manual-spectroflourometerrf5301pc

Table of Contents

PIN 220-92340-00 Table of Contents

1. Introduction 1-1

2. RF-5301 PC Components 2-1 2.1 Parts Inspection 2-1 2.2 Instrument Description 2-2RF-5301PC 2.2.1 Front View 2-2

2.2.2 Right Side View 2-3Personal Fluorescence 2.2.3 Left Side View 2-4 2.2.4 Rear View 2-5Hardware 2.3 RF-5301 PC Specifications 2-6

2.4 Optical System 2-8

3. Hardware Installation 3-1Instruction Manual 3.1 Installation Site 3-1

Revision 1.0 3.2 Installing the Xenon Lamp (Power is OFF) 3-2 3.3 Connecting the PC 3-7 3.4 SWitching Power ON 3-7 3.5 Software Installation 3-8 3.6 Instrument Initialization 3-8 3.7 Adjusting the Light Source Position 3-8

3.7.1 Coarse Adjustment 3-8 3.7.2 Fine Adjustment 3-10

3.8 Resetting the Xenon Lamp Illumination Time 3-11 3.9 Adjusting VRO 3-12 3.10 Performance Check 3-14

4. Maintenance and Inspection 4-1 4.1 Precautions in Relocating the Unit 4-1 4.2 Life Time of the Xenon Lamp 4-1 4.3 Xenon Lamp Illumination Time Management 4-1 4.4 Disposing of a Consumed Xenon Lamp 4-1 4.5 Replacing a Fuse 4-2 4.6 Wavelength Accuracy Check 4-3

4.6.1 Wavelength accuracy check for emission monochromator 4-3 4.6.2 Wavelength accuracy check for excitation monochromator 4-4

4.7 Checking SIN Ratio 4-6

5. Troubleshooting 5-1) 5.1 Errors During Initialization 5-1 5.2§ SI-IIMAOZU 5.3

Hardware Communication Problems Hardware Error Messages Related to Software Operation

5-2 5-4

Shimadzu Scientific Instruments, Inc. 5.4 Troubleshooting Hardware 5-5 7102 Riverwood Drive 5.5 Scanning Problems Columbia, MD U.S.A. 21046-2502 41 0/381 -1227

RF-5301PC Hardware Manual

5-7

iii

Table of Contents Table of Contents

First Edition: April 1995

SHlMADZt: SClENTIFlC INSTRUMENTS, INC. (SSr) PROVIDES THIS PuBUCATION "As Is" WITIlOIJr WARRANTY OF ANy KIND, ErmER EXPRESS OR lMPUED, INCLUDING, BIJr NOT LIMITED To, THE lMpUED WARRANnES OF MERCHANTABD..lTY OR FITNESS FOR A PARTICULAR PURPOSE. Some states do not allow disclaimer of express or implied warranties in certain transactions, therefore this statement may not apply to you.

Any technical inaccuracies, omissions, or typographical errors in this publication will be corrected as soon as feasible. Changes are periodically made to the information herein and incorporated into new editions of the publication. SSi may make improvements and/or changes in the product(s) and/or the program(s) described in this publication at any time.

It is possible that this publication may contain reference to, or information about, SSi products (instruments and programs), programming, or services that are not announced in your country. Such references or information must not be construed to mean that SSi intends to announce such products, programming, or services in your country.

This document and the software described in it are furnished under license from SSi and may be copied only in accordance with the terms of such license.

Address any comments to: Shimadzu Scientific Instruments, Inc., 7102 Riverwood Drive, Columbia, MD 21046. SSi may use or distribute any of the information which you supply in any way it believes appropriate without incurring any obligations whatsoever.

The following registered trademarks are used throughout this document:

IBM, PC DOS and PS/2 are registered trademarks of International Business Machines, Inc.

Microsoft and MS-DOS are registered trademarks and Windows is a trademark of Microsoft Corporation.

PopUp ScanrM is a trademark of Shimadzu Scientific Instruments, Inc., U.S.A.

SpeedBox" is a registered trademark of Shimadzu Scientific Instruments, Inc.,

U.S.A.

© Copyright 1995 Shimadzu Scientific Instruments, Inc., U.S.A.

Figure 2-1 Figure 2-2 Figure 2-3 Figure 2-4 ) Figure 2-5 Figure 3-1 Figure 3-2 Figure 3-3 Figure 3-4 Figure 3-5 Figure 3-6 Figure 3-7 Figure 3-8 Figure 3-9 Figure 3-10 Figure 3-11 Figure 3-12 Figure 3-13 Figure 3-14 Figure 3-15 Figure 3-16 Figure 3-17 Figure 3-18 Figure 4-1 Figure 4-2 Figure 4-3 Figure 4-4 Figure 4-5 Figure 4-6

Table 2-1 Table 5-1

) Table 5-2 Table 5-3 Table 5-4 Table 5-5 Table 5-6 Table 5-7

List of Figures

Front View 2-2 Right Side View 2-3 Left Side View 2-4 Rear View 2-5 Diagram of the RF-5301PC Optical System 2-9 External View ofMain Unit with Dimensions in Millimeters 3-2 Lamp Compartment Cover with Placement ofScrews 3-3 Slide Plate 3-4 Turn Screw Counterclockwise to Loosen 3-4 Xenon Lamp 3-5 Turn Knurled Screw Clockwise to Mount Lamp 3-5 Turn Clockwise to Secure Lamp 3-6 View ofPositive Terminal and Knurled Screw 3-6 Interface Cable Connection 3-7 WL Setting Dialog Box 3-9 Position of the White Paper Adjacent to the Cell Holder 3-9 Horizontal Light Source Adjustment 3-9 Vertical Light Source Adjustment 3-10 Instrument Parameters Dialog Box 3-10 Lamp Alignment Indicator 3-11 Spectrum Parameters Dialog Box 3-12 Raman Peak with Cross Hair Displayed 3-13 SIN Ratio Check Dialog Box 3-14 Fuse Location 4-2 Fuse Holders 4-2 Spectrum Parameters Dialog Box 4-3 Spectrum Screen (Emission) 4-4 Spectrum Parameters Dialog Box 4-5 Spectrum Screen (Excitation) 4-6

List of Tables

List ofParts 2-1 Initialization Error Messages 5-1 Hardware Communication Messages 5-2 Hardware Error Messages 5-3 Hardware Error Messages Related to Software Operation 5-4 Hardware Problems 5-5 Hardware Errors Related to Scanning 5-7 Hardware Errors Related to Fluorescence 5-7

RF-5301PC Hardware Manual iv RF-5301PC Hardware Manual ii

IntrOduction

1. Introduction

Thank you for your purchase of the RF-5301PC Spectrof]uorometer.

The RF-5301 PC allows high sensitivity analysis to be performed based on a ) unique optical system which involves a highly efficient Blazed Holographic Grating (BHG) as well as a low-noise circuitry that includes a digital filter.

Chapter 2 of this Hardware Manual includes sections on parts inspection, views of the instrument with parts identification, specifications, and the optical system. Later chapters contain details on installation and setup of the instrument, and maintenance. The last chapter offers help on hardware error messages, hardware troubleshooting, and scanning problems.

To facilitate operation of this instrument, assistance is available from your Product Specialist at 410/381-1227.

)

RF-5301PC Hardware Manual 1 - 1

RF-5301PC Components

2. RF-5301 PC Components

2.1 Parts Inspection

') This instrument is shipped with the following parts and accessories. Upon receipt, verify that all of the listed items are included in your shipment.

Table 2-1 List of Parts

Type Description PIN ety

RF-5301PC Main unit and standard accessories (see below)

206-81603-92 1

Part Power cord (100 - 120V) 071-60814-01 1

RS-232 cable 220-92172-00 1

Supplies 150W xenon lamp 200-81500-0 1

Fuse SA (100-120V) 072-01661-23 2

Tools Phillips screwdriver 200-94612 1

l Screwdriver for sensitivity adjustment 200-94613 1

RF-5301 PC Hardware Manual 2 - 1

RF-5301PC Components RF-5301PC Components

2.2 Instrument Description 2.2.2 Right Side View

2.2.1 Front View

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0.-i Figure 2-2 Right Side View

1. Light source horizontal adjustment screw

Use to adjust the horizontal position of the light source.0)

2. Light source vertical adjustment screw

Use to adjust the vertical position of the light source.

3. Lamp retaining screw

Use when installing or removing the lamp. The screw is accessed by1 ;D--fi I inserting the provided screwdriver through the guide tube.

/ /

\/

-! ~~ \I~09?CI

Figure 2-1 Front View 4. Power switch

1. Sample compartment Use to switch the instrument ON/OFF.

Set the sample to be measured into the cell holder inside the sample 5. Lamp ON/OFF switch compartment. Keep this switch in the ON position.

2.

3.

4.

5.

Front panel

Detach the front panel to install various accessories.

Reagent injection port cover

Detach the reagent injection port cover to inject a reagent or make other additions to the sample cell.

Light source compartment cover

Detach the light source compartment cover to install or remove the xenon lamp.

Power indicator lamp

Indicates that the power is ON when lit.

)

6.

7.

8.

Voltage switch 1

Switches voltage setting in 2 steps CAC lOOV, 200V), based on the power voltage. Use at the factory setting of lOOV.

Voltage switch 2

Switches voltage setting in 4 steps CAC lOOV, 120V, nov, 240V), based on the power voltage. Use at the factory setting of l20V.

Parallel port

Not used for this instrument.

2-2 RF-5301PC Hardware Manual RF-5301PC Hardware Manual 2-3

RF-5301PC Components RF-5301PC Components

11.

10.

9.

VO - 2 connector

Connects to a sipper.

I/O - 1 connector

Connects to an auto sampler.

RS-232C port

Used for communication with a personal computer.

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2.2.4 Rear View

2.2.3

1.

2.

Left Side View

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u ~

Analog output terminal

Outputs a voltage based on the fluorescence intensity (1 VIFS). Connects to Chromatopac, etc.

Contact closure terminal

Close this contact to start a measurement.

u Figure 2-3 Left Side View

) )

1.

2.

3.

4.

~ Figure 2-4 Rear View

Sensitivity adjustment VRO

Use to adjust the detection sensitivity when the negative high voltage (-HV) control is set to ON. For adjustment, refer to the Hardware Manual, Hardware Installation, Chapter 3, Adjusting VRO, Section 3.9.

Sensitivity adjustment VR1

Use to adjust the detection sensitivity when the negative high voltage control is set to OFF. DO NOT adjust this, as it is set to an appropriate position prior to shipment of the instrument.

Sensitivity adjustment VR2

Use to adjust the detection sensitivity when the light source compensation is set to ON. DO NOT adjust this, as it is set to an appropriate position prior to shipment of the instrument.

Ground terminal

Connects terminal to a ground wire. When the power outlet does not incorporate a ground terminal, be sure to ground the instrument via this terminal.

3

e"" I ( 2

a O~

o 0

RF-5301PC Hardware Manual 2-52-4 RF-5301PC Hardware Manual


2.3 RF-5301 PC Specifications

1. Light source

2. Light source compartment

3. Monochromators

3.1 Number of lines per mm

3.2 Wavelength scan range

3.3 Measuring wavelength range

3.4 Bandwidth

3.5 Wavelength accuracy

3.6 Wavelength scan speed

3.7 Slewing speed

3.8 SIN Ratio

4. Detector

5. Light source compensation method

6. Response

150W xenon lamp

Ozone self-extinction lamp housing

lon-blazed holographic concave grating for both excitation and emission monochromator F/2.5

1300 lines / mm

220 - 900nm and O-order light

220 - 750nm and O-order light

1.5, 3, 5, 10, 15, 20nm (excitation and emission monochromators)

1.5,3,5, 10, 15, 20nm, 6HH (half height on excitation monochromator only)

±1.5 nm

Selectable in 7 steps: Survey, Super, Fast, Very Fast, Medium, Slow, and Very Slow (Survey @ 5,500nm / min.)

Approximately 20,000nm / min.

The SIN ratio at the Raman peak of distilled water is 150 or higher under the following measurement conditions:

Excitation wavelength: 350nm

Emission wavelength: Peak wavelength of the Raman line

Bandwidths: 5nm for both excitation and emission

Response: 2 seconds

Photomultipliers for both sample fluorescence measurement and monitoring [Sample: R 3788-02; Monitoring: R 212-14]

Dynode feedback method by monitored excitation light

o- 98% / 0.02, 0.03, 0.1, 0.25, 0.5, 2, 4, and 8 seconds

RF-5301 PC Hardware Manual


7. Sensitivity selection

8. I/O

\

9. Power

10. Ambient temperature range

11. Ambient humidity range

12. Dimensions

13. Weight

D

)

Two selectable settings, HIGH and LOW (sensitivity difference: approx. 50 times)

One RS-232C port (for communication with PC)

Sipper interface; Autosampler interface; Analog output interface

100V, 120V, 220V, 240V AC, 50/60 Hz

15 - 35QC

45 - 80% r.h. [Less than 70% when temperature is 30QC or higher]

670mm (26.5") wide

530mm (21 ") deep

270mm (10.7") high

43 kg (95 pounds)

RF-5301 PC Hardware Manual 2-6 2-7


2.4 Optical System

The optical system of the RF-5301PC is displayed in Figure 2-5. A 150W xenon lamp (1) is used as the light source, and in the sample compartment, trapped ozone is broken down by the internal heat of the compartment. The bright spot of the xenon lamp is enlarged via the elliptical mirror (2), and after being collimated into a beam, is focused via a concave mirror (4) on to the excitation slit assembly (3) through the entrance slit (19). Part of the beam, which is then dispersed to a spectrum via the concave diffraction grating (5), is directed out of the exit slit (20), passes through a collecting lens assembly (11), and impinges on the sample cell (12).

The concave diffraction grating used in the spectrofluorometer employs a highly efficient ion-blazed holographic grating produced by an original Shimadzu technology. For light source compensation, a portion of the excitation light is reflected by a beam splitter quartz plate (6) to a Teflon reflecting plate (7), and the scattered light reflected by the Teflon plate is passed through an aperture (21) to balance the light quantity, and is then directed to Teflon reflecting plate #2 (8). The scattered light from Teflon plate #2 is reduced by an optical attenuator (9) and directed to a monitor photomultiplier (10).

The emitted light from the cell is passed through a lens (13), and directed into the emission monochromator, consisting of the slit assembly (14) and concave diffraction grating (15). The spectral light is reflected from a convex mirror (16) and directed to the measurement photomultiplier (17).

1) Xenon lamp 150W 2) Si0 coated elliptical mirror

2

3) Excitation slit assembly 4) Concave mirror 5) Concave diffraction grating (Excitation)

6) Beam splitter quartz plate 7) Teflon reflecting plate (1)

8) Teflon reflecting plate (2) 9) Optical attenuator

10) Monitor photomultiplier R212-14 11) Collecting lens assembly (2-lens assembly) 12) Cell

13) Collecting lens 14) Emission slit assembly 15) Concave diffraction grating (emission) 16) Concave mirror


17) Photometric photomultiplier R3788-02 18) Collection point position 19) Entrance slit 20) Exit slit 21) Light quantity balancing aperture

I

D

19

10

Figure 2-5 Diagram of the RF-5301PC OpticaL System

)

2-8 RF-5301 PC Hardware Manual RF-5301PC Hardware Manual 2-9

Hardware Installation

3. Hardware Installation

3.1 Installation Site

To take full advantage of the RF-530IPC's performance capabilities and to ensure its operational stability over a long service life, verify that the installation site selected satisfies the following requirements.

Please note that inferior performance or damage to the instrument caused by installation at a site which does not satisfy these requirements may void your warranty even within the warranty period.

Maintain room temperature between 15 - 35°C.

Avoid a location subject to direct sunlight.

Avoid a location subject to strong vibrations or prolonged weak vibrations.

Avoid a location subject to intense magnetic or electromagnetic fields.

Maintain the humidity between 45 - 80%. (When temperature is greater than 30°C, humidity should not exceed 70%.)

Avoid a location subject to corrosive gases or organic/inorganic gases which absorb in the ultraviolet region.

Maintain in a relatively dust-free environment.

The dimensions of the RF-5301PC are 670 mm (26.5") wide x 530 mm (21") deep x 270 mm (10.7") high. In addition, the operations are conducted from a PC, requiring an installation surface area of approximately 1500 mm (59") wide x 800 mm (31.5") deep, depending on the size of the PC.

The weight of the RF-530IPC is 43 kg (95 Ibs.). Verify that the installation bench is sturdy enough to support at least this weight.


Hardware Installation Hardware Installation

670 ~ ,

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When installing or replacing the lamp, disconnect the power cord from the power receptacle before removing the lamp compartment cover.

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Immediately after the power is turned OFF, residual electric charges could cause an electric shock. Therefore, after the power cord is disconnected, wait at least five (5) minutes before removing the lamp compartment cover.

@ a!'i]L-

W WARNING: Since gas is contained at high pressure inside the xenon lamp, breakage of the lamp would be very dangerous. Be very careful to avoid imparting any shock, vibration or pressure to the lamp which

I ~13 could cause it to break (explode). (For details, please refer to the lamp's inspection certification included with the lamp.)

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I I I~F·.V_O.QECI

Lamp Installation Procedure 1. Leave the lamp switch in the ON position.

T 2. Detach the lamp compartment cover by removing the two retaining c e- screws.N

01l U \.:::I

Position of Screws DFigure 3-1 External View of Main Unit with Dimensions in Millimeters

3.2 Installing the Xenon Lamp (Power is OFF)

When installing the xenon lamp, verify that the power is switched OFF to prevent electrical shocks, and disconnect the power cable from the power receptacle.

NOTE: When installing a new bulb, DO NOT touch the glass surface of the lamp. If accidental contact is made, wipe off the lamp with a Figure 3-2 Lamp Compartment Cover with Placement ofScrews moistened cloth using the cleaner provided with the lamp or wi th a soft cloth moistened with ethyl alcohol. Fingerprints remaining on the 3. Loosen the two sliding plate retaining screws, and slide the plate to

lamp when the lamp is turned on could result in burnout of the lamp. expose the inside of the lamp compartment.

) CAUTION: When the xenon lamp is turned on, about 30,OOOV are applied to the positive electrode (labeled +HV). In addition, while the lamp is turned on, a 90V charge keeps the lamp above IOOce. Therefore, ascertain that the lamp compartment cover is in place whenever the instrument is in use.

3-33-2 RF-5301PC Hardware Manual RF-5301PC Hardware Manual


5. Remove the xenon lamp from the case and remove the knurled screw at its negative terminal.

Slide Plate

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n.~

Xenon lamp bulb

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V:~\oef(,( i 0'f).)~ 0

.,,}h. ~. (}3V"fi""~ Figure 3-3 Slide Plate :)vJ),\~~ ~ 5<'

. {\'7 ~ ~'tv-J-.- ' cJD L..------?-f=IJ'~-----------=---------'

4. Insert the accessory screwdriver into the guide tube through the lamp ~C(Jf' \ ~ Figure 3-5 Xenon Lampmounting screwdriver hole, and loosen the lamp mounting screw by turning it counterclockwise. ~o--'v)O~.'0Insert the negative terminal of the lamp into the lamp compartment with

either the black or red mark in the cemented part of the terminal facing the lamp mounting screw. == == D@ ==

== CAUTION: If the lamp terminals are reversed when inserting the

==== lamp, the lamp will be damaged (explode) when the power is switched

== ON.

Figure 3-4 Turn Screw Counterclockwise to Loosen

, Facing the) lamp mounting screw

Figure 3-6 Turn Knurled Screw Clockwise to Mount Lamp

3-4 RF-5301PC Hardware Manual RF-5301PC Hardware Manual 3-5


7. Insert the accessory screwdriver through the lamp mounting screwdriver hole, and secure the lamp in position by turning the lamp mounting screw clockwise.

=== o == == == == == ==

Figure 3-7 Turn Clockwise to Secure Lamp

8. Close the slide plate and tighten the slide plate set screw.

9. With the positive terminal of the cable attached to the positive terminal of the lamp, fix the xenon lamp in the lamp holder by firmly turning the knurled screw by hand.

CAUTION: Damage to the xenon lamp could result if the positive terminal is pulled by the power cable while the lamp is ON. When tightening the positive terminal with the knurled screw, be sure to leave some slack in the positive terminal cable. Tighten the knurled screw ONLY by hand. Using tools, such as pliers or wrenches, could cause damage to the lamp.

Positive Terminal Screw

Figure 3-8 View of Positive Terminal and Knurled Screw

10. Attach the lamp compartment cover.


3.3 Connecting the PC

After the instrument is positioned, the RS-232 interface cable is used to connect the RF-5301PC to the personal computer (PC). Insert the male cable connector into the connector labeled RS-232C on the right side of the RF5301PC, and secure the cable with the screws. Next, connect one of the female connectors to the PC serial port (IBM compatibles normally have two serial ports, COM 1 and COM2), and secure the cable with the screws

Figure 3-9 Interface Cable Connection

3.4 Switching Power ON

Power Supply The power consumption of the RF-5301PC is about 400V. Operate the RF5301PC from a power supply rated at least 400VA. Supply voltage fluctuations are allowable up to ± 10%. Use a voltage regulator to regulate any voltage fluctuations above ±lO%.

Grounding The power cable of the RF-5301PC consists of three wires, including the grounding conductor. Plug the power cable into a three-wire AC outlet for positive grounding. When the available outlet is of the two-wire type, ground the unit from either the grounding terminal of the power cable or that on the rear of the unit.

Plugging the Power Cable Plug the accessory power cable into the power connector on the rear of the unit, but not before checking to see that the power switch is off. Ascertain that

) the voltage setting selector is adjusted appropriately.

Xenon Power Switch The xenon power switch above the power switch is then turned ON. When all the preparations are complete, switch on the power (listen for a clicking sound). The lamp will automatically light. In addition, verify that the power display lamp on the front of the instrument is on.

RF-5301PC Hardware Manual 3-6 3-7


When the xenon lamp does not light, or if there is no clicking sound when the power is switched on, or when the clicking sound continues without the xenon lamp lighting, immediately switch the power OFF, and refer to

Troubleshooting, Chapter 5 in this Hardware Manual.

3.5 Software Installation

See the Software Instruction Manual, Installation, Chapter 2.

3.6 Instrument Initialization

NOTE: Before turning the power switch ON, open the sample compartment door and check to see that no packing material is left inside and that there is no object in the holder that would block light transmission.

Run the RF-5301PC software and then turn the power switch ON. Upon startup, the unit automatically begins an initialization procedure. Each time an initialization step is successfully completed, the initialization status box displays OK, then proceeds to the next step. If an error is encountered, the unit will stop the process. In this case, see Troubleshooting, Chapter 5 in this Hardware Manual. When the initialization procedure is completed, the main screen appears.

3.7 Adjusting the Light Source Position

The Raman lines emitted from distilled water can be used to adjust the light source position. Light source position adjustment is required when the xenon lamp is installed for the first time or when it is replaced. After turning the power switch ON, wait at least thirty (30) minutes before adjusting the light source position.

3.7.1 Coarse Adjustment

1. Click on the Go to WL push button at the bottom of the screen and enter 500nm for the excitation wavelength (green light). Select the Set push button.


EM WavelengthE~ Wavelength -1.J)/', I.;

~6~ I:jj _lI,lItfJ_J.tI

) Intensity: [9219 I

I .Read" J 1.~eJ I ~cil.l

Figure 3-10 WL Setting Dialog Box

2. Open the sample compartment door. As a green beam of light is emitted from the light source toward the cell, place a piece of white paper just to

the right of the cell holder as shown in Figure 3-11.

\. '

Figure 3-11 Position of the White Paper Adjacent to the Cell Holder

/3. Using the Phillips screwdriver, manually adjust the light source

horizontal direction for maximum brightness.

cB '/-J \. ~ / ~ 0°

Ct-{\ ,--0\l

\ ,,\ "r!'.' <)J p..J, (~\....., t'0 {

\YJ \{-- '-l0 C(~ r ..

\) Ct- .J Figure 3-12 Horizontal Light Source Adjustment0\

CAUTION: Adjust the horizontal direction first. If the vertical

) direction is adjusted first, you may not be able to adjust the beam of light.

4. Likewise, manually adjust the light source vertical direction using the adjustment screw.

3-9RF-5301PC Hardware Manual 3-8 RF-5301PC Hardware Manual


@ 2. Using the number in the center of the Lamp Alignment dialog box as a

guide, adjust the light source horizontal direction adjusting screw for the maximum value (see Figure 3-12).

-, _~!m:""ilI!"allll"

) lamp Time Used: 260 1~;:a~iji1:·;;:;t"I) ~~ Ir~; .~i(4r. ~J

Figure 3-13 Vertical Light Source Adjustment 11·653

5. Remove the paper inserted in step 2. Set a cell filled with distilled water into the cell holder and close the sample compartment door.

6. Set the excitation wavelength to 350 and the emission wavelength to 397. Proceed to the Fine Adjustment.

3.7.2 Fine Adjustment

1. Select Instrument... from the Configure menu. When the dialog box appears (see Figure 3-14), click on the Lamp Align Perform push button to bring up the Lamp Alignment dialog box (see Figure 3-15).

Figure 3-15 Lamp Alignment 1ndicator

3. Likewise, adjust the light source vertical direction adjusting screw to its maximum value (see Figure 3-13). This completes the light source position adjustment.

3.8 Resetting the Xenon Lamp Illumination Time

'SKip fluorometer: @§~] o Off

-.!::!.V Control: @On o Off

E'MT Protect: @On o Off

Auto Shutler:

Dark Level Correction:

SIN Ratio Test:

Lamp Align:

Instrument Serial Number: 00000000000001

Instrument ROM Version: 0.90

Lamp Time Used: 91

"·r;/'~·'j';'W"." "',-

'·,=0,gK; "1 Figure 3-14 1nstrument Parameters Dialog Box

The length of time (in hours) that the lamp has been used is indicated in the Lamp Alignment dialog box (see Figure 3-15). To reset the xenon lamp illumination time, upon installation of the lamp for the first time or when replacing it, perform the following steps:

1. Select Instrument... in the Configure menu to open the Instrument Parameters dialog box.

2. Select the Lamp Align Perform push button to display the Lamp Alignment dialog box. Click on the Reset button. (These steps are unnecessary when continuing from Installing the Xenon Lamp in this chapter, Section 3.2.)

.- / I Z

3 - 10 RF-5301PC Hardware Manual RF-5301PC Hardware Manual 3 - l'


3.9 Adjusting VRO

The sensitivity adjustment is performed using the Raman peak of distilled water.

1. Select the Spectrum mode.

2. Select Instrument... in the Configure menu, and set -HV Control and PMT Protect to ON. Click OK.

q ")

4.

5.

Place a cell containing distilled water in the cell holder and close the sample compartment cover.

Press the Go To WL push button, and set the emission wavelength to 450nm. Select the Set push button. Press the Auto Zero push button and then the Start push button to initiate the measurement. When the scan is completed, enter a file name in the File Name dialog box which appears on a Spectrum screen similar to that in Figure 3-17.

3. Select Parameters••• in the Configure menu to display the Spectrum Parameters dialog box (see Figure 3-16). Set the parameters as follows by tabbing through the box:

Spectrum Type: Emission

EX Wavelength: 350

EM Wavelength Range: 350 - 450

Recording Range: 0.000 (Low); 50.00 (High)

Scan Speed: Fast

Sampling Interval: 1.0nm

EX / EM Slit Width: 5nm / 5nm

Sensitivity: High ( Response Time: Auto

Repeat Scan / Auto File: No setting required at this time.

Spectrum Iype: o Excitation @Emission o Synchronous

EX ~avelength: 3SO Inm

110 ••

file Acquire Mode .configure Manipulate Eresentation Help

%; ~ ~

50000. iii i.

360.0 360.0 396.1390 Wavelength (nm)

iii

420.0 4400 450.0

1 Figure 3-17 Raman Peak with Cross Hair Displayed EM Wavelength Range: -Start 3SO fnd 4SO

1 1

Recording Range: !"ow High I 6. Press the right mouse button, and select Cross Hair from the Graph I 0.000 Iso.ooo PopUp menu, and from that submenu, select Display. When the cross

SJ;anning Speed: IFast ~ hair used for reading values appears, position it on the Raman peak of Sampling Interval [nm): 397nm to read the peak intensity.11.0 I~ -Slit Width [nm): E~ EMEE EE I 7. When the peak intensity value is, 10±2{, the following adjustment is Se!!sitivity: @[H.iii~! o Low unnecessary. When it is outside the stated limit, adjust the uppermost Resl!onse Time (sec): [!l volume trimmer (VRO) on the back of the instrument (see RF-5301 PC

Components, Chapter 2, Section 2.2.4 of this Hardware Manual).

IBepeatscan..·II,AutoFile... ) 1m. OKs_II cancet!

NOTE: Do not turn any other trimmer (i.e., VR 1, VR2), as they are

IAuto

Figure 3-16 Spectrum Parameters Dialog Box adjusted appropriately prior to shipment.

RF-5301PC Hardware Manual 3 - 133 - 12 RF-5301PC Hardware Manual


8. Repeat steps 5 through 7 until the intensity reading satisfies the 5. The amount of noise determined from the time measurement of the requirement. Raman peak is calculated as the SIN Ratio. An SIN ratio of at least 150 is

considered normal. When an abnormal value is obtained, please refer to 3.10 Performance Check this Hardware Manual, Troubleshooting, Chapter 5.

After installing the instrument and the lamp, and adjusting the light source position, the performance check procedure is conducted to verify that the instrument is operating normally.

1. When this operation is not performed immediately after the previous procedures, switch the power ON and light the lamp, and allow the lamp to stabilize for at least 30 minutes. Otherwise, ascertain that the lamp has been on for thirty (30) minutes.

2. Select Instrument... from the Configure menu to display the Instrument Parameters dialog box, and click on the SIN Ratio Perform push button. The SIN Ratio Check dialog box appears, along with the message "Fill a cell with distilled water; Set the cell in the holder." as in Figure 3-18. Place a cell containing distilled water into the cell holder and close the sample compartment cover. Click OK to automatically begin the check.

.0500~1 ~ ~

Fill a cell with distilled water. Set the ullin the holder.

[,~ J!rint;t:rl

ksp";$i;'i;Il'tJ

';;00 [Tf'Eilit'''lilfl

440.0 4500

<00'"200.00

o " 000

000

::[oOOJ[

!

10m> T.ne(sec)

Instrument Serial Number: ~O()OOOOOOOOOOl I Peak Height: [==:=I SIN Ratio: [==:=I

I

~~r~ q~~~~ \t':r-t :' ..." 1lF-5301 PC file Acquire t.4ode tontigure Manipulate fresentation Help

0000[. ! ,,, ..... , d

3500 3800 3800

~,,",:,"~,,....;.: ~n,,~~"":'-,~"""'''''''_._.~,~m,,,,"..,...

.son«0.0'200

~ l CAUTION: Contaminated or low-purity distilled water would elevate) the baseline, increasing noise.

Figure 3-18 SIN Ratio Check Dialog Box J), 3. The Raman peak measurement of distilled water is quickly conducted,

and the peak height is displayed. The SIN Ratio measurement requires approximately ten (10) minutes.

3 - 14 RF-5301 PC Hardware Manual RF-5301PC Hardware Manual 3 - 15

Maintenance & Inspection

4. Maintenance and Inspection

4.1 Precautions in Relocating the Unit

Be sure to remove the xenon lamp from the unit before transporting the RF5301PC. (Store the lamp in its special protective case.) Since gas is contained at high pressure inside the xenon lamp, breakage of the lamp would be very dangerous. Be very careful to avoid imparting any shock, vibration or pressure to the lamp which could cause it to break (explode).

Also, when installing a new lamp, DO NOT touch the surface of the lamp bulb. When accidental contact is made, wipe off the lamp with a piece of cloth moistened with the cleaner provided with the lamp or with ethyl alcohol. Fingerprints remaining on the lamp when the lamp is turned on could result in burnout of the lamp.

4.2 Life Time of the Xenon Lamp

The xenon lamp is a consumable part. After accumulation of excessive hours of use, the lamp will begin to flicker as the emission point fluctuates. In this condition, an unacceptable level of noise will be evident.

The recommended usage time is 500 hours. Avoid using the lamp beyond 1000 hours of service. On rare occasions, the lamp could break, causing major damage to the internal components of the instrument or injury to the operator.

4.3 Xenon Lamp Illumination Time Management

This instrument incorporates a lamp usage monitoring function. To verify the accumulated hours of illumination of a lamp, select Instrument... from the Configure menu in the menu bar. Remember to press the Reset key to reset the time indicator to 0 after replacing the lamp.

4.4 Disposing of a Consumed Xenon Lamp

Care must be taken when discarding a used xenon lamp. Inappropriate handling can be extremely dangerous, due to the possibility of the lamp exploding. When disposing of a used lamp, wrap it in thick cloth or similar material, and break it with a hammer before disposal.


Maintenance & InspectionMaintenance & Inspection

4.6 Wavelength Accuracy Check 4.5 Replacing a Fuse

The emission line (435.8nm) for mercury contained in most fluorescent room When the fuse burns out, replace it with a new fuse using the following lights can be used to check the accuracy of the monochromator wavelengths. procedure.

1. Using the screwdriver provided, pry open the claw on the fuse cover at 4.6.1 Wavelength accuracy check for emission monochromator '" )the rear of the instrument. 1. Select Spectrum from the Acquire mode menu to conduct a spectrum

measurement.

2. Select Instrument.•. in the Configure menu, and set -HV Control and PMT Protect to OFF. Click OK.

3. Select Parameters•.. in the Configure menu to display the Spectrum Parameters dialog box (see Figure 4-3). Set the parameters as follows by tabbing through the box:

Spectrum Type: Emission

EX Wavelength: 350

EM Wavelength Range: 400 - 500

Recording Range: -10.000 (Low); 1000.00 (High)

Scan Speed: Medium Figure 4-1 Fuse Location Sampling Interval: 0.2nm

EX / EM Slit Width: 3.0nm / 3.0nm 2. Remove the fuse holders (two identical holders). Sensitivity: High

3. Replace the used fuses with new ones, and insert the fuse holders into the Response Time: Auto

fuse compartment. Be sure to match the arrows on the fuse holders and the cover.

/ Fuse , ~ ;use,:~HOld"

Figure 4-2 Fuse Holders

Repeat Scan / Auto File: No setting required at this time.

Spectrum Iype: o Excitation @ Emission o Synchronous

EX 't:!'avelength: 350 Inm 1

EM Wavelength Range: )itart 400 £nd1 I 1500 I Recording Range: bOW !:!igh 110001-10 I I SJ;anning Speed: IMedium f!J Sampling !nterval [nm): 210. f!J

EX EMI Slit Width lnm): E:E EE Sensitivity: @High o Lowj) ) ResQonse Time [sec]: IAuto [3

IBepellt sc.;n...J I Auto file.:. ,I I.·.· .'§[' ,.1 I· .Canee'l > J

Figure 4-3 Spectrum Parameters Dialog Box

RF-5301PC Hardware Manual 4-3RF-5301PC Hardware Manual 4-2


4. Select OK to validate the parameters. The main screen reappears. As the parameters are sent to the instrument, the Fluorometer Window on the Status Bar indicates Fluorometer Setup. The EX and the EM wavelengths and the intensity reading are displayed in the Fluorometer Window when completed.

5. Open the sample compartment door, remove the cell from the sample compartment, and verify that the light from the fluorescent lamp is directed into the emission monochromator. (Leave the sample compartment door open for the test.)

6. Press the Start push button to initiate measurement. When the measurement is completed, select Radar. A spectrum is obtained similar to that shown below, depending on the room lighting conditions.

I'll"

420 0

Eile ~cquire Mode J;.onfigure Manipulate flresentation ttelp

i:c

r·~h'· ..~:'.'N 7LG?w...=~

Figure 4-4 Spectrum Screen (Emission)

6. Select Peak Pick in the Manipulate menu (see the RF-5301PC Software Instruction Manual, Peak Pick, Section 5.4.5), and in the Peak Pick window, verify that the peak is at 435.8 ±1.5nm. Record the peak wavelength. If the measured wavelength is not 435.8 ±1.5nm, please contact your Service Representative.

Next, the excitation monochromator wavelength accuracy check is conducted.



4.6.2 Wavelength accuracy check for excitation monochromator

1. Insert a piece of white paper (without fluorescent dye) in the sample compartment according to Figure 4-5.

)

50mm

I....8ill.-... hOlder~

I

I;; ~

I

/Cell

~-

D Figure 4-5 Position of White Paper in Sample Compartment

I Excitation light

/7

White paper

... . 14mm

Size of the white paper

+

L

2. Select Instrument... in the Configure menu, and set -HV Control to OFF. Click OK.

3. Select Parameters•.• in the Configure menu to display the Spectrum Parameters dialog box (see Figure 4-6). Set the parameters as follows by tabbing through the box:

I) )

Spectrum Type:

EM Wavelength:

EX Wavelength Range:

Recording Range:

Scan Speed:

Sampling Interval:

EX / EM Slit Width:

Sensitivity:

Response Time:

Repeat Scan / Auto File:

Excitation

o 400 - 500

0.000 (Low); 1000.0 (High)

Medium

0.2nm

3.0nm / 3.0nm

High

Auto

No setting required at this time.

RF-5301 PC Hardware Manual 4-4 4-5

Maintenance & Inspection Maintenance & Inspection

Spectrum Iype: @ Excitation o Emission o Synchronous

EM ~avelength: 10 1nm

EX Wavelength Range:

Recording Range:

S.!;anning Speed:

Start 1400

low I 0.000

IMedium 0

I I

.End

!:!igh

1500 1

11000.00 1

I Sampling !nterval [nm):

Slit Width (nml:

Sensitivity:

1°·2 11] E~ E::E @High o Low

EM E::E Resl!onse Time (sec): IAuto ~, I

If!epeats.;a~·..:1 I': Auto fii~ ... ,'I I, .o~ "I r':·· C~;'cel"j

Figure 4-6 Spectrum Parameters Dialog Box

4. Select OK to validate the parameters. The main screen reappears. As the parameters are sent to the instrument the Fluorometer Window indicates Fluorometer Setup. The EX and EM wavelengths and the intensity reading are displayed in the Fluorometer Window when completed.

5. Select the Go to WL push button at the bottom of the screen. Set the excitation wavelength to 450nm and the emission wavelength to Onm.

6. Adjust VR1 so that the Intensity value falls within the range of 100.000200.000.

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file ,;cquire Mode £onfigure Manipulate e,esentation .t!elp

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Figure 4-7 Spectrum Screen (Excitation)


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7.

8.

Select Peak Pick in the Manipulate menu (see the RF-530JPC Software Instruction Manual, Peak Pick, Section 5.4.5), and in the Peak Pick window, verify that the 450.1nm bright line of the xenon lamp is within the range of ±2.5nm. The cumulative error, which depends on the position of the white paper (approximately ±1 nm), will affect the wavelength accuracy of the instrument.

Set a cell filled with distilled water into the sample compartment. Execute the Lamp Align function from Instrument in the Configure menu and readjust the VR1 so that the Intensity value falls within the range of 10.000 ±5.

9. Press the Start push button to initiate measurement. When the measurement is completed, select Radar. A spectrum is obtained similar to that shown in Figure 4-7.

This is an easier method for obtaining the wavelength accuracy of the instrument. An Hg lamp is necessary to obtain the exact wavelength accuracy. Please contact Shimadzu or its nearest representative for further information.

D 4.7 Checking SIN Ratio

The SIN ratio is checked using the Raman peak of distilled water. For details, refer to the RF-530I PC Hardware Manual, Performance Check, Section 3.10 or the RF-5301PC Software Instruction Manual, Instrument, Section 5.3.5.

)

RF-5301PC Hardware Manual 4-6 4-7

Troubleshooting

5. Troubleshooting

5.1 Errors During Initialization

When the power is switched on to the spectrofluorometer, initialization of the instrument is performed and eight initialization and self-diagnostic procedures are conducted. An error message is displayed when an abnormality is encountered during the initialization sequence. Take the appropriate corrective action for any errors encountered, according to the directions which follow.

When an error is generated during initialization, acknowledge the message box and click on the Start button or Read button on the lower right of the screen to establish communication between the PC and RF-5301PC, enabling operation of the instrument. As normal operation of the instrument under this condition cannot be guaranteed, it is recommended that you call your Service Representative.

Table 5-1 Initialization Error Messages

Error Indication Remedial Action

ROM Contact your Service Representative.

RAM Contact your Service Representative.

EE-PROM Contact your Service Representative.

Excitation Slit Contact your Service Representative.

Emission Slit Contact your Service Representative.

Excitation Monochromator Contact your Service Representative.

Emission Monochromator Contact your Service Representative.

Baseline Is sample compartment cover open? When sample compartment cover is closed and this error occurs, contact your Service Representative.

RF-530 1PC Hardware Manual 5 - 1

Troubleshooting Troubleshooting

5.2 Hardware Communication Problems Table 5-3 Hardware Error Messages

When there is a problem in communication between the PC and RF-5301PC, take corrective action as directed in Table 5-2. When communication is not being conducted normally, OFF is displayed in the Fluorometer Window of the Status Bar.

Table 5-2 Hardware Communication Messages

Item To Be Checked Remedial Action

Cable Connection Verify that RS-232C cable is properly connected at the RS-232C ports of the PC and the RF-5301PC. After verifying connections and tightening the connector screws, click the Start or Read button on the Main screen to reestablish communication.

Cannot communicate with The PC and spectrofluorometer cannot spectrofluorometer. communicate. Verify the cable connections and the

appropriate COM port setting in the PC Configuration dialog box.

COM Port Setting Referring to the documentation provided with your PC, verify that the COM port (RS-232C port) is set up correctly. Select PC Configuration... from the Configure menu of the RF-5301 PC software, and confirm that the selected COM port radio button (button is black) corresponds to the COM port which is actually connected. If the appropriate button is not currently selected, click on the correct COM port radio button. After completing the setting, close the PC Configuration dialog box, and click on the Start or Read button to reestablish communication. After communication is established, select Save Parameters... in the Configure menu, and save the current settings to the RFPC.CFG file.

D

Error Messages Remedial Action

Cannot open COM port! The specified COM port cannot be opened. This error occurs when another application is using the COM port or when there is a major Windows conflict. In addition, this can also occur when a nonexistent COM port is specified in the PC Configuration dialog box.

Communications Initialization Failed! The specified COM port cannot be initialized.

There maya problem with the PC hardware. Take appropriate action as directed by your PC documentation.

Communications time out! Communication cannot be conducted between the PC and the RF-5301 PC. Verify cable connections and the COM port setting in the PC Configuration dialog box.

Failure of DCB initialization! The Device Control Block for the specified COM port cannot be created. This normally occurs when the RFPC.CFG file is corrupted.

General communications error!

Undefined Control Command.

This error is generated when there is an attem pt to create a file for a directory which does not exist, or when the disk is either full or abnormal. When a floppy disk is being used, be sure to insert the floppy disk fully into the drive.

The command indicated is not defined for control of the spectrofluorometer, and cannot be used. This error occurs when the RFPC.CFG file is corrupted or when there is a poor cable connection, etc.

Unknown Communications Error!

Same as Undefined Control Command.

)

5-2 RF-5301 PC Hardware Manual RF-5301PC Hardware Manual 5-3

Troubleshooting

5.3 Hardware Error Messages Related to Software Operation

Error messages associated with software operation, the cause of such messages and appropriate corrective actions are listed in Table 5-4.

Table 5-4 Hardware Error Messages Related to Software Operation

Troubleshooting

5.4 Troubleshooting Hardware

If problems arise with the instrument, take corrective action as directed in Table 5-5. If the symptom does not correspond to any of the descriptions in the table, contact your Service Representati ve.

Table 5-5 Hardware Problems

Error Message Cause and Remedial Action

Cannot Auto Zero Displayed when the signal level is too high to allow running the Auto Zero function. Set the sensitivity to LOW and narrow the slit to reduce the level of the signal. When analyzing a solid or powder sample, use of an appropriate filter is an effective solution. When the excitation and emission wavelengths are too close to one another, increase the distance between them. If the above measures do not resolve the problem, or if Auto Zero cannot be performed even when the shutter is closed, the instrument may not be operating normally. In this case, contact your Service Representative.

Cannot turn ON negative high voltage (-HV). (Lamp does not light.)

When the lamp is not illuminated, the lamp negative voltage cannot be turned ON.

An error occurred in the emission monochromator wavelength drive. Contact your Service Representative.

EM monochromator has slipped.

EX monochromator has slipped.

An error occurred in the excitation monochromator wavelength drive. Contact your Service Representative.

The xenon lamp illumination time is incorrect. Try resetting the lamp illumination time to O. If this problem occurs again, contact your Service Representative.

Replace the xenon lamp.

Lamp usage time is invalid.

The number of hours the lamp has been on has exceeded SOD! For optimum instrument performance replacement of the lamp is recommended.

Symptom Probable Cause Remedial Action - - ~

Power is not supplied when power switch is turned on.

AC cable is not correctly inserted into socket.

Plug the AC cable firmly into the unit inlet and the AC outlet.

Replace the fuse with a new one.Power fuse blown.

Any other cause. Call your Service Representative. --

SIN Ratio does not meet specified value.

Poor lamp source positioning.

Re-adjust thelight source position.

Wait at least thirty (30) minutes after turning on the power to allow the lamp to reach a stable state.

Unstable lamp illumination.

Old xenon lamp. Replace with new lamp.

Any other cause. Call your Service Representative. --.

Signals are not generated.

The lamp is off. See "The xenon lamp does not light."

Extremely poor position adjustment Re-adjust the light source position. for light source.

f---

Shutter closed. Open the shutter.

Improper Set the wavelength and bandwidth measurement condition setting.

properly.

Call your Service Representative. Any other cause. -

5-55-4 RF-530 1PC Hardware Manual RF-5301PC Hardware Manual

----- - - --

Troubleshooting Troubleshooting

Table 5-5 Hardware Problems (continued) 5.5 Scanning Problems

1. The scan of data is very noisy (and not within specifications).

Table 5-6 Hardware Errors Related to Scanning

)

Symptom Probable Cause Remedial Action

The xenon lamp does not light.

The xenon lamp switch is off.

Turn on the xenon lamp switch on the right side of the instrument.

Improper wiring contact.

Verify the connection of the high-voltage cord to the positive terminal of the xenon lamp. Be sure to unplug the AC cable before making this connection to prevent the xenon lamp from being turned on accidentally.

Overheated lamp. Leave the lamp OFF for ten (10) minutes to let it cool.

Any other cause. Call your Service Representative.

Items to be checked Remedial Action

Instrument Refer to the instruction manual and check the operation and performance by following the outlined procedures.

Light source The light source may have failed. Replace when necessary.

2. The relative fluorescence intensity is abnormal.

Table 5-7 Hardware Errors Related to Fluorescence

Items to be checked I Remedial Action

D Auto Zero has been selected unintentionally.

I Remove sample, replace with blank and select Auto (The intensity is set with

I Zero again. the cell in the cell holder.) ---- - ------~~~{----------

Wavelength setting is Set the wavelength appropriately.

not appropriate -~----~---~- --~~--

Faulty sample , Prepare the sample correctly.

preparation

Improper cell being used: The glass cell is opaque in the UV region. Use a quartz cell.

Light sensitivity of Use Auto Shutter, increase Scan Speed, and sample decrease Slit Width.

)

RF-5301 PC Hardware Manual 5-75-6 RF-5301PC Hardware Manual

Hardware Manual Index

A Accessories 1-1 Adjusting VRO 2-12

C Cable Connections 2-7

D Dimensions 2-1

F Fuse Replacement 3-2

G Grounding 2-7

H Hardware Communication Trouble 4-2 Hardware Error Messages 4-4 Hardware Installation 2-1

I Initialization Errors 4-1 Installation Site 2-1 Instrument Description 1-2 Instrument Initialization 2-8

L Light Source Position Adjustment

Coarse 2-8 Fine 2-10

o Optical System 1-8

P ) Parts Inspection 1-1

Performance Check 2-14 Power Cable 2-7 Power Supply 2-7 Precautions in Relocating the Unit 3-1

Index

R Room temperature 2-1

S SIN Ratio Check 2-14, 3-7 Scanning Problems 4-7 Self-diagnostic Procedures 4-1 Specifications 1-6

T Troubleshooting Hardware 4-5

w Wavelength Accuracy Check

Emission monochromator 3-3 Excitation monochromator 3-5

Weight ofInstrument 2-1

X Xenon Lamp

Disposal 3-1 Illumination Time Management 3-1 Installation 2-2 Life Time 3-1 Power Switch 2-7 Resetting Illumination Time 2-11

RF-5301PC Hardware Manual I - 1

manual-spectroflourometerrf5301pc

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