N-500 NIRFlex®
Operation Manual
093020G en
Imprint
Product Identification:
Operation Manual (Original), N-500 NIRFlex®
093020G en
Publication date: 05.2016
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH-9230 Flawil 1
E-Mail: quality@buchi.com
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experience; especially in respect to structure, illustrations and technical detail.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of this manual without
prior written agreement is also prohibited.
Table of contents
3
NIRFlex N-500 Operation Manual, Version G
Table of contents
1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6
1.1 Trademarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
1.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2 Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7
2.1 User qualification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.2 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.3 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.4 Safety warnings and safety signs used in this manual . . . . . . . . . . . . . . . . . . 8
2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.5.1 General hazards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.5.2 Warning labels on housing and assemblies . . . . . . . . . . . . . . . . . . . . . . 11
2.5.3 Personal protective equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
2.5.4 Built-in safety elements and measures . . . . . . . . . . . . . . . . . . . . . . . . 12
2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.1 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.2 Technical data basic instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.2.1 Basic instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.2.2 Computer requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.3 Non-fiber optic measuring cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.3.1 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.3.2 NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.3.3 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.4 Fiber-optic measuring cells and accessories. . . . . . . . . . . . . . . . . . . . . . 16
3.4.1 NIRFlex Fiber Optic Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.4.2 NIRFlex Fiber Optic Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.4.3 NIRFlex Fiber Optic SMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
4.1 Functional principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
4.2 Measuring cells and their modes . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
4.2.1 Transflectance mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
4.2.2 Diffuse reflection mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
4.2.3 Transmission mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
4.2.4 Diffuse transmission mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
4.3 Basic instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
4.3.1 Lamp unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
4.3.2 Laser unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.3.3 Standard wheel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.4 NIRWare software suite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.4.1 Available NIRWare packages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
4.5 About the software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
4.5.1 NIRWare Control System Service . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
4.5.2 NIRWare software suite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
4.5.3 NIRCal chemometric software. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.6 Measuring cells with their add-ons and accessories . . . . . . . . . . . . . . . . . . 28
4.6.1 Operating panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.6.2 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
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4.6.3 Petri dish add-on for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . . . . . . . 30
4.6.4 Vial add-on for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
4.6.5 Tablet add-on for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
4.6.6 XL add-on for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
4.6.7 XL add-on with iris aperture for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . 32
4.6.8 XL add-on for B+L sample cups for NIRFlex Solids . . . . . . . . . . . . . . . . . . 33
4.6.9 External Reference for XL and petri dish add-on. . . . . . . . . . . . . . . . . . . . 33
4.6.10 Spinner add-on . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
4.6.11 Flow-cell adapter add-on . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
4.6.12 NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4.6.13 Sample plates for the NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . 36
4.6.14 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
4.6.15 NIRFlex Fiber Optic Solids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
4.6.16 Transflectance adapter for NIRFlex Fiber Optic Solids . . . . . . . . . . . . . . . . . 41
4.6.17 NIRFlex Fiber Optic Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
4.6.18 NIRFlex Fiber Optic SMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
5.1 Transportation lock . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
5.2 Requirements concerning the installation site . . . . . . . . . . . . . . . . . . . . . 45
5.3 Electrical connection requirements . . . . . . . . . . . . . . . . . . . . . . . . . . 46
5.4 Installing the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
5.4.1 Setting up the Ethernet communication . . . . . . . . . . . . . . . . . . . . . . . . 47
5.4.2 Network integration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
5.5 Installing the measuring cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
5.6 Installing the cover of the NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . 50
5.7 Preparing the transflectance adapter . . . . . . . . . . . . . . . . . . . . . . . . . 51
5.7.1 Adjusting the pathlength of the transflectance adapter to the probe head . . . . . . . 51
5.7.2 Exchanging the spacer ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
5.7.3 Installing the transflectance adapter to perform measurements . . . . . . . . . . . . 53
5.8 Installing measurement equipment to the NIRFlex Fiber Optic SMA . . . . . . . . . . 54
5.9 Starting up the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.9.1 System Suitability Test. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.9.2 Temperature tests in detail. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.9.3 NIR linearity test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.9.4 Signal-to-noise ratio determination . . . . . . . . . . . . . . . . . . . . . . . . . . 56
5.9.5 Wavenumber stability test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
5.9.6 SST with NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . 56
5.10 Reference measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
6.1 General recommendations for measuring solids . . . . . . . . . . . . . . . . . . . . 58
6.2 General recommendations for measuring liquids . . . . . . . . . . . . . . . . . . . 59
6.3 Starting a measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
6.4 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
6.4.1 Reference measurement for the Petri dish add-on. . . . . . . . . . . . . . . . . . . 60
6.4.2 Reference measurement for the XL add-on . . . . . . . . . . . . . . . . . . . . . . 60
6.5 NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
6.6 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
6.7 NIRFlex Fiber Optics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
6.7.1 NIRFlex Fiber Optic Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
6.7.2 NIRFlex Fiber Optic Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
6.7.3 NIRFlex Fiber Optic SMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
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7 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
7.1 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
7.2 Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
7.2.1 Optical surfaces and probes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
7.2.2 Cleaning of the External Reference . . . . . . . . . . . . . . . . . . . . . . . . . . 66
7.2.3 Cleaning of the Transflectance adapter . . . . . . . . . . . . . . . . . . . . . . . . 67
7.3 Advanced testing with NIRWare Automatic Diagnose . . . . . . . . . . . . . . . . . 68
7.4 Lamp module replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
7.5 Laser unit replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
7.6 Filter pad replacement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
7.7 Main fuse replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
7.7.1 Measuring cell fuse replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
7.8 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78
7.9 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78
7.10 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
8 Storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
8.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
8.2 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
9 Spare parts and accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
9.1 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
9.1.1 Interferometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
9.1.2 Measuring cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83
9.1.3 Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84
9.1.4 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
9.1.5 Optional accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
9.2 NIRFlex spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
9.3 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90
9.4 NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
9.5 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
9.6 NIRFlex Fiber Optic Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
9.7 NIRFlex Fiber Optic Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
9.8 NIRFlex Fiber Optic SMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
9.9 Transflectance adapter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
10 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
10.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . . 93
1 About this manual
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NIRFlex N-500 Operation Manual, Version G
1 About this manual
This manual describes the NIRFlex N-500 including its standard software and provides all information
required for its safe operation and to maintain it in good working order.
It is addressed to laboratory personnel and operators in particular.
Read this manual carefully before installing and running your system and note the safety precautions
in section 2 in particular. Store the manual in the immediate vicinity of the instrument, so that it can be
consulted at any time.
No technical modifications may be made to the instrument without the prior written agreement of
Buchi. Unauthorized modifications may affect the system safety or result in accidents. Technical data
are subject to change without notice.
NOTE
The symbols pertaining to safety are explained in section 2.
This manual is copyright. Information from it may not be reproduced, distributed or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of
this manual without prior written agreement is also prohibited.
The English manual is the original language version and serves as basis for all translations into
other languages. If you need another language version of this manual, you can download available
versions at www.buchi.com.
1.1 Trademarks
The following product names and any registered and unregistered trademarks mentioned in this
manual are used for identification purposes only and remain the exclusive property of their respective
owners:
• NIRFlex® is a registered trademark of BÜCHI Labortechnik AG
• NIRCal® is a registered trademark of BÜCHI Labortechnik AG
• Kimwipes® is a registered trademark of Kimberly Clark
• Meliseptol® is a registered trademark of B. Braun
1.2 Abbreviations
EMEA: European Agency for the Evaluation of Medicinal Products
EP: European Pharmacopoeia
FDA: Food & Drug Administration
MTBF: Mean time between failures
NIR: Near infrared
PMMA: Polymethylmetacrylat
S/N: Signal to noise ratio
USP: United States Pharmacopeia
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NIRFlex N-500 Operation Manual, Version G
2 Safety
This section introduces the safety concept of the instrument and contains general rules of behavior
and warnings from direct and indirect hazards concerning the use of the product.
For the users safety, all safety instructions and safety messages in the individual sections shall
be strictly observed and followed. Therefore, the manual must always be available to all persons
performing any tasks described herein.
2.1 User qualification
The instrument may only be used by laboratory personnel and other persons who on account of
training and professional experience know the potential dangers that can develop when operating the
instrument.
Untrained personnel, or persons who are currently being trained, require careful supervision by a
qualified person. This Operation Manual serves as a basis for training.
2.2 Proper use
The NIRFlex N-500 has been designed and built as a rugged analysis instrument. It serves to determine the matter and concentration of substances in samples above its measuring tolerance limit (no
trace analysis). Thanks to its ruggedness, the instrument is suitable for use on most production floors
(at-line, near-line). For suitable environmental conditions see tables of technical data.
The NIRFlex N-500 system can be applied for the following tasks:
Qualitative analysis
• Differentiation of chemically different substances (e.g. raw material testing of incoming goods);
• Differentiation of chemically similar substances or substance grades.
Quantitative analysis
• Determination of quantifiable product properties such as concentrations or physical parameters
(viscosity, particle size).
2.3 Improper use
Any other use than the one stated above and any application that does not comply with the technical
data is considered to be improper use. Improper use can cause hazardous situations for the operator
and / or for the instrument and might cause consequential property damage.
The operator bears the sole risk for any damages or hazards caused by improper use!
In particular, the following uses shall not be permitted
• Installation and use in environments where explosion protection is required
• User repair and maintenance work other than described in this manual
• Reuse of sample material for production that has been in direct contact with non-food safe materials and surfaces
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2.4 Safety warnings and safety signs used in this manual
DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of
hazards and risks related to personal injury and property damage. All signal words, which are related
to personal injury are accompanied by the general safety sign.
For your safety it is important to read and fully understand the table below with the different signal
words and their definitions!
Sign Signal word Definition Risk level
DANGER
Indicates a hazardous situation which, if not avoided, will result in
death or serious injury.
★★★★
WARNING
Indicates a hazardous situation which, if not avoided, could result
in death or serious injury.
★★★☆
CAUTION
Indicates a hazardous situation which, if not avoided, may result
in minor or moderate injury.
★★☆☆
no
NOTICE
Indicates possible property damage, but no
practices related to personal injury.
★☆☆☆
(property damage only)
Supplementary safety information symbols may be placed in a rectangular panel on the left to the
signal word and the supplementary text (see example below).
Space for
supplementary
safety
information
symbols.
!
SIGNAL WORD
Supplementary text, describing the kind and level of hazard / risk seriousness.
• List of measures to avoid the herein described, hazard or hazardous situation.
• ...
• ...
Table of supplementary safety information symbols
The reference list below incorporates all safety information symbols used in this manual and their
meaning.
Symbol Meaning
General warning
Electrical hazard
LASER emission
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Symbol Meaning
Explosive gases, explosive environment
Hot item, hot surface
Device damage
Fragile components
Unplug device
Wear protective goggles
Wear protective gloves
Do not dispose as unsorted household waste!
Additional user information
Paragraphs starting with NOTE transport helpful information for working with the device / software or
its supplementaries. NOTEs are not related to any kind of hazard or damage (see following example).
NOTE
Useful tips for the easy operation of the instrument / software.
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2.5 Product safety
The NIRFlex N-500 has been designed and built in accordance with state-of-the-art technology, at the
time of development. Safety warnings in this manual (as described in section 2.4) serve to make the
user alert to and avoid hazardous situations emanating from residual dangers by giving appropriate
counter measures.
However, risks to users, property and the environment can arise when the instrument is damaged,
used carelessly or improperly.
Always follow laboratory safety rules. E.g. wear personal protective equipment such as protective eye
googles, protective clothing and gloves when working with the instrument.
2.5.1 General hazards
The following safety messages show hazards of general kind which may occur when handling the
instrument. The user shall observe all listed counter measures in order to achieve and maintain the
lowest possible level of hazard.
NOTE
The instrument contains a laser for wavenumber calibration. When closed the instrument is considered a Class 1 laser product (DIN Standard: GZS values DIN VDE 0837). When the housing is open,
the instrument is considered a Class 3R laser product.
Additional warning messages can be found whenever actions and situations described in this manual
are related to situational hazards.
!
DANGER
Death or serious injuries by use in explosive environments.
• Do not store or operate the instrument in explosive environments
• Remove all sources of flammable vapors
• Do not store chemicals in the vicinity of the device
• Only operate and maintain the device in environment with sufficient ventilation
!
WARNING
Serious eye damage by unfiltered LASER emission at open housing.
• Do not operate the instrument with open or damaged housing
!
Caution
Minor or moderate injuries by dangerous current.
• Do not spill any liquids over the Measurement Cell connector of the instrument
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NOTICE
Risk of instrument damage by mechanical shocks.
• Do not move the instrument when it is active
• Do not drop the instrument or its components
• Keep external vibrations away from the instrument
• Do not transport the instrument without transportation lock engaged
2.5.2 Warning labels on housing and assemblies
The following warning sticker(s) can be found on the housing or assemblies of the NIRFlex N-500:
Symbol Meaning Location
Hot item, hot surface Inside housing, next to lamp modules
LASER emission
Sticker at the rear side
Sticker inside housing, at the LASER module
Electrical hazard HV supply LASER
Device labels Meaning Location
FCC declaration Sticker at the rear side
See text. Sticker at the rear side
LASER emission class Sticker at the rear side
See text.
Sticker on top of the housing, near the Measurement Cell connector.
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Device labels Meaning Location
LASER emission Sticker inside housing, at the LASER module
2.5.3 Personal protective equipment
Safety precautions and personal protective equipment might be necessary to comply with industrial
safety standards in some working environments. However, for standard operation with the instrument,
no additional protective equipment is necessary.
2.5.4 Built-in safety elements and measures
The instrument is equipped with the following safety elements:
• One outer filter elements with covering frame
• Multiple magnet sensors to detect opening of any housing element
• Multiple overtemperature sensors to monitor thermal spots inside the instrument
• Transportation lock of interferrometer
2.6 General safety rules
Responsibility of the operator
The head of the laboratory is responsible for training his/her personnel.
The operator shall inform the manufacturer without delay of any safety-related incidents which might
occur during operation of the instrument or its accessories. Legal regulations, such as local, state and
federal laws applying to the instrument or its accessories must be strictly followed.
Duty of maintenance and care
The operator is responsible for the proper condition of instrument. This includes maintenance, service
and repair jobs that are performed on schedule as described in this manual. Any work, not explicitly
described in this manual must be performed by authorized and trained personnel (e.g. service technicians) only.
Spare parts to be used
Use only genuine consumables and spare parts for maintenance to assure good system performance,
reliability and safety. Any modifications of spare parts or assemblies are only allowed with the prior
written permission of the manufacturer.
Modifications
Modifications to the instrument are only permitted after prior consultation and with the written approval
of the manufacturer. Modifications and upgrades shall only be carried out by an authorized Buchi technical engineer. The manufacturer will decline any claim resulting from unauthorized modifications.
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3 Technical data
This section introduces the reader to the instrument specifications and the list of materials used.
3.1 Materials used
Materials used
Component Material designation
Base plate Aluminium / stainless steel
Wedges TeO
2
Polarizers Glass
Housing Polyurethane foam
Detector InGaAs
Magnets NdFeB
3.2 Technical data basic instrument
3.2.1 Basic instrument
Technical data basic instrument
Dimensions housing ( W x H x D) 350 x 250 x 450 mm
Electric power supply 100−230 VAC ± 10 %, 50/60 Hz, 350 W
Ambient conditions < 80 % relative humidity for T < 31 °C, linear decreasing
to 67 % at 35 °C, max. 2500 m, for indoor use only
Ambient temperature 5−35 °C ( 25 ± 5 °C recommended)
Pollution degree 2
Installation category II
Spectral range 800 - 2500 nm (default 1000 - 2500 nm)
12‘500 - 4‘000 cm-1 (default 10‘000 - 4‘000 cm-1)
(if not specified otherwise for measuring cell)
Resolution 8 cm-1 (with boxcar apodisation)
Type of interferometer Polarisation interferometer with TeO2 wedges
Wavenumber accuracy ± 0.2 cm
-1
(measured with HF gascell at an ambient
temperature of 25 °C ± 5 °C)
S/N 10000 (peak-to-peak noise of a linear corrected baseline
between 5600−6000 cm-1, measured with NIRFlex
Liquids, 2 x 64 scans, Blackman apodisation)
Number of scans/sec. 2−4
Analog digital converter 24 bit
Type of lamp/lifetime lamp (MTBF) Tungsten halogen lamp / 12000 h (2 x 6000 h)
Type of laser 12 VDC HeNe, wavelength at 632.992 nm
Ethernet connection 100 Mbit/s
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3.2.2 Computer requirements
The spectral data are collected in the NIRWare database on the PC. The following minimum configuration is needed for the PC running the NIRWare Software Suite (1.4):
Computer hardware and software requirements
Windows XP Professional (32-bit only), SP3 or higher
/ Windows 7 Professional / Ultimate (32-bit only)
Dual Core 2.4 GHz or faster
3 GB RAM or more (2 GB minimum)
10 GB of free harddisk space
CD– ROM drive
2 Network adapter (1 adapter minimum)
Display res.: 1280 x 1024 (1024 x 768 minimum)
Please consider a more powerful computer system if you are working with a bigger amount of data,
doing automated (cyclic) measurements or calculating your own calibrations.
3.3 Non-fiber optic measuring cells
3.3.1 NIRFlex Solids
Technical data NIRFlex Solids
Detector extended range InGaAs (temperature controlled)
Electric power supply 100 - 230 VAC ± 10%, 50/60 Hz, 20 W
Ambient conditions < 80 % relative humidity for T < 31 °C, linear decreasing to 67 % at
35 °C, max. 2500 m, for indoor use only
Ambient temperature 5−35 °C ( 25 ± 5 °C recommended)
Pollution degree 2
Installation category II
3.3.2 NIRFlex Solids Transmittance
Technical data NIRFlex Solids Transmittance
Detector InGaAs (temperature controlled)
Electric power supply 100 - 230 VAC ± 10%, 50/60 Hz, 20 W
Ambient conditions < 80 % relative humidity for T < 31 °C, linear decreasing
to 67 % at 35 °C, max. 2500 m, for indoor use only
Ambient temperature 5−35 °C ( 25 ± 5 °C recommended)
Pollution degree 2
Installation category II
Spectral range 12’500 - 6’000 cm-1
(recommended range 11’520 - 6000 cm-1)
800−1660 nm (recommended range 870 - 1660 nm)
Photometric dynamic range 0 - 6 AU
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Technical data NIRFlex Solids Transmittance (cont.)
Photometric linearity The “addition of filter technique” has been used.
A 2% transmission filter and a wavelength standard
(Rare Earth Oxide mixture) were used for the addition.
Both filters were measured individually and together in
series. The addition of the individual measurements has
been compared with the measurement of both filters ihn
series. The difference had been < 2 x 10-7 T
at 7’876 cm
-1
Typical signal-to-noise ratio
open beam
5 mm white standard
rms for spectral segments of 300 cm-1 in the range of
11’000 - 6’500 cm
-1
mean 2 x 10-5 AU (16 scans; Blackman apodization)
mean 10 x 10-5 AU (64 scans; Blackman apodization)
3.3.3 NIRFlex Liquids
Technical data NIRFlex Liquids
Detector extended range InGaAs (temperature controlled)
Electric power supply provided from NIRFlex N-500 100−230 VAC ± 10 %, 50/60 Hz, 250 W
Ambient conditions < 80 % relative humidity for T < 31 °C, linear
decreasing to 67 % at 35 °C, max. 2500 m, for indoor
use only
Ambient temperature 5−35 °C ( 25 ± 5 °C recommended)
Pollution degree 2
Installation category II
Sample temperature range Ambient temperature plus 10 °C up to 65 °C
Reproducibility of set sample temperature
± 0.5 °C
Temperature overshoot < 5 °C
Overheating protection, automatic switch-off T > 90 °C
Diameter of measurement spot 2 mm
Type of cuvettes to be used Standard cuvettes 12.5 x 12.5 x 45 mm with path-
length of 2 mm, when spacers are used, 1, 5, 10 mm
cuvettes can be inserted as well
Time needed to reach a stable control of the set temperature Ambient temperature to 65 °C: 15 min
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3.4 Fiber-optic measuring cells and accessories
3.4.1 NIRFlex Fiber Optic Solids
Technical data NIRFlex Fiber Optic Solids
Detector extended range InGaAs (temperature controlled)
Electric power supply 100−230 VAC ± 10 %, 50/60 Hz, 20 W
Ambient conditions < 80 % relative humidity for T < 31 °C, linear decreasing
to 67 % at 35 °C, max. 2500 m, for indoor use only
Ambient temperature 5−35 °C ( 25 ± 5 °C recommended)
Pollution degree 2
Installation category II
Temperature range at probe tip 0 °C−80 °C
Standard length of fiber optic probe 2 m (available up to 5 m)
Accessories
Technical data Transflectance adapter (Fiber Optic Solids)
Max. operating temperature 120 °C
Material Transflectance sleeve material: Steel no. 1.4435
Spacer ring material: Steel no. 1.4305
Transflectance adapter window: Quartz glass
(Infrasil 303) sealed with fluorine rubber O-rings
Available pathlengths 0.5 mm, 1 mm, 1.5 mm
3.4.2 NIRFlex Fiber Optic Liquids
Technical data NIRFlex Fiber Optic Liquids
Detector extended range InGaAs (temperature controlled)
Electric power supply 100−230 VAC ± 10 %, 50/60 Hz, 20 W
Ambient conditions < 80 % relative humidity for T < 31 °C, linear decreasing
to 67 % at 35 °C, max. 2500 m, for indoor use only
Ambient temperature 5−35 °C ( 25 ± 5 °C recommended)
Pollution degree 2
Installation category II
Temperature range of the probe head at the probe tip 0 °C−150 °C
Max. pressure at the probe tip 6 bar
Standard length of fiber optic probe 2 m (available up to 7 m)
Pathlength 2 mm
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3.4.3 NIRFlex Fiber Optic SMA
Technical data NIRFlex Fiber Optic SMA
Detector extended range InGaAs (temperature controlled)
Electric power supply 100−230 VAC ± 10 %, 50/60 Hz, 20 W
Ambient conditions < 80 % relative humidity for T < 31 °C, linear decreasing
to 67 % at 35 °C, max. 2500 m, for indoor use only
Ambient temperature 5−35 °C ( 25 ± 5 °C recommended)
Pollution degree 2
Installation category II
NOTE
Limit ranges of environmental conditions at the point of measurement highly depend on individual
accessories (i.e. process probe, flow cell, etc.).
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4 Description of function
This section explains the basic principle of the instrument, shows how it is structured and gives a
functional description of the assemblies.
4.1 Functional principle
The NIRFlex N-500 is a modular optical instrument (basic instrument and measuring cell) to determine
the matter and concentration of substances in samples.
In detail, the NIRFlex N-500 is a Fourier Transformation Near Infrared spectrometer (FT-NIR). It generates an invisible near infrared interferogram beam which interacts with the molecules of a sample,
generating a characteristic feedback. The feedback is picked up via a measurement cell by a detector
and mathematically processed via Fourier transformation into a spectrum. This spectrum is used to
extract the requested material information.
Inside the spectrometer, a laser beam is used as a high-precision wavelength reference to allow best
possible reproducibility and accuracy of detection.
Advantages of FT-NIR polarization inteferometer
• Simultaneous measurement of all wavenumbers giving an improved signal-to-noise ratio
• Higher intensity giving an improved signal-to-noise ratio and short measuring times
• Laser as wavenumber reference giving high wavenumber stability and good data
transferability
• Single-beam interferometer without typical double-beam divergence for mechanically and temperature stable beam alignment
• More robust design than standard Michelson interferometer
How the interferogram is generated
An interferogram is an interference pattern of phase-shifted beams. The NIRFlex N-500 is a single-
beam polarisation interferometer, generating its interferogram in four steps:
Step 1— Polarization of the light source output
The polarizer B generates a well-defined polarization output of the undefined polarized light, emitted
by the light source A. Thus, only diagonally polarized light is transmitted.
Step 2 — Beam splitting and orthogonal polarization
The polarized light enters a double refracting block (comparator) C. Here, the light is broken down
into two, orthogonally polarized components with a small, static phase shift.
Step 3 — Generating the ongoing phase shift
An assembly of two double refracting wedges is arranged after the comparator. Wedge D is
stationary, while wedge E is constantly shifted back and forwards by a fast linear-drive. The movement and the geometric arrangement provides a change of thickness in the light path. This leads to an
ongoing phase shift between the light beams.
Step 4 — Beam recombination and interferogram output
A second polarizer F converts the phase shifted beams into a single light output with intensity variation – the interferogram.
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Reference laser control
The laser deliveres a constant, wavelength-stable beam of 633 nm. The laser beam a is coupled into
the NIR beam b to pass the interferometer before being decoupled d and analysed by the “Laser
feedback sensor” e. A fraction of the beam is splitted at the polarizer b and picked up by an intensity sensor c to monitor the laser beam quality. The position and movement-frequency of the wedge
by the linear drive f causes an alternating relative phase shift of the laser light. Being reflected by the
second polarizer d, the phase shift generates an alternating amplitude. This alternating amplitude is
detected via the the “Laser sensor” e, giving precise information about velocity and (relative) position
of the wedge. The feedback signal is used to control the velocity of the linear drive f as well as to set
the sampling-points of the NIR interferogram.
A
B
+ dC
DE
H G
e
a
f
LASER – 633 nm
F + b
c
Spare lamp
Effective NIR light path
A
NIR light source assembly with spare lamp and motorized parabolic reflector
B
First polarizer
C
Comparator (double refracting block)
D
Stationary double refracting wedge
E
Moving double refracting wedge
F
Second polarizer
G
Sample
H
Interferogram detector
Reference laser signal path
a
Laser output window
b
Second polarizator (works as a beam splitter for the laser)
c
Laser output-power sensor
d
First polarizer
e
Laser feedback detector
f
Linear motor for wedge movement
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Data processing and interferogram analysis
The NIR light interacts with the sample G material in different ways, leaving a characteristical finger-
print on the interferogram. At liquids the light is mostly transmitted and at solids reflected. The
remaining light is collected by the detector H. The built-in computer further processes the raw signal.
Process steps Result
Signal preprocessing Interferogram
Fourier transformation Raw spectrum
Signal background correction Spectrum of sample
Chemometric analysis of the spectral data Sample analysis
Display of the result via NIRWare Operator on the attached monitor Sample analysis is displayed
4.2 Measuring cells and their modes
The NIRFlex N-500 system is of modular design. The interferometer is located in the basic instrument.
Different measuring cell modules for different kinds of sample materials can be easily attached to the
basic intrument. To choose the best measuring cell for a specific range of samples the optical properties of the sample material must be know.
Measuring cell matrix
Sample characteristics
(for NIR light)
Section Measuring cell Typical application
Diffuse reflection 4.2.1 NIRFlex Solids;
NIRFlex Fiber Optic Solids;
NIRFlex Fiber Optic SMA*
Predominantly non-translucent
materials such as most tablets,
cereals and powders
Transmission 4.2.3 NIRFlex Liquids;
NIRFlex Fiber Optic Liquids
NIRFlex Fiber Optic SMA*
Translucent and transparent liquids
Diffuse transmission 4.2.4 NIRFlex Solids Transmittance Predominantly translucent solids
such as some tables, crystal
powders and other light conducting
materials
Transflectance 4.2.5 NIRFlex Fiber Optic Solids / NIRFlex
Solids with Transflectance Adapter;
NIRFlex Fiber Optic SMA*
Solids with weak diffuse reflection
and low transmission rate characteristics
*Depending on the custom accessory
and measurement setup
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4.2.1 Transflectance mode
Translucent and opaque liquids can be analyzed via transflectance mode. The light penetrates the
liquid, is diffusely reflected by the reference plate and passes the sample a second time. The transflected rays contain the spectral information of the sample.
Factors that can influence the measurement:
• Not enough sample material available
• Air bubbles in the measurement path and under the transflectance cover
• Sample not homogeneous or representative
• Temperature of sample material
• Sample cup or transflectance cover inadequate (e.g. cup material and thickness, blind spots, dirt
etc.)
NIRFlex Solids:
Diffuse reflecting / reference plate
Small, defined gap for liquid samples
Detector
NIR light
Sample cup / petri dish
NIRFlex Fiber Optic Solids / SMA:
Diffuse reflecting / reference plate
Small gap for liquid samples
Fiber optics (example)
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NOTE
• With special accessories, reflection-mode probes can be equipped for transflectance.
• The samples should either be measured at a constant temperature or the temperature influences
must be considered during calibration.
• Recommended number of scans: Qualitative calibration: 4−16; quantitative calibration: 16−32
• Most liquid sample materials can be constantly analyzed with the help of a flow-cell adapter.
4.2.2 Diffuse reflection mode
Most non-translucent materials (e.g. solids such as powders, pellets and cereals) can be analyzed
via diffuse reflection. The NIR light penetration is limited by the sample material. It interacts with the
sample, is refracted and diffusely reflected into the sensor. The reflected rays contain the spectral
information of the sample.
Detector
NIR light
Sample material
Factors that can influence the measurement:
• Not enough sample material available
• Sample not homogenious or representative
• Humidity of sample material
• Temperature of sample material
• Sample cup inadeqate (e.g. cup material and thickness, blind spots, dirt etc.)
NOTE
• The samples should either be measured at a constant temperature or the temperature influences
must be considered during calibration.
• Coarse grained samples should be milled before carrying out the measurement. Recommended
number of scans: Qualitative calibration: 4−16; quantitative calibration: 16−32;
granules: 64.
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4.2.3 Transmission mode
NIR light is sent through a defined pathlength of sample material (e.g. in a cuvette). The transmitted
light contains the spectral information. This is the preferred method for testing liquids.
Detector
Cuvette
NIR light
pathlength
4.2.4 Diffuse transmission mode
The diffuse transmission mode is a mixture of “diffuse reflection” and “transmission” mode.
The NIR light penetrates the sample:
• is refracted
• diffusely reflected
• diffusely transmitted
The transmitted rays contain the spectral information of the sample.
Detector
NIR light
Sample
Collecting lens
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4.3 Basic instrument
The basic instrument consists of the spectrometer unit with the interferometer, the lamp unit with two
lamp modules, the laser unit and electronic boards. The Instrument Software (embedded software)
controls the spectrometer and communicates with the PC running NIRWare and with the measuring
cell. It controls all actors (stepper motor, heating, etc.) and sensors (light barrier, temperature sensor,
etc.) in the measuring cell. The sensor is part of the measuring cell.
4
a
b
c
e
f
g
a Main switch
b Primary fuses
c Power supply socket
d Type plate with serial number
e Ethernet connection
f Interfaces for service intervals (USB 1, USB 2, KBD, MS,
VGA, COM)
g Ventilation filter
4.3.1 Lamp unit
The lamp unit comprises two lamp modules:
• A primary lamp module, which is normally in use.
• A secondary lamp module, which is only in use during failure of the primary lamp module.
When the NIRWare software detects a lamp failure, it automatically switches to the secondary lamp
module. Until the primary lamp module has been exchanged the spectrometer measures spectra with
the secondary lamp module.
The operator will be reminded to exchange the primary lamp module, which he can easily do by
himself, see section 7.4. The secondary lamp module can only be exchanged by service personnel.
The hours of operation are logged separately for each lamp module. The lifetime of the lamps is about
6000 h each.
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4.3.2 Laser unit
The laser unit comprises:
• Laser tube
• High voltage power supply
The intensity of the laser light is continuously checked. When it falls below a certain threshold, the
operator has to change the laser, see section 7.5. The hours of operation are logged.
The typical lifetime of a laser is about 20000 h.
4.3.3 Standard wheel
Standard wheel
Every NIRFlex N-500 is equipped with a standard wheel with standards that are used for the System
Suitability Test (SST).
The standards within the wheel have the following functions:
• Wavelength standard (PMMA) to check the wavelength accuracy.
• Open beam for normal measurements.
• Five different grey standards to check the linearity.
The software is designed for the automatic use of the standard wheel, i.e. the operator does not have
to start one of the above mentioned tests manually, to ensure proper measurement of the SST and
NADIA.
4.4 NIRWare software suite
NIRWare is the interface program suite between the instrument and the operator. All program parts are
hosted on an external PC. The PC communicates with the spectrometer via internal network adapter.
NOTE
• A second network interface at the PC is recommended to connect the NIRFlex N-500 to a local
PC network, e.g. for data backup or to communicate with enterprise resource planning etc.
• It is recommended to turn off all power saving options. For Windows XP: In the Control Panel
of the operating system open the dialog Power Options Properties and select Power schemes
Always On.
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About the external PC
The external PC must run Windows® XP or Windows® 7 as operating system and meet the system
requirements (see technical data, section 3.2.1). The NIRWare software suite must be installed
successfully on the computer. The database might be installed on a network drive, to be accessible by
different spectrometer.
4.4.1 Available NIRWare packages
Two predefined NIRWare packages are available for the NIRFlex N-500:
Available NIRWare packages
Basic Advanced
NIRWare Operator x x
NIRWare Management Console
Application Designer x x
Sample Manager x x
Administrative Tools x x
Security Designer x x
Library Designer x
Regulatory Kit x
Each package includes the following program elements by default:
• Operator interface, to run routine analysis
• Administrative tools
• Report templates
• Comprehensive database with analysis data and other
The NIRWare Basic package offers the minimum requirements to use the NIRFlex N-500 FT-NIR
system. This package is recommended for routine analyses with pre-calibrated applications or as
satellite systems in a large application network.
The NIRWare Advanced package offers all components to comply with pharmaceutical requirements based on a lifecycle concept. It is recommended to complete this package with the NIRCal
Chemometric Software, which enables the development of own calibrations. Together with the Library
Designer a bunch of possibilities for identity control is available.
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4.5 About the software
The NIRWare software meets industrial standards in terms of inner structure combined with a comprehensive and intuitive, wizard guided user interface. It is also ideally suited for many applications in the
pharmaceutical, food and feed industry.
Advanced software and system management is done with the NIRWare Management Console tool.
The NIRWare Management Console combines various software modules:
• NIRWare Application Designer to define NIRWare Operator applications
• NIRWare Sample Manager to administrate all samples and reference values
• NIRWare Administrative Tools for applications and calibrations interchange and other administra-
tive tasks
• NIRWare Security Designer to define users and user groups according to custom security policies
Optional:
• NIRWare LIMS to import and export sample information and measurement data
• NIRWare Library Designer is a powerful software module for substance identity control using full
spectral comparison. It is designed for the development of spectral libraries tailored to individual
user requirements.
• NIRWare Regulatory Kit provides all components to comply with pharmaceutical regulations.
4.5.1 NIRWare Control System Service
The NIRWare Control System Service controls the complete system. It runs in the background as a
service. Normally there is no user interaction necessary.
4.5.2 NIRWare software suite
The PC is running the NIRWare Software Suite. NIRWare is the interface between the instrument and
the operator. All software tools are included, like Administrative Tools, report templates, elements to
create new applications and to run routine analyses, and the database to save all results and data.
The outstanding features of NIRWare are its logical structure, an industry-standard design and at the
same time an easy to understand user interface.
The NIRWare Software Suite comprises the following modules:
• NIRWare Management Console combines various software modules:
– NIRWare Application Designer defines the applications performed using NIRWare Operator
– NIRWare Sampe Manager administers all samples and reference values
– NIRWare Administrative Tools imports and exports applications and calibrations and is used for
other administrative work
– NIRWare Security Designer is used for the administration of users and user groups and for the
definition of security policies
• Optional modules for the NIRWare Management Console:
– NIRWare Library Designer is a powerful software module for identity control using full spectral
comparison. It is designed for the development of spectral libraries tailored to individual user
requirements.
– NIRWare Regulatory Kit provides all components to comply with pharmaceutical regulations.
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4.5.3 NIRCal chemometric software
NIRCal is a modern chemometric software package for use with Buchi FT-NIR Spectrometers. It can
be used for qualitative and quantitative applications. For method development a lot of comprehensive
pretreatments are available. However, the software is easy to use even for novices. The Calibration
Wizard guarantees the development of reproducible calibrations. Complex calibrations and interpretations are greatly simplified by the use of wizards, which automate standard procedures and help to
develop calibrations.
4.6 Measuring cells with their add-ons and accessories
The modulated light coming from the interferometer interacts with the sample. The light is then
detected in the measuring cell and the data is sent to the basic instrument.
The measuring cell has its own power supply and is galvanically isolated from the basic instrument. It
can be swapped without switching off the basic instrument and is automatically identified (plug & play).
4.6.1 Operating panel
Each measuring cell is equipped with an operating panel:
a
b
c
a LED
b START button
c STOP button
Operating panel of a measuring cell
The START button is used to start a measurement without using a PC keyboard.
The STOP button is used to stop a measurement without using a PC keyboard.
An LED informs the user about the current instrument state:
Red: Instrument is in error state
Green: Instrument is ready to use
Green flashing: Instrument is busy measuring
Yellow: Power is on but the instrument is not yet initialized by the NIRWare software
For a description of the LEDs at the handle of the fiber optic, see sections 4.6.15 and 4.6.17.
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4.6.2 NIRFlex Solids
List of NIRFlex Solids add-ons
Spinner / Petri dish
add-on
Vial add-on Tablet add-on XL add-on Flow cell
Max. number of samples per
sequence
1 6 10 1 1
Measurement based on
diffuse reflection
x x x x -
Measurement based on
transflectance
x - - - x
Measurement with petri
dishes
x - - - -
Measurement with vials - x - - -
Measurement of tablets - - x - -
Measurement using small
plastic bags
- - - x -
Internal reference x - - x x
External Reference x x x x x
Sample dimensions Spinner 34 mm
Petri dish 100 mm
Glass vials
10−15 mm
Tablets
5−10 mm
>0.3 ml
The NIRFlex Solids is the ideal configuration to measure solid samples like powders, pastes and
pellets in diffuse reflection mode. The measuring cell for solids allows the use of different add-ons for
specific sample containers.
The software automatically detects the type of add-on in use as soon as the corresponding application is started in the NIRWare Operator.
For a description of the add-ons to be used with the NIRFlex Solids, see section 4.6.3 to 4.6.8.
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