Analytik Jena SPECORD S600 User manual

SPECORD®S600
Simultaneous
Spectrophotometer

Analytik Jena AG
Kundendienst
Konrad-Zuse-Str. 1
07745 Jena
Phone: Hotline: + 49 (3641) 77-7407
Fax: + 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 2000, Windows XP, Windows NT, MS Excel are registered trademarks of Microsoft
Corp.
Publication No.: 211:502.23
Edition – February 2008
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 2008 Analytik Jena AG

Contents
Contents
1Introduction .....................................................................3
1.1 Intended use of the SPECORD S600 ...................................................3
1.2 Notes on the User's Manual..................................................................3
2Safety notes .....................................................................5
2.1 Warning labels on SPECORD S600 .....................................................5
2.2 General safety regulations ....................................................................5
3Technical Data of SPECORD S600.................................9
3.1 Physical-optical data .............................................................................9
3.2 General technical data ........................................................................10
4Device description and operating principle ................11
4.1 Mechanical design ..............................................................................11
4.2 Operating principle ..............................................................................12
5Transport and installation requirements.....................15
5.1 Conditions for storage and transport...................................................15
5.2 Installation conditions..........................................................................15
6Installation and start-up................................................17
6.1 Connectors and display elements.......................................................17
6.2 Connecting the SPECORD S600........................................................18
6.3 Start-up................................................................................................18
6.4 Switching off the SPECORD S600 .....................................................20
7Accessories ...................................................................21
7.1 Standard cell holders ..........................................................................21
7.1.1 Universal holder .............................................................................................21
7.1.2 Cell holder ......................................................................................................22
7.2 Further accessories.............................................................................23
8Care, maintenance, lamp change.................................25
8.1 Care and maintenance........................................................................25
8.2 Cleaning ..............................................................................................25
8.3 Changing lamps ..................................................................................26
8.3.1 Part numbers of lamps ...................................................................................26
8.3.2 Note on the service life of lamps ....................................................................26
8.3.3 Opening the flap of the lamp compartment ....................................................26
8.3.4 Changing the deuterium lamp ........................................................................27
8.3.5 Changing the halogen lamp ...........................................................................28
8.4 Changing fuses ...................................................................................29
9Disposal .........................................................................31
10 List of illustrations ........................................................33
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Contents
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Introduction
Intended use of the SPECORD S600
1 Introduction
1.1 Intended use of the SPECORD S600
The SPECORD®is a powerful, computer-controlled high-performance diode array
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 – 1020 nm.
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.
1.2 Notes on the User's Manual
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.
Danger! Hot surface!
Touching the hot surface may cause burns.
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 S600 p.3)
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Introduction
Notes on the User's Manual
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Safety notes
Warning labels on SPECORD S600
2 Safety notes
2.1 Warning labels on SPECORD S600
Observe the warning labels on the SPECORD®S600!
The following warning labels have been affixed to the lamp housings of the
SPECORD®S600.
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.
Extremely dangerous electrical voltage!
Several parts inside the lamp housing carry electrical voltage. Therefore, before
opening the lamp housing, switch off the SPECORD®S600 at the power switch and
disconnect the power cable from the power outlet!
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.
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.
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Safety notes
General safety regulations
Emergency shutdown!
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!
On the SPECORD®S600, a deuterium lamp delivers the radiation for the UV
measuring range. While measurements are running, UV radiation transmits the
sample compartment in the sample beam. In measurement breaks, no UV radiation is
accessible there, as the sample beam is closed by a shutter. Besides, UV radiation
appears in the lamp compartment. Before any lamp replacement, switch off the
SPECORD®S600 and disconnect the power cable!
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!
Longer exposure of the skin to UV radiation may cause skin damage!
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®S600!
Before you switch on the SPECORD®S600, remove its dust cover!
Handling liquids
Take care to ensure that no liquids can enter the SPECORD®to avoid any damage to
the device.
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Safety notes
General safety regulations
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.
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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Safety notes
General safety regulations
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Technical Data of SPECORD S600
Physical-optical data
3 Technical Data of SPECORD S600
3.1 Physical-optical data
Technical Data SPECORD®S 600
Optical principle High-performance diode array for UV NIR range
Optics Polychromator with concave holographic grating
and photodiode array (1024 pixels)
Wavelength range 190-1100 nm ±2 nm
Photometric measuring range -3 to 3 A
Photometric display range -4 to 4 A
Wavelength accuracy
(with holmium oxide filter)*
±0.5 nm
Wavelength accuracy
(D2E-peaks at 486,0 nm and
656,1 nm)
±0.3 nm
Wavelength reproducibility
(with holmium oxide filter)*
±0.02 nm
Photometric accuracy
VIS at 546nm with Hellma F4
neutral-density filter
±0.005 A
Photometric accuracy
UV with potassium dichromate acc.
to Ph.Eur.
±0.012 A
Stray light 198 nm
( KCl Merck 1.08164.0001)
≤1.0 %T
Stray light 220 nm (NaI) ≤0.05 %T
Stray light 340 nm (NaNO2) ≤0.05 %T
Long-term stability at 500 nm ≤±0.002 A/h
UV resolution (Toluene hexane) ≥1.6
Minimum measuring time 12 ms for one spectrum
* allowing for tolerances of used standard
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Technical Data of SPECORD S600
General technical data
3.2 General technical data
Weight 11 kg
Footprint (W x D) approx. 900x750 mm2with PC
Dimensions (W x H x D) 680 x 190 x 250 mm3
Line voltage 230 VAC ±10 % or
115 VAC ±10 % (switchable by service)
Frequency 47 ... 63 Hz
Power consumption 140 VA
Fuses:
Line fuses
230 VAC: T 3.15 AH/250V, Type 19181 Wickmann
115 VAC: T 3.15 AH/250V, Type 19181 Wickmann
Radio noise suppression EN 61326 Class B
Noise immunity EN 61326
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 Windows XP
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Device description and operating principle
Mechanical design
4 Device description and operating principle
4.1 Mechanical design
The appearance of the SPECORD®S600 is marked by the lamp compartment on the
right side, the central sample compartment that is open to three sides, and the
polychromator section on the left side.
1 Lamp compartment
2 Sample compartment with carrier rails for holding accessories
3 Polychromator
Fig. 1 Mechanical design of SPECORD®S600
Unlike scanning spectrophotometers with monochromator, the optical design of the
SPECORD®S600 with its polychromator requires a few moving components only and is
mechanically very stable.
Fig. 2 Optical path of SPECORD®S600
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Device description and operating principle
Operating principle
Light sources The light sources used are a halogen lamp for the VIS and infrared
region and a deuterium lamp for the UV region.
The lamp-selector slider serves to couple the light of either the
halogen or the deuterium lamp, or the light of both lamps
simultaneously into the optical path.
In measurement breaks, lamp radiation is shut off by shutters. That
way, it is possible to perform dark-current measurements and
protect the sample from unnecessary radiation exposure.
Sample
compartment
The optical setup with polychromator allows an open sample
compartment. The bundle of rays is restricted by optical slits to the
lamp compartment and the polychromator side each. The
accessory units are clamped to the carrier rails of the sample
compartment.
Polychromator The polychromator used is the patented MCS module (Multi
Channel System) from Carl Zeiss. The entrance slit, the imaging
holographic grating and the detector are embedded in a ceramic
housing.
4.2 Operating principle
The undispersed light of the halogen and/or the deuterium lamp transmits the sample
and is partly absorbed by the sample. The thus altered light is spectrally dispersed in the
polychromator by the holographic grating. The produced spectrum is imaged onto the
diode array. The measured values of the individual photodiodes thus represent the value
of intensity Iover a small spectral region. As this is done in a very fast process, this type
of measurement is called simultaneous.
However, reading the individual photodiodes takes a certain time (integration time). This
integration time can be varied within predefined limits. The shortest integration time
possible depends, inter alia, on the number of photodiodes per line. A compromise has
to be made in selecting the most favorable integration time. A smaller integration time
means, that there is less time for the photodiode to capture the light to be measured. The
level of the measured signal will be lower and thus the signal-to-noise ratio deteriorate.
On the other hand, a too high integration time may result in an intensity that exceeds the
level the photodiode can receive (degree of saturation). The corresponding sections of
the diode array are overdriven and the found transmission or absorbance values are
wrong. However, a high integration time may be quite desirable if measurements shall be
taken in low-energy regions of the spectrum (e.g. 900 – 1020 nm) and the overdriven
areas are deliberately eliminated for the analysis. The system provides software-
supported automatic search of integration times suitable for the analytical measuring
range.
In absorption measurements, the incident intensity IR (reference value) and the intensity
ISattenuated by the sample is measured at every wavelength of interest. Measurement
is in arbitrary units, as only the ratio of both values is of importance. Quantitatively, the
absorption behavior is expressed in transmission T[%] or absorption A:
However, also the dark current must be considered for result generation. The dark
current is the intensity IDof the ambient light that may enter the polychromator through
the open sample compartment including the currents on the diode array caused by
electronics. The intensity of the dark current must be subtracted from the intensities of
sample and reference. The dark current can be measured automatically or – in very
time-critical measurements – started manually. The corresponding options are to be
selected along with other measurement parameters in WinASPECT®software.
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Device description and operating principle
Operating principle
Transmission and absorption are calculated according to the following formulas:
DR
DS
II
II
D−
−
=D Transmission
IRUnattenuated intensity (reference value)
ISIntensity after attenuation by the sample
ID Dark current
100DT[%] ∗= T[%] Percent transmission
DlgA −= A Absorption
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Device description and operating principle
Operating principle
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Transport and installation requirements
Conditions for storage and transport
5 Transport and installation requirements
5.1 Conditions for storage and transport
For transport and storage, the following ambient conditions must be complied with:
• Temperature range in transport: -40...+70 °C
• Relative humidity in transport: up to 95 %
5.2 Installation conditions
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)
Considering the dimensions of the SPECORD®S600 and a clearance of approximately
100 mm to the sides and the front, the device needs a bench space of 880 x 450 mm2.
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Transport and installation requirements
Installation conditions
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Installation and start-up
Connectors and display elements
6 Installation and start-up
6.1 Connectors and display elements
The connectors and display elements of the SPECORD®are arranged on its front and
back wall for easy access.
The LED indicators on the left front side of the SPECORD®serve to indicate line power
and lamp operation.
1 Halogen lamp ON LED (red)
2 D2E lamp ON LED (yellow)
3 Line power ON LED (green)
Fig. 3 Display elements on front panel
The LED's light when the SPECORD®has been switched on and the lamps are on.
The power-input connector with fuse holder, the power switch, and the connectors for PC
and accessories are arranged on the back panel of the device.
12345678
1 Connector for accessories 5 Type label
2 Connector for accessories 6 Power switch
3 RS232 port for PC 7 Fuse holder for line fuse
4 USB port for PC 8 Power input connector
Fig. 4 Connectors on back panel
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Installation and start-up
Connecting the SPECORD S600
6.2 Connecting the SPECORD S600
Observe correct position of device!
Move the SPECORD®only in upright position (observe label on transport case).
Do not turn the device upside down.
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.
Connecting SPECORD®and PC
1. Remove the device from its transport packaging and remove the plastic cover. Wait
until the device has adjusted to the ambient temperature.
2. Install the software on the PC (→Refer to WinASPECT®User's Manual).
3. Connect the SPECORD®S600 (→see Connectors and display elements p.17) to
the PC (free COM port or USB port) using the supplied connecting cable.
Note
When you use the APG 53 or APG 100 Autosampler, you must connect the PC to the
USB port and the autosampler to the serial port!
4. Connect one power cable each to the SPECORD®S600 and the PC. Connect the
power cables of the SPECORD®S600 and the PC to power outlets that are
connected to the same phase of the line power supply (multiple socket outlet, if
possible).
6.3 Start-up
Do not cover ventilation slots!
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 not be
covered by light objects placed on the tabletop (e.g. a loose sheet of paper.
Caution in handling liquids!
Do not place any objects, especially no containers with liquids, on the SPECORD®.
1. Start WinASPECT®software by a click on the program icon on the Windows
desktop or by clicking the Start button on the taskbar:
Start / Programs / WinASPECT / WinASPECT
Fig. 5 WinASPECT®program icon
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