Analytik Jena SPECORD 200 User manual

SPECORD®PC
200 / 205 / 210 / 250
UV VIS Spectrophotometer

Analytik Jena AG
Kundendienst
Konrad-Zuse-Str. 1
07745 Jena
Phone: Hotline: + 49 (0) 3641 77 74 07
Fax: + 49 (0) 3641 77 74 49
E-Mail: [email protected]
General information about Analytik Jena AG
on the internet: http://www.analytik-jena.de
Copyrights and Trademarks
Microsoft, Windows XP, Windows NT, Windows 2000, MS Excel are registered trademarks of Microsoft
Corp.
Publication No.: 221:416.23
Edition – April 2005
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 2005 Analytik Jena AG

SPECORD®Contents
Contents
1 Introduction .....................................................................3
1.1 Intended use of the SPECORD.............................................................3
1.2 Notes on the User's Manual..................................................................4
2 Safety notes .....................................................................5
2.1 Warning labels on SPECORD...............................................................5
2.2 General safety regulations ....................................................................5
3 Technical data of the spectrophotometers ...................9
3.1 Optical data of SPECORD ....................................................................9
3.2 General technical data of SPECORD .................................................11
4 Device description and operating principle ................13
4.1 Mechanical design of SPECORD .......................................................13
4.2 Design of subassemblies ....................................................................14
4.2.1 Light sources..................................................................................................14
4.2.2 Spectrometer system and photometer section ...............................................16
4.2.3 Sample compartment .....................................................................................17
5 Installation and transport conditions ..........................19
6 Installation and start-up................................................21
6.1 Connectors and display elements.......................................................21
6.2 Removing the transport lock ...............................................................23
6.3 Connecting the SPECORD .................................................................24
6.4 Start-up................................................................................................25
6.5 Switching the device off ......................................................................26
6.5.1 Switching the deuterium lamp off ...................................................................26
6.5.2 Switching the SPECORD off ..........................................................................26
7 Accessories ...................................................................27
7.1 Standard cell holders ..........................................................................27
7.2 Receptacle for cells with turbid samples.............................................28
7.3 Additional accessories ........................................................................29
8 Care, maintenance, lamp change.................................31
8.1 Care and maintenance........................................................................31
8.2 Cleaning ..............................................................................................31
8.3 Changing lamps ..................................................................................32
8.3.1 Note on the service life of lamps ....................................................................32
8.3.2 Opening the flap of the lamp compartment ....................................................32
8.3.3 Changing the deuterium lamp ........................................................................35
8.3.4 Changing the halogen lamp ...........................................................................37
8.4 Changing the desiccator .....................................................................39
8.5 Changing fuses ...................................................................................39
9 Disposal .........................................................................41
10 Index to Illustrations .....................................................43
11 Index to Overviews........................................................43
SPECORD® 200/205/210/250 User's Manual – Edition 04/2005 Page 1
Analytik Jena AG

SPECORD®Introduction
Intended use of the SPECORD
1 Introduction
1.1 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 1; 2 and 4 nm
SPECORD®205 1.4 nm
SPECORD®210 0.5, 1, 2 and 4 nm
SPECORD®250 0.5; 1; 2 and 4 nm, with premonochromator
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.
SPECORD® 200/205/210/250 User's Manual – Edition 04/2005 Page 3
Analytik Jena AG

Introduction SPECORD®
Notes on the User's Manual
1.2 Notes on the User's Manual
This manual contains the description of the following devices
• SPECORD®200
• SPECORD®205
• SPECORD®210
• SPECORD®250
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.
• Steps of operation are numbered.
• Cross-references are marked by an arrow (e.g. →Intended use of the
SPECORD p.3)
Page 4 SPECORD®200/205/210/250 User's Manual – Edition 04/2005
Analytik Jena AG

SPECORD®Safety notes
Warning labels on SPECORD
2 Safety notes
2.1 Warning labels on SPECORD
Observe the warning labels on the SPECORD®!
The following warning labels have been affixed to the lamp housings of the SPECORD®:
Danger! UV radiation!
Do not look directly or indirectly via a mirror into the radiation emitted by the UV lamp.
The lamp radiation may cause conjunctivitis!
Danger! Hot surface!
When lamps are switched on, their covers heat up strongly. If you intend to change
the lamps or open the lamp covers, switch the lamps off and allow for a sufficient cool-
down time.
2.2 General safety regulations
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.
Intended use!
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 labor-
safety 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.
SPECORD® 200/205/210/250 User's Manual – Edition 04/2005 Page 5
Analytik Jena AG

Safety notes SPECORD®
General safety regulations
Emergency stop!
In the case of emergency, disconnect the SPECORD®and its components from line
power by removing the power plug from the power outlet.
Electric shocks!
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!
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!
Therefore, switch off the lamp for lamp replacement!
Lamp damage!
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!
Handling liquids
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!
Page 6 SPECORD®200/205/210/250 User's Manual – Edition 04/2005
Analytik Jena AG

SPECORD®Safety notes
General safety regulations
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.
SPECORD® 200/205/210/250 User's Manual – Edition 04/2005 Page 7
Analytik Jena AG

SPECORD®Technical data of the spectrophotometers
Optical data of SPECORD
3 Technical data of the spectrophotometers
3.1 Optical data of SPECORD
Technical Data SPECORD®200 / 205 /210
Principle Double-beam spectrophotometer with two large-area
photodiodes
Optics Monochromator with holographic concave grating
Light split into two beams by a beam-splitting plate
Wavelength range 190-1100nm
Photometric display range -8A ... 8A
Photometric measuring range -3A ... 3A
Wavelength accuracy
(with holmium oxide filter)*
≤±0.5nm
Wavelength reproducibility
(with holmium oxide filter)*
≤±0.05nm
Photometric accuracy VIS
at 546nm with Hellma F4
neutral-density filter
≤±0.005
Photometric accuracy UV
with potassium dichromate as per
Ph.Eur.
≤±0.01
Stray light at 200nm
(KCl Merck 1.08164.0001)
≤0.5%T
Stray light at 220nm (NaI) ≤0.05%T
Stray light at 240nm (NaI) ≤0.05%
Stray light at 340nm (NaNO2) ≤0.05%T
Baseline noise at 500nm ≤0.00015 (RMS)
Long-term stability at 500nm ≤±0.001
Scanning speed up to 6000nm/min
* allowing for tolerances of used standard
SPECORD® 200/205/210/250 User's Manual – Edition 04/2005 Page 9
Analytik Jena AG

Technical data of the spectrophotometers SPECORD®
Optical data of SPECORD
Technical Data SPECORD®250
Optical principle Double-beam spectrophotometer with two large-area
photodiodes
Optics Premonochromator and monochromator with holographic
concave grating
Light split into two beams by a beam-splitting plate
Wavelength range 190-1100nm
Photometric display range -8A … 8A
Photometric measuring range -4A … 4A
Wavelength accuracy
(with holmium oxide filter)*
≤±0.5nm
Wavelength reproducibility
(with holmium oxide filter)*
≤±0.05nm
Photometric accuracy VIS
at 546nm with Hellma F4
neutral-density filter
≤±0.005
Photometric accuracy UV
with potassium dichromate as per
Ph.Eur.
≤±0.01
Stray light at 200nm
(KCl Merck 1.08164.0001)
≤0.2%T
Stray light at 220nm (NaI) ≤0.008%T
Stray light at 240nm (NaI) ≤0.008%
Stray light at 340nm (NaNO2) ≤0.008%T
Baseline noise at 500nm ≤0.00015 (RMS)
Long-term stability at 500nm ≤±0.001
Scanning speed up to 6000nm/min
* allowing for tolerances of used standards
SPECORD®200 SPECORD®205 SPECORD®210 SPECORD®250
Spectral
bandwidth
1; 2; 4 nm variable 1.4 nm 0.5; 1; 2; 4 nm 0.5; 1; 2; 4 nm
Toluene / hexane
resolution
> 2.1 > 1.7 > 2.1 > 2.1
Overview 3-1 Technical data of SPECORD®200
Page 10 SPECORD®200/205/210/250 User's Manual – Edition 04/2005
Analytik Jena AG

SPECORD®Technical data of the spectrophotometers
General technical data of SPECORD
3.2 General technical data of SPECORD
Weight 23.5 kg
Footprint (W x D) ca. 1200 x 750 mm2 mit PC
Dimensions (W x H x D) 680 x 240 x 620 mm3
Line voltage 230 VAC ±10 % or
115 VAC ±10 % (switchable by service)
Line frequency 47 ... 63 Hz
Power consumption 200 VA
Fuses:
Line fuses
230 V~: T 3,15 AH/250V, Type 19181 (Wickmann)
115 V~: T 3,15 AH/250V, Type 19181 (Wickmann)
Radio noise suppression as per EN 55011 Class A
Noise immunity as per DIN EN 50082-1
Protection Type IP 20
Data interfaces 2 x RS-232 for accessories
1 x USB port for the connection of an external PC
1 x RS–232 for the connection of an external PC
PC requirements for software:
WinASPECT
Pentium processor 133 MHz, 16 MB RAM,
Windows 2000 or higher
Overview 3-2 General technical data of SPECORD®
SPECORD® 200/205/210/250 User's Manual – Edition 04/2005 Page 11
Analytik Jena AG

SPECORD®Device description and operating principle
Mechanical design of SPECORD
4 Device description and operating principle
4.1 Mechanical design of SPECORD
1
2
3
4
5
6
7
8
9
1 Premonochromator on SPECORD®250 or
toric illuminating mirror on SPECORD®200/205/210
2 Light sources
3 Cover of spectrometer system and photometer section
4 Device control
5 Power supply module
6 Detector board
7 Holder for turbid samples
8 Mount for standard cell holder
9 Sample compartment
Fig. 4-1 Mechanical design of SPECORD®
The major subassemblies of the SPECORD®are:
Light sources Halogen lamp and deuterium lamp generate the light that is
monochromatized in the spectrometer system. Then, it passes
through the sample.
Premonochromator
(only on SPECORD®250)
The premonochromator is a holographic grating that rotates
synchronously with the monochromator grating. The thus
obtained predispersion of light reduces stray light.
Spectrometer system The spectrometer system is protected against extraneous light
and dust by cover. The desiccator regulates the humidity
inside the system.
SPECORD® 200/205/210/250 User's Manual – Edition 04/2005 Page 13
Analytik Jena AG

Device description and operating principle SPECORD®
Design of subassemblies
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 .
Sample compartment The sample compartment contains two pairs of carrier rods for
the accommodation of various accessory units. To the support
plate, two holders for the accommodation of cells (9) and the
detector board are mounted.
Detector board Two photodiodes are used as radiation detectors, which are
Peltier temperature-controlled on SPECORD®200/210/250.
Power supply
module
The power supply modules supply the electrical voltage to the
electronic system and the fans for the thermoelectric
temperature control of the detectors on SPECORD®200/210.
Device control
computer
The device control computer coordinates the interaction of the
subassemblies involved in the measurement processes.
4.2 Design of subassemblies
4.2.1 Light sources
SPECORD®200 / 205 / 210
1 Halogen lamp in protective
housing
2 D2E lamp compartment
3 Reflecting mirror
4 Toric illuminating mirror
5 Setscrew for mirror
adjustment
Fig. 4-2 Lamp compartment of SPECORD®200/205/210
Page 14 SPECORD®200/205/210/250 User's Manual – Edition 04/2005
Analytik Jena AG

SPECORD®Device description and operating principle
Design of subassemblies
SPECORD®250
1
2
3
4
1 Halogen lamp in protective housing
2 D2E lamp compartment
3 Reflecting mirror
4 Premonochromator with holographic
grating
Fig. 4-3 Lamp compartment of SPECORD®250
The light sources used are a deuterium lamp (Fig. 4-2, 2) for the UV region and a
halogen lamp (Fig. 4-2, 1) for the VIS region of the spectrum.
Depending on the position of reflecting mirror (Fig. 4-2, 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.
On the SPECORD® 200/205/210, the toric mirror (Fig. 4-2, 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 (Fig. 4-2, 5).
On the SPECORD® 250, the holographic grating of the premonochromator takes the
place of the toric illuminating mirror (Fig. 4-4, 4).
SPECORD® 200/205/210/250 User's Manual – Edition 04/2005 Page 15
Analytik Jena AG

Device description and operating principle SPECORD®
Design of subassemblies
4.2.2 Spectrometer system and photometer section
Sample compartment
Concave grating
Filter wheel
Plane mirror
Beam splitter
Quartz-coated
toric mirrors
Entrance
slit
Exit
slit
DElamp
2
Halogen lamp
Swivel mirror
Detector
Detector
Cavity for
Cavity for
turbid samples
turbid samples
Cell
Cell
Toric illuminating mirror on SPECORD 200/205/210
or premonochromator grating on SPECORD 250
Fig. 4-4 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 Used to suppress unwanted radiation in the monochromator.
Holmium filter Standard for the automatic recalibration of wavelengths.
2 blank positions For the passage of non-dispersed light.
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 1, 2, 4 nm
SPECORD®205 1.4 nm
SPECORD®210 / 250 0.5, 1, 2, 4 nm.
The imaging grating disperses the incident light and spreads it out into a spectrum.
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.
Page 16 SPECORD®200/205/210/250 User's Manual – Edition 04/2005
Analytik Jena AG

SPECORD®Device description and operating principle
Design of subassemblies
4.2.3 Sample compartment
1Sample beam path with two carrier
rods
2Reference beam path with two
carrier rods
3Connector for sipper and cell
changer
4Connector (reserve)
5Stopper for conduit of optical fiber of
measuring probe or electrical cables
of accessories
6Conduit for coolant hoses
7Receptacle for cells with turbid
samples (reference)
8Mount for cell holder (reference)
9Receptacle for cells with turbid
samples
10 Mount for cell holder
11 Conduit for drain hose (not visible)
12 Conduits for sample-aspirating
hoses (sipper)
Fig. 4-5 Sample compartment
Sample (1) and reference beam (2) enter the sample compartment through the left-hand
wall.
The mounts for the cell holders (8), (10) 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 (7), (9) 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 cell changer or the sipper system.
The optical fibers of the measuring probe or the cables of the Peltier temperature-
controlled 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 (12) are provided for the aspiration tubes of
the super sipper system.
The illustration below shows the geometrical dimensions of the sample compartment.
SPECORD® 200/205/210/250 User's Manual – Edition 04/2005 Page 17
Analytik Jena AG

Device description and operating principle SPECORD®
Design of subassemblies
400
193
94
70
70
70
96
Fig. 4-6 Dimensions of sample compartment
Page 18 SPECORD®200/205/210/250 User's Manual – Edition 04/2005
Analytik Jena AG