destination, if different

1 or 2

2 Fuse, 3.15 A 2

3 Signal cable, double core, shielded, 2 meter length

1

4 Inlet tubing, stainless steel, preflanged, with nut and ferrule

1

5 Outlet tubing, stainless steel, with nut, ferrule and Teflon tubing

1

6 5 mm Allen wrench 1

7 Reference manual 1


Installing the Detector POWER REQUIREMENTS

The RI-150 refractive index detector requires a 50 or 60 Hz single-phase power source capable of providing 100 to 240 Vac.

CAUTION! The RI-150 refractive index detector operates with single-phase power only. If your facility provides only three-phase power, consult your local Thermo Electron representative.

LOCKING SCREWS

To prevent damage that might occur during shipment, the optical block of the detector is fixed by two locking screws (5 mm Allen bolts). After you place the detector on your laboratory bench top, loosen these screws as follows:

1. Move the RI-150 detector to the edge of the laboratory bench top until the locking screws on the bottom of the detector are accessible. Do not place the detector on its side to access the locking screws. Be careful to support the detector during this procedure to prevent it from falling.

2. Use a 5 mm hexagonal Allen wrench to loosen the screws. Do not remove the screws.

3. After you have loosened the locking screws, move the detector back to a secure position on the bench top.

NOTE: The detector will not stabilize if the locking screws are not loosened.

5 mm Allen wrench

Be careful not to tip the detectoroff the bench top as you loosenthe locking screws.

Figure 2-1. View of the RI-150 detector overhanging the edge of the bench top


ELECTRICAL CONNECTIONS

Connect the power cord to the power receptacle on the rear panel of the detector.

CAUTION! Ensure that you are using an appropriate power cord for your power source. The RI-150 refractive index detector is shipped with a 3-prong parallel blade plug that is appropriate for a 120 V, 50 to 60 Hz line power source and a power cord that is appropriate for the shipping destination.

CAUTION! Ground the instrument properly to protect the operator from electrical shock. Proper grounding also protects the instrument from power line noise. Use the ground terminals that are located on the lower right side of the rear panel to ground your instrument if you are not connecting it to a power outlet with a protective earth contact (ground). See Figure 2-2.

SEE MANUAL

T3, 15A100-240V

150VA50-60Hz

(250V)~LINE

POWER MAX.FREQUENCY

!

Figure 2-2. Grounding terminals

Make the appropriate signal cable connections using the accessory signal cable. Be sure to connect the shielded terminal of the cable to the FG terminal. See the integrator connections shown in Figure 2-3 and the recorder connections shown in Figure 2-4.

INTEG OUT

+_

FG+_REC

OUT GroundingLead

Red Lead

White Lead

Figure 2-3. Integrator connections


INTEG OUT

+_

FG+_REC

OUT

GroundingLead

Red Lead

White Lead

Figure 2-4. Recorder connections

Use a duplex wire to connect the following contact closure terminals to external devices as appropriate:

• Input signal terminals: Purge In, Zero In, and Marker

• Output signal terminals: Ready Out, Leak Out, Error Out

To connect the contact closure terminals to external devices, do the following:

1. Strip about 7 to 8 mm of insulating sleeve off the end of a duplex wire.

2. As you depress the terminal button by using a small flat-head screwdriver, insert the end of the wire into the terminal. Then, release the terminal button to lock the wire into the terminal. See Figure 2-5.

PURGEIN

ZEROIN

MARKERIN

READYOUT

LEAKOUT

ERROROUT

Figure 2-5. Terminal block connections


PLUMBING CONNECTIONS

Make the following connections after ensuring that the liquid chromatograph and the column are thoroughly purged with the solvent to be used and that the solvent is thoroughly filtered and degassed.

1. Remove the plugs from the IN and OUT ports on the side panel. Do not discard the plugs.

2. Connect the accessory stainless steel inlet tubing (Table 2.1, item 4) to the IN port.

3. Connect the accessory stainless steel/Teflon outlet tubing (Table 2.1, item 5) to the OUT port.

CAUTION! The RI-150 refractive index detector must be the last component in your LC system. Do not connect another detector, a backpressure regulator, or narrow-bore tubing to the OUT port.


3 Operation

Introduction This chapter provides step-by-step instructions for general detector operation as well as suggestions for ensuring the accuracy and reliability of the detector.

Before You Begin Before you begin this chapter, your detector should be installed in a chromatographic system (see Chapter 2), and you should have completed the Startup Checklist located at the front of this manual. We also recommend that you review Chapter 1: Getting Started to familiarize yourself with the layout of the detector controls.

Operating Instructions (General) 1. Turn on the detector by pressing the POWER key on its

front panel. 2. Set the Temperature parameter to an appropriate setting and

then allow the temperature to stabilize for at least 15 minutes. For maximum sensitivity, allow the temperature to stablize for 24 hours. Refer to page 1-8 for instructions on setting the detector’s temperature. A 76 °C thermal fuse prevents the unit from overheating by shutting down power to the heating element if necessary.

NOTE: To avoid long warm-up periods, you can leave the detector in continuous operation. The typical lifespan of the tungsten lamp is 4.5 years during continuous operation.

NOTE: If the sample or eluent cannot be heated to 35 °C, set the temperature parameter to OFF and use the detector in a room with minimum temperature fluctuations.

2. Pump eluent at a flow rate of 1 mL/min through the detector

for about 10 minutes.


3. Press the PURGE key to the ON position to thoroughly flush both the sample and reference compartments of the flowcell. Leave the PURGE key in the On position and pump mobile phase through both compartments of the flowcell for approximately 5 minutes. As you purge the detector, verify that no eluent leaks from the flowcell. If you suspect that the flowcell contains adhering gas bubbles, remove the bubbles by pressing the PURGE key On and Off every 10 seconds until all the bubbles are removed.

4. Press the PURGE key Off. 5. When a recorder is used, set the desired RANGE and turn on

the recorder. 6. Wait until the baseline has stabilized. Then, press the A/Z key

to adjust the zero position. 7. Use the Baseline Shift parameter setting to shift the baseline as

required. 8. Perform a validation test (refer to page 3-3), if required. Then,

start your analysis.

Suggestions Observe the following precautions.

• The flowcell has a pressure rating of 75 psi (5.2 bar). • Do not apply backpressure to the outlet of the detector. When the

detector is used in series with other detectors, place it at the end of the series.

• When using mobile phases containing salts, be sure to thoroughly wash the flowcell with water after use to prevent precipitation, which will damage the detector. Some salts will precipitate if exposed to high concentrations of organic solvents.

• When a high concentration of sample is analyzed, pump a sufficient amount of the eluent through the detector to remove the entire sample.

• Always use a thoroughly degassed eluent. Place the waste liquid receptacle a little higher than the detector so as not to cause negative pressure to develop at the eluent outlet.

• Be aware of potential miscibility problems when changing solvents in the detector. If the solvents are insoluble, flush the detector completely with an intermediate solvent such as acetone or ethanol.

• If a leak occurs, turn off the detector immediately and contact your local Thermo Electron representative.

• Do not use any chemical substances that can corrode stainless steel, such as hydrochloric acid.


Validation Test Thermo Electron recommends that you validate the accuracy of the detector on a regulary scheduled basis. Validation data is stored in the VALIDATION INFORMATION screens.

SUCROSE SOLUTION

Prepare a fresh solution of sucrose as follows: 1. Weigh out 350 mg of sucrose and transfer quantitatively to a

100 mL volumetric flask. 2. Add approximately 50 mL of deionized, filtered, degassed

water to the flask. Swirl the flask to dissolve the sucrose. Then, fill the flask to volume with water.

SPAN

Determine the span of the detector as follows: 1. With the PURGE key ON, equilibrate the detector by pumping

deionized water through both the reference and sample compartments of the flowcell at a flow rate of 1 mL/min.

2. Ensure that the baseline is stabilized. The baseline drift should be less than or equal to 500 nRIU/hour.

3. Go to the VALIDATION EXECUTE screen. Then, press the ENT key to access the INPUT DATE screen.

4. Enter a date for the validation. Then, press the ENT key to access the ZERO MEASUREMENT screen.

5. Press the A/Z key to autozero the refractive index readout. Then, press the ENT key to access the SAMPLE MEASUREMENT screen.

6. Disconnect the tubing from the IN port of the detector. Then, attach an adapter to the IN port of the detector.

7. Press the PURGE key to turn the purge valve off. This shuts off the flow of solvent through the reference compartment of the flowcell. Ensure that the PURGE LED is not lit.

8. Fill a syringe with the freshly prepared sucrose solution. Then, gently inject approximately 2mL of the solution into the IN port of the detector.

CAUTION! The flowcell cannot withstand a backpressure greater than 700 kPa (100 psi). Therefore, you can easily break the flowcell by forcing fluid through it.

ZERO MEASUREMENT PUSH ENTER 0.0


VALIDATION EXECUTE

INPUT DATE 04.05.12


9. Check the refractive index reading in the SAMPLE MEASUREMENT screen. The value should be within 487 to 537 µRIU (512 µRIU ±5%). The full scale reading for the detector is 1024 µRIU (1.0 V).

10. Press the ENT key once to approve the result. The confirmation screen appears, showing the span and lamp intensity readings for the detector. Press the ENT key a second time to store the sample measurement and return to the VALIDATION EXECUTE screen.

11. After you complete the validation accuracy test, reattach the tubing to the IN port of the detector.

12. Set up the LC system to pump deionized water at a flow rate of 1 mL/min. Then, press the PURGE key to flush the sucrose solution out of the detector’s flowcell. After a period of approximately 5 to 10 minutes, press the PURGE key a second time to return to normal operation.

QUICK START LC SYSTEM SETUP AND PREPARATION

1. Prepare a sample solution of sucrose (2.5 ppm) dissolved in 100% water. This example uses a 100% water mobile phase at a flow rate of 1 mL/min and a 10 cm C8 column. You can substitute other samples, solvents, and columns as needed for specific applications, but you will have to make appropriate changes in the method.

CONFIGURING THE LC SYSTEM

2. Configure your LC system as you normally would prior to analysis. Use the chromatography conditions listed below for this analysis.

Table 3-1. Chromatographic conditions

Parameter Setting

Mobile phase 100% water

Flow rate 1 mL/min

Run time 10 minutes

Column Octyl B, C-8, 4.6 × 10 cm, 5 µm particle size

Injection type PushLoop™

Injection volume 20 µL (50 ng of sucrose)

Flush solvent 100% water

SPAN 512.0 LAMP VOLTAGE 3.75



PURGING THE DETECTOR’S FLOWCELL

3. When using any refractive index detector, the elimination of air bubbles, which can be accomplished by flushing the flowcell (sample and reference compartments), is critical for optimal performance. To remove air bubbles, do the following: a) Press the POWER key to turn on the detector. b) To begin flushing the flowcell, press the PURGE key.

The green LED above the PURGE key should light indicating that the purge function is activated.

c) Pump 100% water at a flow rate of 1 mL/min through the flowcell for 10 minutes. Purging is complete when the purge valve can be switched from ON to OFF with minimal baseline disturbance.

DETECTOR FUNCTIONAL TESTS

4. Before attempting to use the RI-150 detector, do the following: a) Before the initial use of the detector, ensure that the

locking screw on the bottom of the detector has been loosened. Refer to the installation procedure on page 2-3.

b) Perform an accuracy validation test. Refer to the validation procedure on page 3-3.

c) Ensure that the temperature of the detector has stabilized. The “TEMP UNSTABILIZED” message is displayed on the second line of the Status screen until the temperature of the detector stabilizes.

d) Ensure that no error messages are displayed in the Status screen. Refer to pages 1-11 to 1-12 for a list of possible error messages.

e) Press the A/Z key and verify that the refractive index display in the Status screen reads zero.

For assistance, refer to Chapter 5: Troubleshooting if any of the above checks fail.


SAMPLE ANALYSIS 5. From the TIME CONSTANT screen, set the detector’s

response to 1.5 seconds. 6. Optimize the offset and the range settings if you are using a

chart recorder. Refer to pages 1-7 to 1-9 for instructions on entering your analysis parameters.

7. Inject 20 µL of the sample. If you are using a chart recorder, you might want to press the MARKER key to indicate the start of the injection.

The sucrose peak should elute at approximately 3 minutes. If the peak is negative, switch the polarity. The peak will be negative if the refractive index of the sample is less than the refractive index of the solvent used to flush the reference side of the flowcell.

EXPECTED RESULTS

Table 3-2 shows the typical retention times and peak areas for a 2.5 ppm solution of sucrose in water analyzed on the RI-150.

Table 3-2. Sucrose analysis data

Compound Injection Amount (ng)

Retention Time (min)

RI-150 Display (µRIU)

Sucrose 50 2.6 0.4 Note: The RI-150 display is 1 × 10-6 RIU. The actual reading for this example is 0.4 × 10-6 RIU.


SOLVENT SELECTION

NOTE: Chromatographic solvents should be thoroughly degassed before and during use. This is especially important for obtaining the best performance with the refractive index detector.

Detector response can be enhanced or degraded by the choice and preparation of the mobile phase. In addition to providing proper separation, the solvent must also be compatible with the detector and provide a sufficient refractive index difference so that the sample can be measured.

Any refractive index detector is sensitive to small changes in solvent composition, and the majority of problems associated with refractive index detectors can be traced to this cause. Changes in composition can occur from incompletely mixed binary or ternary solvents, column bleed, leaching of prior samples or solvents, decomposition of the solvent, or by changing the amount of dissolved gas in the solvent.

A specific example of the refractive index detector’s sensitivity to small changes in solvent composition is the baseline drift caused by absorption of air in a previously degassed solvent. If a degassed solvent is left exposed to air, air will absorb in the top layer of solvent and will gradually disperse through the solvent by natural convection and molecular diffusion. As the solvent reservoir is drawn down, the withdrawn solvent will increase in amount of dissolved air, and the refractive index detector will drift towards lower refractive index.

It is better to use continuously degassed solvents or maintain a helium blanket over a vacuum degassed solvent so that this drift effect is eliminated. Vacuum membrane degassing (using the Thermo Electron, Finnigan Vacuum Membrane Degasser) and helium sparging are two acceptable methods of continuously degassing the solvent.

Binary and ternary solvents must be thoroughly mixed and remain mixed to prevent baseline offsets. This detector is typically sensitive to changes in composition in the low parts per million range. Pre-mixed solvents in a stirred reservoir provide the most stable operation. Stream mixing of solvents from separate reservoirs can result in baseline upsets. Solvent delivery systems used in HPLC ordinarily have compositional mixing precision of about 1% and not parts per million. Solvents mixed and delivered by the pump will show compositional changes detectable by the refractive index detector even after passage through the chromatographic system. This effect can be minimized but not eliminated by adding additional mixing before the injector.



4 Theory of Operation

Introduction This brief theory of operation describes the functions of the components that make up your RI-150 refractive index detector. For more information, contact your Thermo Electron representative.

Optical System A beam of light is directed through a flowcell with separate compartments containing a reference solvent and the sample to be analyzed. As the light passes through the reference and sample compartments of the flowcell, it is deflected. This deflection is proportional to the difference in the refractive indices of the reference and sample solvents. The deflection is detected by a photodiode and the result is displayed as the ∆RI. This process is shown in Figure 4-1. The numbered components shown in Figure 4-1 are described in Table 4-1.


1

2

3

ns

nr 5

4 76

Figure 4-1. Deflection type refractive index detector

Table 4-1. Deflection type refractive index detector

Item No.

Description

1 Light

2 Sample compartment

3 Reference compartment

4 Light beam at the time of ns > nr

5 Light beam at the time of n s = nr

6 Displacement

7 Photodiode

ns Refractive index of liquid in sample compartment

nr Refractive index of liquid in reference compartment


The optical system is shown in Figure 4-2. The numbered components shown in Figure 4-2 are described in Table 4-2.

Figure 4-2. Optical system

Table 4-2. Optical system

Item No.

Description

1 Tungsten lamp

2 Condensing lens

3 Slit No. 1

4 Collimator lens

5 Slit No. 2

6 Flow cell

7 Mirror

8 Null glass

9 Photodiode

The condensing lens (item 2) and slit no.1 (item 3) form an image of the tungsten filament (item 1). This image passes through the collimator lens (item 4) and slit no.2 (item 5), which project the image of slit no. 2 through the flowcell (item 6) and onto the photodiode (item 9).

When there is a difference in the refractive indices of the sample and reference solvents in the flowcell, the image on the photodiode moves horizontally as illustrated in Figure 4-3. The components shown in Figure 4-3 are described in Table 4-3.

1

9

2 3

45 6 7

8


1 2

3 3

2 1

a) No difference inthe refractiveindex

Some differencein the refractiveindex

b)

Figure 4-3. Movement of the image on the photodiode

Table 4-3. Movement of the image on the photodiode

Item No.

Description

1 Diode A

2 Diode B

3 Image

The electrical signals emitted respectively from the diodes A and B change in proportion to the movement of the image. A signal corresponding to the difference in refractive index can be obtained from the difference between the two signal outputs.

Purging the Flowcell The flowcell is designed to enable replacement of a reference liquid by pushing the Purge key. Figure 4-4 shows a block diagram of the flowcell. The components shown in Figure 4-4 are described in Table 4-4.

• When the PURGE key is in the ON position, NC is open and NO is closed, allowing flow out of the sample compartment to the waste liquid receptacle by way of the reference compartment.

• When the PURGE key is in the OFF position, NC is closed and NO is open, allowing flow from the sample compartment directly to the waste liquid receptacle without going through the reference compartment.


Figure 4-4. Schematic of solvent path

Table 4-4. Solvent path

Item No.

Description

1 Heat exchanger

2 Flow cell

3 Sample compartment

4 Reference compartment

5 Heat exchange

6 Joint block

7 3-Way solenoid valve

From column

To waste liquid receptacle

1

6

7

316 stainless tubing

Teflon tubing

Connection by female nut

Connection by flange

316 stainless tubing (closed)

PURGE On

5

3

4 2

COM

NC NO

PURGE Off

NC = Normally Closed NO = Normally Open COM = Valve Exit


Electrical System The electrical system consists of various circuits such as a signal processing circuit, light quantity control circuit, temperature control circuit and flow channel changeover circuit. Figure 4-5 shows a block diagram of the electrical system.

Figure 4-5. Electrical system

12

13

17

15

14

20

18 19

25

11 10

9 8 7 6 3

3’

2

2’

1

16

5 4

26

22 21

23 24 27


Table 4.5 Electrical System

Item No.

Description

1 Tungsten lamp

2a Diode A

2b Diode B

3a Operational amplifier A

3b Operational amplifier B

4 Summing circuit

5 Light quantity control circuit

6 Subtracting circuit

7 Response circuit

8 Automatic zeroing circuit

9 Range selector circuit

10 Polarity changeover circuit

11 Event marker summing circuit

12 Output to integrator

13 Output to recorder

14 Input for polarity changeover

15 Input for event marker

16 Event marker transmission circuit output

17 Event marker output zeroing

18 Input for automatic zeroing

19 Zero over alarm output

20 Intensity alarm output

21 Temperature sensor

22 Temperature control circuit

23 Thermal fuse

24 Heater

25 Input for channel changeover

26 Flow channel for changeover circuit

27 3-way solenoid valve


Two photodiodes (2a, 2b) generate electric current in proportion to the quantity of incident light. These currents are converted by operational amplifiers (3a, 3b) into voltage signals. The difference between the two voltage signals is obtained by the subtracting circuit (6). The difference in signal corresponds to the refractive index of the eluent in the sample compartment. The signal is sent to the recorder output (13) after noise attenuation, zero adjustment, range selection, polarity changeover and event marker summing. These respective functions are carried out by the following circuits: the response circuit (7), automatic zeroing circuit (8), range selector circuit (9), polarity changeover circuit (10) and event marker summing circuit (11).

An output signal to an integrator (12) is transmitted from the automatic zeroing circuit (8) through the polarity changeover circuit (10).

The light quantity control circuit (5) controls the lamp current (luminance of the lamp) so that the light intensity obtained by inputting the voltage signals from operational amplifiers (3a, 3b) into the summing circuit (4) agrees with the present light quantity value. This stabilizes the detector sensitivity even when the flow cell is contaminated or the intensity of the lamp decreases.

The temperature control circuit (22) controls the temperature of the optical system by turning on and off the electric current to the heater (24) so that signal from the temperature sensor agrees with the existing and/or present temperature of 35 °C.

The flow channel changeover circuit (26) actuates the 3-way solenoid valve (27) according to the input for flow channel changeover and reduces the voltage by one half after starting with the rating voltage.


5 Troubleshooting

Introduction This chapter provides you with helpful information for troubleshooting possible detector and chromatographic system problems. It includes a troubleshooting guide that lists symptoms, possible causes and remedies for common problems

Common Problems The troubleshooting provides a list of symptoms, possible causes, and remedies for some common problems you may observe in detector response. Many of the problems attributed to the detector may actually be due to other components in the chromatographic system, so we have included references to these types of problems and solutions as well.


Troubleshooting Table Symptom Cause Remedy

1 Stair step disturbance of baseline

A) Bubbles in the flowcell

1) Remove the bubbles by pumping a thoroughly degassed eluent through the flowcell as you press the PURGE key On and Off repeatedly.

When the eluent is aqueous, use a solvent that is easily wettable, such as methanol, which can facilitate bubble removal.

After removing the bubbles, continue to pump thoroughly degassed eluent through the system.

2) Development of periodic noise

B) Pulsation from the pump being used

2) Add a device to eliminate the pump pulsations.

C) Bubbles in the flowcell 3) See 1) above 3) Development of

nonperiodic noise

D) Insufficient eluent degassing

4) Use a thoroughly degassed eluent

E) Contaminated flowcell 5) Clean the flowcell with a 15% nitric acid solution. Then, rinse it thoroughly with water.

F) Salts separated in the tubing or flowcell

6) Press the PURGE key to the On position and pump a sufficient amount of solvent through the system to dissolve the salts. Then, flush the system with water.

4) Swelling or drifting baseline

G Incomplete eluent replacement

7) Replace the eluent completely.

H) Unstable ambient temperature

8) Move the detector to a location with a stable ambient temperature.

I) Bubbles in the flowcell 9) See 1) above J) Contaminated flowcell 10) Purge the flowcell with water or an

organic solvent that will easily remove the adhering contamination.

5) INTENSITY message appears

K) Insufficient replacement of the eluent in the reference compartment

11) Fill the reference compartment by pushing the PURGE key into the ON position and pump a sufficient amount of eluent to fill the flowcell.

L) Bubbles in the flowcell 12) See 1) above M) Tungsten lamp burned

out 14) Call service

N) Defective solenoid valve

15) Call service

6) OPT. BALANCE message appears

O) Optical Balance out of adjustment

16) Completely purge the flowcell. If problem persists, call service.


6 Service and Preventive Maintenance

Introduction This chapter contains recommendations for situations in which you should call your local Thermo Electron service representative and recommendations for preventive maintainance.

Service Service of the RI-150 refractive index detector should be performed only by qualified personnel, such as a Thermo Electron service representative specifically trained in the repair of this type of instrument.

• The RI-150 contains no user serviceable or replaceable parts. • Do not attempt service procedures beyond the capabilities of

your facility. • Observe all cautions and warnings.

If assistance is required regarding procedures relating to this instrument, refer to Customer Support on page iii of this manual.

CAUTION! This unit contains no user serviceable or replaceable parts. Do not remove cover or disassemble.

CAUTION! Do not touch optical surfaces and do not subject the optics to potential film forming conditions or environment.

Preventive Maintenance

The RI-150 does not require specific maintenance to be performed at periodic time intervals. Preventive maintenance consists primarily of taking the necessary action, as required, in order to maintain the instrument and its flowcell in the best condition.


In addition to standard laboratory cleanliness practices, the following preventive measures are recommended:

• Use only high purity liquid in all “wetted surface” contact areas for the analysis, for flushing and for cleaning. Use only high purity gases when drying same.

• All peripheral plumbing, pumps, and so on, should be thoroughly flushed and cleaned before connection to the fluid cell.

• Avoid particulate contamination and fluid path blockage by maximum use of filtration.

• Avoid leaving buffers standing in the cell for long periods. Plan usage to minimize standing time between runs.

• Thoroughly flush all plumbing (including the fluid cell) after each use, remembering that water is the recommended “last contact” liquid. Keeping the fluid cell absolutely clean is necessary to maintain low-noise operation. Organic films and residues are major causes of noise. Consideration should also be given to the analytical solutions passing through the cell. If they pose a possible contamination problem where ordinary flushing would be insufficient, then flush-cleaning is recommended. However, flush-cleaning should only be used as a last resort when flushing with water or methanol is unsuccessful.

FLUSH-CLEANING THE FLOWCELL

An applied lamp voltage greater than 4.5 V can be an indication of a dirty flowcell. If purging the flowcell with water does not reduce the lamp voltage, you might need to flush-clean the flowcell.

A 20% nitric acid (v/v) solution is an effective flush-cleaning agent for organic films and residue. The pump and flow cell should be thoroughly flushed with water prior to performing a nitric acid flush. There should be no traces of any organic liquid in the pump, plumbing to the flow cell, or the flow cell itself, prior to initiating the acid flush. A 20% nitric acid solution will not damage a Thermo Electron analytical pump.

CAUTION! Nitric acid is a corrosive solution.

CAUTION! Chemical Hazard! Nitric acid is an oxidizer and can react violently with any organics present in the system.

To flush-clean the flowcell, do the following: 1. Disconnect the injector or autosampler and column from the

system. 2. Connect the pump directly to the detector. The PURGE key

should be in the ON position.


3. Pump the acid solution at 1 mL/min for 3 to 4 minutes. 4. Shut the pump off and allow the nitric acid to stand in the flow

cell for 3 to 10 minutes. 5. Turn the pump ON and continue pumping acid for

3 to 5 minutes. If the acid is allowed to stand in the cell for longer periods (several hours) it may harm the cell.

6. Remove the nitric acid solution by pumping degassed, deionized water through the cell at 1 mL/min for 15 to 20 minutes. Set the PURGE key to the OFF and ON positions several times during this water flush step.

REPLACING THE FUSES

The fuses for the RI-150 detector are time lag, 3.15 A, 250 Vac. To replace a fuse, do the following:

1. Press the POWER key to power off the detector. 2. Remove the power cord from the rear panel of the detector. 3. Squeeze the lever located just below the fuse holder cover until

you hear a clicking sound. Then, pull the fuse holder out of the detector’s autoswitching power supply.

4. Remove the old fuses and replace them with fresh fuses. See Figure 6-1.

5. Push the fuse holder back into the rear panel of the detector until you hear a clicking sound.

Fuse Holder

Lever

Fuse Holder

Fuses~ Line

Figure 6-1. Power supply, fuse holder, and fuses


05/2004 Thermo Electron A-1

A Specifications

Specifications

Method of detection Deflection

Refractive index range 1.00 to 1.75 RIU

Attenuator range 1/4 to 512 µRIU

Linearity range 600 µRIU

Noise ≤ 2.5 × 10-9 RIU (Response:1.5 seconds)

Time constant Settable: 0.1, 0.25, 0.5, 1, 1.5, 2, 3, 6 seconds

Polarity Positive/Negative

Zero adjustment Optical zeroing, automatic zeroing

Automatic zeroing range ± 10 × 10-5 RIU

Resolution of autozeroing ± 10 × 10-9 RIU

Offset adjustable range 0 to 500 mV (same with Integrator output sensitivity)

Resolution of offset 10 mV (same with Integrator output sensitivity)

Integrator output 0 to 1V/FS (Sensitivity: 2mV/µRIU, 8mV/µRIU)

Recorder output 0 to 10 mV/FS

External Communication RS-232

Event Marker Marker Out: ≥ 5% of FS

Signal Output Contact: ≤ 24VDC, 0.1 A Ready, Solvent Leak, Error (Overheating, Null glass home position, Lost parameters, Optical balance)

Signal Input Autozero, Marker, Polarity, Purge

Temperature control OFF, 30 to 50 °C (1 °C increment): 77 °C Temp. Fuse

Cell volume 8 µL

Maximum flow rate 10 mL/min (mobile phase: deionized water)

Pressure rating 50 kPa (0.5 kgf/cm2)

Liquid-contact materials 316 stainless steel, Teflon, Quartz optical glass

Power Requirement 100 to 240 VAC ± 10%, 50/60 Hz

Power consumption 150 VA maximum

Dimensions 260 mm W × 430 mm D × 150 mm H

Weight 12 kg (27 lbs)


05/2004 Thermo Electron B-1

B Accessories and Replacement Parts

Table B-1 lists the accessories and replacement parts for the RI 150 detector that you can order from Thermo Electron. Table B-1. Accessories and replacement parts

6015-0001 Cable, signal, RI-150

3105-2545 Tubing, inlet set, RI-150

126078 Fuse, 3.15A(T3.15AL/250V)

6003-0160 Cord, power

A0099-060 Reference manual, RI-150


05/2004 Thermo Electron index-i

INDEX

A A/Z key, 1-3, 3-2 accessories, 2-1, 2-2, B-1 accessory kit, 2-1 accuracy of detector, validating, 1-10 accuracy validation, 3-3 Allen wrench for loosening locking screws, 2-3 Australasia and Asia, customer support, vi Autozero message, 1-12

B back panel (figure), 1-4 band broadening, 1-1 baseline shift parameter, 1-9 bolts, locking, 1-6 bottom panel (figure), 1-6

C CL key, 1-3 column bleed, 3-7 COM port, 1-4 communications, RS232, 1-4 connecting

contact closure terminals, 2-5 integrator, 2-4 plumbing, 2-6

connections, vii, 2-6 contact closure terminals (figure), 2-5 contamination from samples, 3-2 customer support

Australasia and Asia, vi Europe, v North America, iii

D detector parameters, setting, 1-8 diodes, 4-4 dirty flowcell, 1-10, 6-2 drain port, 1-1, 1-5 drifting baseline, 5-2

E eluent degassing, 5-2 ENT key, 1-3 environmental conditions for detector, 2-1 Erase Current Setting? message, 1-9

error messages, 1-11 ESC key, 1-2 Europe, customer support, v

F flowcell, vii, 1-1, 4-4

cleaning, 6-2 connections, 2-1 pressure rating, 3-2 purging, 1-12, 3-2, 4-4 removing air bubbles, 3-5 schematic, 4-3

front panel (figure), 1-2 fuses

replacing, 6-3 thermal fuse, 3-1

G gases, dissolved, 3-7 ground terminal, 1-4

H high lamp voltage, 1-10 Home Position Error message, 1-11

I IN and OUT ports, connecting, 2-6 IN port, 1-5 Initializing message, 1-7 Input Date screen, 1-10 input terminals, 1-4 installation

checklist, vii contact closure terminals, 2-5 integrator connections, 2-4 loosening the locking screws, 2-3 power requirements, 2-3 procedures, 2-1

instrument startup, 1-7 integrator

connecting, 2-4 terminals, 1-4

integrator range parameter, 1-8 Intensity message, 1-12

index-ii Thermo Electron 05/2004

K keys

arrow, 1-3 autozero, 1-3 clear, 1-3 enter, 1-3 escape, 1-2 marker for run start, 1-3 purge, 1-2

L Lamp Voltage screen, 1-10 Last Validation Date screen, 1-10 LCD display

changing contrast, 1-9 error messages, 1-11 figure, 1-2 user screens, 1-7

LEAK LED, 1-3 leak output signal, 1-4 Leakage Error message, 1-11 LEDs

autozero, 1-3 LEAK, 1-3 purge, 3-5

locking screws, 1-6, 2-3

M maintenance, 6-1 MARKER key, 1-3 messages

error, 1-11 initializing, 1-7 intensity, 1-12 temperature unstabilized, 1-7

N nitric acid, 5-2, 6-2, 6-3 noise, 5-2

attenuation, 4-8 nonperiodic, 5-2 reducing, 6-2

North America, customer support, iii

O operating range, 1-1 Optical Balance Error message, 1-11 optical system, 4-3, 4-8 OUT and IN ports, connecting, 2-6 OUT port, 1-5 output terminals, 1-4 Overheat Error message, 1-12

P Parameter Error message, 1-12 Parameter Setting screens, 1-8 plumbing, 1-5 polarity parameter, 1-9 power connections, 1-4 POWER key, 1-2 power requirements, 2-3 PURGE key, 1-2 PURGE LED, 3-3, 3-5 Purge message, 1-12 purging the flowcell, 1-12, 3-5

Q QuickStart, 3-4

R recorder

connecting, 1-4 terminals, 1-4

recorder range parameter, 1-8 reference compartment of flowcell, 1-12 removing air bubbles, 5-2 repair, 6-1 replacement parts, B-1 RS232 communications, 1-4

S Sample Measurement screen, 1-11 screens

Baseline Shift, 1-9 error messages, 1-11 Input Date, 1-11, 3-3 Integrator Range, 1-8 Lamp Voltage, 1-10, 3-4 LCD Contrast, 1-9 Parameter Settings, 1-8 Polarity, 1-9 Recorder Range, 1-8 Sample Measurement, 1-11, 3-3 Span, 1-10, 3-4 start-up, 1-7 Temperature, 1-8 Time Constant, 1-9 Validation Execute, 1-10, 3-3 Validation Information, 1-10 Zero Measurement, 1-11, 3-3

screws, locking, 1-6, 2-3 side panel (figure), 1-5 solvent connections, 2-6 solvent leak output signal, 1-4 solvents, 2-6, 3-2, 3-4, 3-7, 4-1, 4-3 Span screen, 1-10 specifications, A-1 stainless steel tubing, 2-6 start run marker, 1-3

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startup, instrument, 1-7 Status screen, 1-7 sucrose test solution, 3-3, 3-6

T Temp Unstabilized message, 1-7, 1-12 temperature parameter, 1-8 test solution, suggested, 3-3, 3-6 time constant parameter, 1-9 Time Constant screen, 3-6 tools, Allen wrench, 2-3 troubleshooting, 5-1 tubing

stainless steel, 2-6 Teflon, 2-6

U unpacking detector, 2-1 unstable temperature message, 1-7

V Validation Execute screen, 1-10 validation test procedure, 3-3

Z zero adjustment, 4-8 Zero Measurement screen, 1-11 zeroing the refractive index readout, 3-5

Documents

SpectraSYSTEM RI-150 Refractive Index Detector Reference ......Italy: Strada Rivoltana • I-20090 Rodano (Milano) • [39] (02) 95059 226 Japan: C-2F • 3-9, Moriya-cho, Kanagawa-ku