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UV VIS Spektralphotometer
SPECORD
SPECORD
SPECORD
200
PC
205
PC
210
PC
Operating
Jena
Analytik Jena AG
Kundendienst
Konrad-Zuse-Str. 1
07745 Jena
Telefon: Hotline:
Fax:
+ 49 (3641) 77-7401
+ 49 (3641) 77-7449
E-Mail: [email protected]
General information about Analytik Jena AG on the internet:
http://www.analytik-jena.de
Copyrights and Trademarks
Microsoft, Windows 98, Windows NT, MS Word, MS Excel are registered trademarks of
Microsoft Corp.
Publication No.:
221:416.23
Edition – March 2003
Technical documentation made by:
Analytik Jena AG
This documentation describes the state of this product at the time of publishing. It need not necessarily agree with future versions of the product.
Subject to change!
© Copyright 2003 Analytik Jena AG
SPECORD ® Contents
Contents
1
Introduction 3
Technical data of the spectrophotometers
.................................................................................... 11
General technical data of SPECORD ®
................................................................... 12
5 Device description and operating principle 13
7 Installation and start-up 23
Care, maintenance, lamp change 35
SPECORD
®
200/205/210 User's Manual – Edition 03/2003
Analytik Jena AG
Page 1
Contents SPECORD ®
Page 2 SPECORD
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Analytik Jena AG
SPECORD ® Introduction
Conventions
1 Introduction
1.1 Conventions
This manual contains the description of the following devices
• SPECORD ® 200
• SPECORD ® 205
• SPECORD ® 210
If the descriptions equally refer to all three models, only the collective term
SPECORD ® will be used. If a property of an individual model shall be particularly stressed, the full name of the model will be mentioned.
In this manual, the following symbols are used to refer you to warnings and notes:
Warning!
Warning messages alert you to a specific procedure or practice which, if not followed correctly, could cause personal injury.
Caution!
Caution messages refer you to procedures which, if not observed, could result in damage to the equipment.
Dangerous electric voltage!
Emission of UV radiation!
Disconnect power cable!
Note
This note must be followed to obtain correct measurement results.
For easier navigation within the manual, the manual uses the following system:
• Chapters and illustrations are numbered consecutively.
• Every illustration has its own caption.
■ This symbol denotes a step of operation.
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Page 3
Introduction
Intended use of the SPECORD®
SPECORD ®
□ This symbol denotes a step of operation being alternative to the previously described and having the same effect or leading to a follow-up step of a branching step of operation.
→ Cross-reference: Refers to another section/illustration of the manual.
1.2 Intended use of the SPECORD
®
The SPECORD ® is a powerful, computer-controlled double-beam spectrophotometer for the measurement of the transmission, absorbance, reflection as well as the energy of liquid and solid samples. It is designed for measurements in the spectral range 190 – 1100 nm.
The double-beam spectrophotometers of the SPECORD ® family provide different spectral resolutions:
SPECORD ® 200
SPECORD ® 205
SPECORD ® 210
1; 2 and 4 nm
1.4 nm
0.5, 1, 2 and 4 nm
The optical system without electromechanical modulator ensures true real-time operation, so that even variations in the absorbance of references can be compensated during the measurement.
The internal wavelength calibration with a holmium oxide filter provides a high wavelength accuracy and reproducibility.
The SPECORD ® complies with the regulations of the DAB (German
Pharmacopoeia) and international regulations, such as PhEur., BP, USP or JPXIII.
In combination with the powerful WinASPECT ® software, the SPECORD ® is particularly suitable for the use in routine laboratories with a high sample throughput, but also provides solutions for special applications, if used in combination with the diverse accessories available.
Page 4 SPECORD
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SPECORD ® notes
For your personal safety and for a trouble-free operation, carefully read this chapter before starting up the SPECORD ® .
Observe all safety notes given in this manual and all messages and notes displayed by the control software on the screen.
In addition, observe the safety notes for system components of other manufacturers
(e.g. PC, printer, autosampler) supplied together with the device.
In particular, you should also observe the safety notes given on the labels and the information on the use, storage and disposal of reagents, reaction cells and the notes on the package inserts of test kits.
The SPECORD ® , including original accessories, may only be used for the applications described in this manual. The manufacturer cannot assume any liability for any other application, including that of individual modules or single parts. This also applies to all service or repair work that is not carried out by authorized service personnel. All warranty claims shall be forfeited.
Local safety regulations!
Observe the local safety regulations relevant to the operation of the device (e.g. labor-safety regulations, regulations for the prevention of and protection against accidents).
References to possible risks given in this manual do not replace the relevant laborsafety regulations that are to be followed.
Personnel!
The SPECORD ® may only be operated by appropriately qualified and trained personnel.
For that, the knowledge of the information provided by this manual is indispensable and taken for granted.
In the case of emergency, disconnect the SPECORD ® and its components from line power by removing the power plug from the power outlet.
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Page 5
Safety notes SPECORD ®
The SPECORD ® is electrically powered. At several parts inside the system, extremely hazardous electrical voltages are accessible!
To ensure Protection Class I (protective earth connection) of the device, connect the power plug of the device only to a power outlet with protective earth conductor. The protective effect must not be undone by the use of an extension cable without protective earth conductor.
Before opening the device or removing any device covers, disconnect the power cable!
Before connecting the SPECORD ® to the power outlet, make sure the line voltage supplied agrees with the operating voltage specified on the rating plate at the rear panel of the device. Operation of the device with any other operating voltage than that specified may result in the destruction of the device.
Only use fuses of the specified type.
Do not operate the device in explosion-risk rooms!
Never look directly or indirectly, e.g. via a mirror, into the radiation emitted by the lamp to avoid the risk of getting conjunctivitis!
Therefore, switch off the lamp for lamp replacement!
Lamp !
Do not grasp functioning halogen and deuterium lamps on their glass bulbs.
Contamination on the bulb affects the radiation properties of the lamps.
Especially protect the beam-exit window of the deuterium lamp.
Make sure to remove the protective cap from the halogen bulb after having inserted it to avoid any risk of fire!
Non-observance will result in damage of the lamp.
Accumulation of heat
Heat accumulation might result in overheating and faults on the device.
Make sure not to cover the ventilation slots of the SPECORD ® !
Before you switch on the SPECORD ® , remove its dust cover!
Page 6 SPECORD
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Analytik Jena AG
SPECORD ® notes
Take care to ensure that no liquids can enter the SPECORD ® to avoid any damage to the device.
Risk of corrosion
Do not set up the device in the vicinity of aggressive vapors, e.g. strongly corrosive acid or caustic vapors! The vapors might corrode the connections, mechanical and optical components of the device.
Avoid exposing the sample compartment to strongly corrosive substances! For the analysis of such samples, use vapor-tight stoppered cells.
After the measurement, do not leave the samples unnecessarily long in the sample compartment of the device!
The SPECORD ® was produced and tested in compliance with the following standards and regulations:
• DIN EN 61010-1 (IEC 1010-1)
• 73/23/EC
• 89/336/EC.
The SPECORD ® meets the requirements as per Protection Type IP 20.
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Page 7
Safety notes SPECORD ®
Page 8 SPECORD
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Analytik Jena AG
SPECORD ® Disposal
3 Disposal
The owner/operator of the SPECORD ® must ensure to dispose of the waste material
(samples) cropping up in the analyses in accordance with the relevant legal and local regulations.
When the service life of the device is over, dispose of the device with its electronic components as electronic scrap observing the relevant regulations.
You can also return the SPECORD ® to Analytik Jena AG for disposal. Please contact our Technical Service.
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Page 9
Disposal SPECORD ®
Page 10 SPECORD
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SPECORD ® Technical data of the spectrophotometers
Optical data of SPECORD®
4 Technical data of the spectrophotometers
4.1 Optical data of SPECORD
®
Principle
Optics
Light sources
SPECORD
®
200 / 205 / 210
Double-beam spectrophotometer with two largearea Peltier temperature-controlled photodiodes
Monochromator with holographic concave grating
Light split into two beams by a beam-splitting plate
Deuterium lamp and halogen lamp, pre-aligned
Wavelength range
Photometric range
Wavelength accuracy
Wavelength reproducibility
Stray light
Photometric accuracy VIS
Photometric accuracy UV
Photometric reproducibility
Long term stability
Baseline stability
Zero-line of transmission
RMS noise
190 ... 1100 nm
- 3 ... + 3 A
± 0.5 nm at 360,9 nm with holmium glass filter
*
± 0.1 nm (5 measurements)
< 0.5 % T at 200 nm (KCl)
*
< 0.05 % T at 220 nm (NaJ, ASTM) *
< 0.05 % T at 340 nm (NaNO
2
, ASTM)
*
± 0.005 A at A = 1
± 0.005 A at A = 1; potassium dichromate
± 0.0005 A/h at A = 1
± 0.001 A/h at 500 nm (1 h warm-up)
± 0.001 A from 200 to 800 nm with slit 2 nm
± 0.03 %T
± 0.0001
Scanning speed 30, 60, 120, 300, 600, 1200, 3000, 6000 nm/min
*)allowing for tolerances of used standard
Spectral bandwith
Toluene / hexan resolution
SPECORD
®
200 SPECORD
1 / 2 / 4 nm, variable 1.4 nm
®
205 SPECORD
®
0.5 / 1 / 2 / 4 nm, variable
210
> 2.1 > 1.7 > 2.1
Overview 4-1 Technical data of SPECORD ® 200
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Page 11
Technical data of the spectrophotometers
General technical data of SPECORD®
SPECORD ®
4.2 General technical data of SPECORD
®
Weight
Footprint (W x D)
Dimensions (W x H x D)
Line voltage
Line frequency
Power consumption
Fuses:
Line fuses
Radio noise suppression
Noise immunity
Protection Type
Data interface
PC requirements for software:
Aspect Plus and WinASPECT
Overview 4-2 General technical data of SPECORD ®
18 kg approx. 1200 x 750 mm 2 with PC
680 x 240 x 620 mm 3
230 VAC ±10 % and switchable to
115 VAC ±10 % (by Technical Service)
47 ... 63 Hz
195 VA
230 VAC: T 3.15 AH/250V, Type 19181
(Wickmann)
115 VAC: T 3,15 AH/250V, Type19181
(Wickmann) as per EN 55011 Class A as per DIN EN 50082-1
IP 20
RS-232 port
MS Windows 2000 operating system or higher
Page 12 SPECORD
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SPECORD ® Device description and operating principle
Mechanical design of SPECORD®
5 Device description and operating principle
5.1 Mechanical design of SPECORD
®
Fig. 5-1 Mechanical design of SPECORD ®
2 Desiccator
3 Cover of spectrometer system and photometer section 8
4
5
Device control
Power supply module
9
10
The major subassemblies of the SPECORD ® are:
Light sources
(1)
Spectrometer system
Support plate
Holder for cells
Sample compartment
Halogen lamp and deuterium lamp generate the light that is monochromatized in the spectrometer system. Then, it passes through the sample.
The spectrometer system is protected against extraneous light and dust by cover
(3)
. The desiccator
(2) regulates the humidity inside the system.
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Page 13
Device description and operating principle
Mechanical design of SPECORD®
SPECORD
Photometer section This subassembly serves to split the light exiting the monochromator into sample and reference beam. The optical system shapes the beam cross-section in the sample compartment. The photometer section, too, is protected by cover
(3)
.
Sample compartment
(10)
The sample compartment contains two pairs of carrier rods for the accommodation of various accessory units.
To the support plate
(8)
, two holders for the accommodation of cells
(9)
and the detector board are mounted.
Detector board
(6)
Two photodiodes are used as radiation detectors, which on the SPECORD ® 200/210 are Peltier temperaturecontrolled.
Power supply module
(5)
Device control computer
(4)
The power supply modules supply the electrical voltage to the electronic system and the fans for the thermoelectric temperature control of the detectors on the SPECORD ® 200/210.
The device control computer coordinates the interaction of the subassemblies involved in the measurement processes.
®
Page 14 SPECORD
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SPECORD ®
5.2 Design of subassemblies
Device description and operating principle
Design of subassemblies
Fig. 5-2 Lamp compartment (without cover)
1 Halogen lamp in protective housing
2 D
2
E lamp compartment
4
5
Toric illuminating mirror
Setscrew for mirror adjustment
The light sources used are a deuterium lamp
(2)
for the UV region and a halogen lamp
(1)
for the VIS region of the spectrum.
Depending on the position of reflecting mirror
(3)
, which is mounted onto a moving magnet, the radiation of either deuterium or halogen lamp is sent onto the entrance slit of the monochromator. You can choose the wavelength at which the lamp is changed over a wide range using the WinASPECT ® control and analysis software.
The toric mirror
(4)
serves for imaging the light sources onto the entrance slit of the monochromator. To obtain the maximum possible energy of the deuterium lamp for the measurement, you can sensitively adjust the setscrew for mirror adjustment
(5)
.
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Page 15
Device description and operating principle
Design of subassemblies
SPECORD
5.2.2 Spectrometer system and photometer section
SPECORD 200 – Optical Diagram
Concave grating
Entrance slit
Exit slit
Plane mirror
Filter wheel
Reference cell
Beam splitter
Sample compartment
Sample cell Halogen lamp
Swivel mirror
Quartz-coated toric mirrors
Cavity for turbid samples
Detector
Fig. 5-3 Schematic setup – Optical diagram of SPECORD ®
The spectrometer system with the optical elements illustrated above – filter wheel, concave grating and slit assembly – works as monochromator.
The filter wheel contains the following filters:
4 color glass filters
Holmium filter
2 blank positions
Used to suppress unwanted radiation in the monochromator.
Standard for the automatic recalibration of wavelengths.
Block position Needed for the generation of measured data.
The entrance and exit slits of the spectrometer system are mounted to the slit carrier. Depending on the device model, the slits allow the following spectral slit widths:
SPECORD ® 200
SPECORD ® 205
SPECORD ® 210
1, 2, 4 nm
1.4 nm
0.5, 1, 2, 4 nm.
The imaging grating disperses the incident light and spreads it out into a spectrum.
®
Page 16 SPECORD
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SPECORD ® Device description and operating principle
Design of subassemblies
Computer-controlled stepper motors drive the filter wheel, the slit carrier and the linear actuator for moving the grating. Because of the little number of moving parts used in the spectrometer system, the SPECORD ® ensures a high reliability of its optical parameters.
In the photometer section, the mirror system divides the beam coming from the monochromator into sample and reference beam. The imaging mirrors shape the beam to the cross-sections needed in the sample compartment.
Spectrometer system and photometer section are protected against dust and reagents by a cover. However, corrosive reagents or strongly evaporating liquids should be inserted in the sample compartment only in stoppered cells.
4
3
2
1
5
6
7
8
9
10
11
1
2
3
4
5
6
Fig. 5-4 Sample compartment
Sample beam path with 2 carrier rods
Reference beam path with 2 carrier rods
Connector for sipper and cell changer
Reserve connector
Stopper for optical fiber of measuring probe
Conduits for coolant hoses
7
8
9
10
11
Mount for cell holder
Receptacle for cells with turbid samples
Mount for cell holder
Conduit for sample drain hose
Conduits for sample-aspirating hoses (sipper)
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Page 17
Device description and operating principle
Design of subassemblies
SPECORD ®
Sample
(1)
and reference beam
(2)
enter the sample compartment through the lefthand wall.
The mounts for the cell holders
(7)
,
(8)
are arranged in front of the exit windows in the right-hand sample compartment wall.
The two pairs of carrier rods serve to accommodate the universal holder and other accessories, which easily clamp to the rods.
The receptacles for the cells
(8)
with turbid samples are located directly in front of the detector at the right-hand sample-compartment wall.
Two 9-pin connectors
(3), (4)
allow the connection of electrically driven accessories, such as the automatic temperature-controlled cell changer or the sipper system.
The optical fibers of the measuring probe or the cables of the Peltier temperaturecontrolled cell holder or the cell changer are threaded through the recess in the rear wall of the sample compartment
(5)
.
The three conduits
(6,11)
in the right-hand sample compartment wall are used for threading through the sample drain hose and two coolant hoses for the thermostat.
Two openings in the front of the device cover are provided for the aspiration tubes of the super sipper system.
The illustration below shows the geometrical dimensions of the sample compartment.
Page 18 SPECORD
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SPECORD ®
193
Device description and operating principle
Design of subassemblies
2
1
Fig. 5-5 Dimensions of sample compartment
1 Front side of sample compartment
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Device description and operating principle
Design of subassemblies
SPECORD ®
Page 20 SPECORD
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SPECORD ® requirements
Considering the dimensions of the SPECORD ® and a clearance of approximately
100 mm to the sides and the front, the device needs a bench space of at least
860 x 720 mm.
660
Fig. 6-1 Dimensions of SPECORD ®
520
Caution!
Do not cover the ventilation slots of the device!
Do not place any objects on the device!
Do not operate the device in explosion-risk rooms!
Keep aggressive vapors, e.g. strongly corrosive acid or caustic vapors away from the vicinity of the device.
The installation site of the SPECORD ® must meet the following requirements:
• The place should be free of draft, dust, corrosive vapors as well as vibrations.
• Do not set up the SPECORD ® near electromagnetic fields (e.g. of motors).
• Avoid dripping or splashing water near the instrument.
• Do not expose the device to direct sunlight or the radiation of heaters.
• Temperature range: + 15 ... + 35 °C
• Humidity: up to 90 % (at + 30 °C)
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Page 21
Installation requirements SPECORD ®
Page 22 SPECORD
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SPECORD ® and
Connectors and display elements
7 Installation and start-up
7.1 Connectors and display elements
The connectors and display elements of the SPECORD ® are conveniently located on the front and the side panels of the SPECORD ® .
The LEDs indicating Power ON and lamp standby are located on the left side of the front panel of the SPECORD ® .
1 2 3
Fig. 7-1 Display elements on front panel
1 Power ON indicator LED (green)
2 D
2
E lamp ON indicator LED (yellow)
3 Halogen lamp ON indicator LED (red)
The LEDs light when the SPECORD ® has been switched on and the lamps are on.
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Page 23
Installation and start-up
Connectors and display elements
SPECORD ®
The line power input connector with fuse holder and the power switch are located on the left-hand side panel of the device.
4 3 2 1
Fig. 7-2 Connectors on left-hand side panel
1
2
Power switch 3
Power input connector 4
Fuse holder for line fuse
Nameplate
On the right-hand side panel of the device, the following connectors are located:
RS 232 and USB ports for the connection of a PC and the connectors for the xyz autosampler and the control of the Peltier temperature-controlled cell holder.
Page 24
4 3 2 1
Fig. 7-3 Connectors on right-hand side panel
1
2
RS 232 port for PC
USB port for PC
3
4
Connector for xyz autosampler
Connector for control of Peltier temperature-controlled cell holder
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SPECORD ® and
Removing the transport lock
7.2 Removing the transport lock
The SPECORD ® is equipped with a transport lock to prevent damage to the device and its optical system during transportation. The lock screw is located at the rear right on the bottom part of the device.
Transport lock
1
Fig. 7-4 Transport lock on SPECORD ®
1 Transport screw
Note
The transport lock screw is not removed from the device, but is left in its holder in the SPECORD ® .
If the device must be transported again or returned for repair to Analytik Jena AG, lock the transport lock again.
Releasing the transport lock
Using a screwdriver turn the transport lock screw
(1)
anti-clockwise as far as it will go.
Locking the transport lock
First, initialize the device to bring the monochromator into its starting position.
Switch the device off.
Using a screwdriver, turn the transport lock screw
(1)
clockwise as far as it will go.
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Installation and start-up
Connecting the SPECORD®
SPECORD ®
7.3 Connecting the SPECORD
®
Observe correct position of device!
Move the SPECORD ® only in upright position (observe label on transport case).
Do not turn the device upside down.
Loosen the transport lock screw located on the rear left of the SPECORD ® .
Electric shock
Before connecting the SPECORD ® and the PC to line power, make sure the available line voltage agrees with the operating voltage specified on the type labels.
Operation of the devices on line voltages other than the specified operating voltage may result in their destruction.
Standard equipment
The standard equipment of the SPECORD ® includes the following items:
• 2 cell holders
• Installation CD-ROM of WinASPECT ®
• Spare halogen lamp
basic module
• Deuterium lamp
• Power cable
• PC – SPECORD ® connecting cable
• Spare fuses 5 x 20 T 3.15 A L
• User's Manuals for the SPECORD ® , the accessories and the
WinASPECT ® control and analysis software.
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SPECORD ® Installation
Connecting the SPECORD®
Connecting SPECORD ® and PC
Remove the device from its transport packaging and remove the plastic cover.
Wait until the device has adjusted to the ambient temperature.
Remove the foamed plastic packaging from the SPECORD ® sample compartment. The packaging contains the items included in the standard equipment (see above) and the installation disks for the WinASPECT ® optional module you ordered.
Install the software on the PC ( → Refer to WinASPECT ® User's Manual).
Insert the deuterium lamp following the instructions given in Section
Connect the SPECORD ® ( → see
7.1 Connectors and display elements p. 23 ) to
the PC (free COM port) using the supplied connecting cable.
Connect one power cable each to the SPECORD ® and the PC. Connect the power cables of the SPECORD ® and the PC to power outlets that are connected to the same phase of the line power supply (multiple socket outlet, if possible).
Note
When required, align the lamps following the instructions given in Section
Changing lamps, p. 36 after start-up.
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Installation and start-up
Start-up
SPECORD ®
7.4 Start-up
Do not cover ventilation slots of the device!
Take care to ensure that the ventilation slots on the top and on the right and left bottom of the SPECORD ® are not covered. Do not place any objects in front of the openings. The suction intakes for the two fans on the bottom of the device must be kept free.
Caution!
Do not place any objects, especially no containers with liquids, on the SPECORD ® .
Start WinASPECT ® software by a click on the program icon
Windows desktop or by clicking the Start button on the taskbar:
< Start I Programs I WinASPECT I WinASPECT > .
on the
Using the power switch on the left panel of the device, switch the SPECORD ® on ( →
Refer to Fig. 7-2 Connectors on left-hand side panel, p. 24 ).
The green Power ON LED on the front panel of the device lights.
( →
Refer to Fig. 7-1 Display elements on front panel, p. 23 ).
In WinASPECT ® software, select the COM port for the SPECORD ® – PC connection:
Activate the menu command < Measurement I Set Parameters > to open the window of the device driver SPECORD xxx ...
.
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SPECORD ® and
Start-up
Fig. 7-5 Dialog box of SPECORD ® 200 device driver
Click on the Device tab.
From the COM Port list box, select the COM port of your PC, to which the
SPECORD ® is connected.
Click on [OK] to close the device driver window.
Note
The selected COM port will be saved and remain set until you change the COM port setting. Thus, you need not select it after every restart of the device.
Initialize the device:
Establish communication between SPECORD ® and PC using the menu command < Measurement I Initialize Device > .
The SPECORD ® is now ready for taking measurements.
Note
Please note that the SPECORD ® reaches thermal stability only after a warm-up time of one hour. Therefore, you should not start precision measurements unless the device has warmed up.
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Installation and start-up
Switching the device off
SPECORD ®
7.5 Switching the device off
7.5.1 Switching the deuterium lamp off
If you have worked with the deuterium lamp and you are sure that you do not need it any longer this day, you can switch it off by software control following this procedure:
In WinASPECT ® , activate the device driver with menu command
< Measurement I Set Parameters > .
Activate the Device tab.
In the Lamp change at field, deactivate the D
2
E automatically function.
Close the device driver window by a click on [OK] .
Reinitialize the device using the following menu command: < Measurement I
Initialize Device > .
A query appears on the screen asking you if you want to switch on the UV lamp.
Click the [No] button.
The UV lamp goes out.
7.5.2 Switching the SPECORD ® off
We recommend that the SPECORD ® be powered down by software control after you have finished taking measurements:
Exit WinASPECT ® using menu command < File I Exit > .
Then, shut down the computer.
Finally, switch the SPECORD ® off with the power switch.
Note
If you have finished the measurements on the SPECORD ® but want to analyze the obtained results on the PC, you can also switch off the SPECORD ® without shutting down the computer before.
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SPECORD ® Accessories
Standard cell holders
8 Accessories
8.1 Standard cell holders
The standard equipment of the SPECORD ® includes two cell holders for cells of up to 50 mm pathlength.
The mount for the cell holder is located on the right-hand sample compartment wall in front of the beam-exit window ( →
Fig. 5-4 Sample compartment, p. 17 ). The cell
holder is designed for cells having a pathlength of up to 50 mm and a width of
12.5 mm.
Fig. 8-1 Standard cell holder
1
2
Cell support
Guide
Push the cell holder with its guide
(2)
from top onto the cell-holder mount.
The beam transmits the cells at a height of approximately 5 to 15 mm above the support of the cell holder.
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Accessories
Receptacle for cells with turbid samples
SPECORD ®
Inserting the cell
Fill the sample into the cell up to a level of at least 20 mm.
Insert the cell so it rests against the right-hand support surface of the cell holder.
Correct
Fig. 8-2 Inserting the cell
Note
In absorbance measurements, the pathlength is one of the crucial factors.
Therefore, it is important to insert all samples (samples and references) in the same location and position. In this way, you can avoid measurement errors caused by angular differences and parallel offset of the beam.
8.2 Receptacle for cells with turbid samples
In the measurement of strongly turbid samples, a considerable portion of the radiation does not exit the sample cell straightly, but is scattered within a solid angle.
For photometrically accurate measurements it is necessary that the detector capture the total scattered radiation. For this purpose, the sample and the reference substance must be arranged as close to the detector as possible.
Therefore, the receptacles for the cells with scattering samples are located in the right-hand sample-compartment wall of the SPECORD ® in front of the photodiode detectors (
). The receptacles can accommodate standard cells of
10 mm pathlength.
Remove the foamed-plastic caps covering the cell receptacles and insert the cells for the analysis.
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SPECORD ® Accessories
After the measurement is finished, make sure to cover the cell receptacles again with the foamed-plastic caps. If you fail to do so, extraneous light might be incident on the detector and distort the results of the measurements.
Optionally the following accessories are available for the SPECORD :
• Universal cell holder
• Thermostatted cell holder, water-cooled
• Thermostatted cell holder; Peltier-controlled
• Adjustable cell holder for micro, submicro or HPLC cells
• 6-cell changer, water-cooled
• 6-cell changer, Peltier-controlled
• Holder for cylindrical cells of up to 100 mm
• Holder for round cells
• Holder for solid samples
• 11° ... 60° variable Angle Reflectance Accessory
• Absolute Reflectance Accessory
• Universal sipper system with flow cell and peristaltic pump
• XYZ autosampler
• Fiber coupling with measuring probes
• 75-mm integrating sphere for transmission and diffuse reflectance
• PTC 100, Peltier temperature-controlled cell holder
• PTC 600, Peltier temperature-controlled 6-cell changer
• SMA fiber connector
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Accessories
Additional accessories
SPECORD ®
Page 34 SPECORD
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SPECORD ®
9 Care, maintenance, lamp change
Care, maintenance, lamp change
Care and maintenance
The SPECORD is largely free of maintenance.
To ensure your laboratory certification with device validation, Analytik Jena AG offers you a service/maintenance agreement.
User care and maintenance is limited to the following operations:
• Cleaning of sample compartment and device casing
• Lamp change
• Change of line fuses
• Change of desiccator
You should only use spares from Analytik Jena AG .
You can order consumables and wear parts by phone from our Service Department:
Hotline No.: + 49 3641-77-7401
In the case of malfunction of the device, please contact our Service Department. For the address, refer to the → inside cover page .
9.2 Cleaning
Avoid keeping filled cells unnecessarily long in the sample compartment to prevent the spectrometer from being affected by any solvent vapors.
Wipe off spilt samples in the sample compartment or on accessory units instantly with cleaning tissue.
Wipe off contamination on the instrument with a soft, clean cloth slightly moistened with a commercially available, neutral detergent.
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Care, maintenance, lamp change
Changing lamps
SPECORD
9.3.1 Note on the service life of lamps
The service life of lamps is:
• Halogen lamp: > 500 h (at 5.0 V operating voltage)
• Deuterium lamp: > 1000 h
The service life of the lamps is reduced, if the SPECORD is frequently switched on and off. This particularly applies to the deuterium lamp, because of the relatively high ignition voltage required.
The following rule applies as criterion for the service life of the deuterium lamp:
With one daily ON/OFF switching operation, its radiation intensity is allowed to decrease to 50% after 1000 hours.
The deuterium lamp must be changed, if its heating coil has burnt out, its energy is insufficient or the operating hours counter indicates 2000 h.
9.3.2 Opening the flap of the lamp compartment
The flap of the lamp compartment (front left corner of device cover) is to be opened to check the operating hours of the deuterium lamp, change the lamps or change the desiccator.
Switch the SPECORD ® off and allow the lamps to cool down for at least five minutes.
Release the lock
( 2 )
of the flap of the lamp compartment by folding the lock frontward so it sticks out from the SPECORD ® approximately vertically.
Remove the flap of the lamp compartment by lifting it from below by 1 to 2 mm and then pulling it off to the left.
®
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SPECORD ® Care, maintenance, lamp change
2 1
Opening the flap of the lamp compartment
1
2
Flap of lamp compartment
Lock
Fig. 9-1
In the open lamp compartment, you can see the deuterium lamp at the front left and the halogen lamp. Both lamps are enclosed by a protective cover.
4 3 2
Fig. 9-2 Open lamp compartment
1
2
Protective cover of halogen lamp
Knurled screw of halogen lamp sleeve
1
3
4
Protective cover of deuterium lamp
Top part of deuterium lamp cover
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Care, maintenance, lamp change
Changing lamps
SPECORD ®
9.3.3 Changing the deuterium lamp
Risk of electric shock!
Before changing the deuterium lamp, make sure to switch the device off with the power switch.
Caution: Risk of burns!
Allow the deuterium lamp to cool down to avoid the risk of burns!
Emitted UV radiation!
Never look directly or indirectly, e.g. via a mirror, into the radiation emitted by the lamp to avoid the risk of getting conjunctivitis!
Dirt on beam exit window!
Do not touch the glass bulb of the new deuterium lamp. Particularly avoid contamination on the quartz glass beam exit window! If you touched the glass bulb with your fingers, wipe the fingerprints off with a clean, lintfree cloth and pure alcohol. The performance of the lamp will deteriorate by contamination.
Before you can change the lamp, remove the top part of the protective cover (
(4)
) by pulling it upward.
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SPECORD ® Care, maintenance, lamp change
6 7 8
5
4
3
9
10
2 1 12 11
Fig. 9-3 Lamp protective cover partly removed
1 Holder for halogen lamp
2 Knurled screws
3 Halogen lamp
4 Deuterium lamp
5 Connector
6 Spring-loaded straps
7
8
9
10
11
12
Operating hours counter
Quick-lock nuts
Guiding groove
Illuminating mirror
Setscrew
Fastening screws for halogen lamp holder
Disconnect the three-pin connector
(5)
by compressing the lateral straps
(6) and taking the connector off. Release the quick-lock nuts
(8)
and pull out the defective deuterium lamp
(4)
.
Remove the new deuterium lamp from its packaging and insert it in the lamp holder taking care that the locating pin of the lamp holder fits into groove
(9)
of the lamp base.
Screw down the deuterium lamp by means of both quick-lock nuts.
Fasten the connector to the lamp.
Finally, reattach the top part of the protective cover.
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Care, maintenance, lamp change
Changing lamps
SPECORD ®
Fine alignment of deuterium lamp
Despite stringent manufacturing tolerances of the deuterium lamps, it may be necessary to realign the lamp after lamp change to ensure that maximum intensity of the lamp is incident on the entrance slit of the monochromator. For this purpose, you can slightly move the illuminating error
(10)
by means of setscrew
(11)
.
Switch the SPECORD ® on and initialize it.
To this end, start WinASPECT ® and activate the following menu command:
<Measurement I Initialize Device> .
Set up a parameter record containing the following parameters:
Integration time 0.5 s
Display Energy
For the alignment, the protective cover of the halogen lamp must be kept in place.
Start the measurement with the sample compartment kept closed. Keep the flap of the lamp compartment open.
Sensitively turn the setscrew
(11)
in both directions until the detected energy reaches its maximum.
This adjustment also influences the alignment of the halogen lamp. However, the variation is comparatively small and normally negligible.
Finally, close the flap of the lamp compartment.
Note
Please note that the deuterium lamp needs a warm-up of one hour after ignition to reach full thermal stability.
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SPECORD ® Care, maintenance, lamp change
9.3.4 Changing the halogen lamp
Before changing the halogen lamp, make sure to switch the device off with the power switch.
Caution: Risk of burns!
Allow the halogen lamp to cool down to avoid the risk of burns!
Warning!
Never look into the lighting lamp as the radiation may cause eye injury!
Caution!
Do not touch the glass bulb of the lamp to avoid any contamination affecting its performance!
After having opened the flap of the lamp compartment, you can see the protective cover of the halogen lamp.
Loosen the knurled screw (
(2)
) and remove the protective cover by lifting it off.
Loosen the two clamping screws (
Fig. 9-3
(2)
).
Pull the defective halogen lamp (
Fig. 9-3
(3)
) out of its holder
(1)
.
Remove the new halogen lamp from its packaging, but keep the protective sheath attached.
Insert the new halogen lamp taking care to ensure that the notch at its base encloses the pin in the bottom part of the holder.
Caution!
Make sure to remove the protective sheath of the halogen lamp now! Failure to do so involves the risk of fire and lamp damage. Do not touch the glass bulb of the new halogen lamp! Any contamination will impair the lamp performance.
Reattach the protective cover of the halogen lamp and refasten it.
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Care, maintenance, lamp change
Changing lamps
SPECORD ®
Fine alignment of halogen lamp
Check the alignment of the halogen lamp.
For this purpose, switch the SPECORD ® on and initialize it.
To this end, start WinASPECT ® and activate the following menu command:
< Measurement I Initialize Device > .
Exit WinASPECT ® to run the Service Check routine.
Activate the Service Check routine as follows:
Click on the Start button of the Windows taskbar. In the Programs folder, click on the WinASPECT folder. There, click on the Service xxx command. This will bring up the SPECORD xxx - Service Check dialog box.
Click on the Zeroth Order button and choose the halogen lamp ( HL – Lamp ).
View the image of the sample beam in the sample compartment by holding a white sheet of paper in the plane where normally the cell is placed.
There, a 7 – 8 mm high and 1 – 2 mm wide light spot should be visible that is evenly illuminated from top to bottom.
If you find that the light spot on the sheet of paper is badly uneven, verify that the halogen lamp is correctly seated.
If you are not satisfied with the alignment of the halogen lamp, loosen the fastening screws (
) and move the lamp sensitively while running an energy measurement as described above for the fine alignment of the deuterium lamp. In this case, the ideal wavelength is 500 nm.
Note
Please note that the halogen lamp needs a warm-up of about one hour after switch on to reach full thermal stability.
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SPECORD ®
9.4 Changing the desiccator
Care, maintenance, lamp change
Changing the desiccator
Before changing the desiccator, switch the SPECORD ® off with the power switch and disconnect the power cable from the power input connector of the SPECORD ® .
The desiccator protects the optical system of the SPECORD ® against too high air humidity. The desiccator is accessible, when the lamp compartment has been opened (
→
Refer to
Especially in tropical countries, the adsorption capacity of the desiccator should be checked regularly. The adsorption capacity of the desiccator is exhausted, if the color of the indicator paper in the inspection window has changed from blue to pinkyellow.
For changing the desiccator, follow this procedure:
Open the flap of the lamp compartment by folding the lock frontward so it sticks out vertically. Lift the flap from below by 1 to 2 mm and then pull it off to the left.
Using a flat tool, such as an appropriate coin, unscrew the desiccator from its holder.
Remove the new desiccator from the packaging and screw it into the holder.
Finally, close the flap of the lamp compartment.
Used up desiccators can be reused after heating them up for five hours in a drying oven. New desiccators are available from our Service Department ( → for the address, refer to the inside cover page).
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Page 43
Care, maintenance, lamp change
Changing fuses
SPECORD ®
If the line fuses are defective, you can change them yourself.
Risk of electric shock!
Before changing the fuses, make sure to switch the SPECORD ® off with the power switch and disconnect the power cable from the power input connector of the device.
Remove the power cable from the SPECORD ® .
Open the fuse holder (
→
by pulling on its lid.
Replace the defective line fuses.
Make sure to use only the following fuse types:
T 3.15 H/250 V, Type 19181 for line voltages of 150 VAC and 230 VAC.
Close the fuse holder again.
Reconnect the power cable to the power input connector of the SPECORD ® and the power outlet.
Switch the SPECORD ® on again.
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SPECORD ® Index to Illustrations
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Page 45
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