BUCHI N-500 User Manual

Operation Manual
®
NIRFlex
N�500
093020
en
Table of contents
Table of contents
1.1 Trademarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.1 User qualification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
2.2 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
2.3 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
2.4 Safety warnings and safety signs used in this manual . . . . . . . . . . . . . . . . . . 9
2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.5.1 General hazards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.5.2 Warning labels on housing and assemblies . . . . . . . . . . . . . . . . . . . . . . 12
2.5.3 Personal protective equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.5.4 Built-in safety elements and measures . . . . . . . . . . . . . . . . . . . . . . . . 13
2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.1 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.2 Technical data basic instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.2.1 Basic instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.2.2 Computer requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.3 Non-fiber optic measuring cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.3.1 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.3.2 NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.3.3 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.4 Fiber-optic measuring cells and accessories. . . . . . . . . . . . . . . . . . . . . . 17
3.4.1 NIRFlex Fiber Optic Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.4.2 NIRFlex Fiber Optic Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.4.3 NIRFlex Fiber Optic SMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
4.1 Functional principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
4.2 Measuring cells and their modes . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
4.2.1 Transflectance mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
4.2.2 Diffuse reflection mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
4.2.3 Transmission mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
4.2.4 Diffuse transmission mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
4.3 Basic instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.3.1 Lamp unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.3.2 Laser unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
4.3.3 Standard wheel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
4.4 NIRWare software suite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
4.4.1 Available NIRWare packages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
4.5 About the software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.5.1 NIRWare Control System Service . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.5.2 NIRWare software suite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.5.3 NIRCal chemometric software. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.6 Measuring cells with their add-ons and accessories . . . . . . . . . . . . . . . . . . 29
4.6.1 Operating panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.6.2 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
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Table of contents
4.6.3 Petri dish add-on for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . . . . . . . 31
4.6.4 Vial add-on for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
4.6.5 Tablet add-on for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
4.6.6 XL add-on for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
4.6.7 XL add-on with iris aperture for NIRFlex Solids . . . . . . . . . . . . . . . . . . . . 34
4.6.8 XL add-on for B+L sample cups for NIRFlex Solids . . . . . . . . . . . . . . . . . . 34
4.6.9 External Reference for XL and petri dish add-on. . . . . . . . . . . . . . . . . . . . 35
4.6.10 Spinner add-on . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4.6.11 Flow-cell adapter add-on . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
4.6.12 NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
4.6.13 Sample plates for the NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . 38
4.6.14 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
4.6.15 NIRFlex Fiber Optic Solids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
4.6.16 Transflectance adapter for NIRFlex Fiber Optic Solids . . . . . . . . . . . . . . . . . 42
4.6.17 NIRFlex Fiber Optic Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
4.6.18 NIRFlex Fiber Optic SMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
5.1 Transportation lock . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
5.2 Requirements concerning the installation site . . . . . . . . . . . . . . . . . . . . . 46
5.3 Electrical connection requirements . . . . . . . . . . . . . . . . . . . . . . . . . . 47
5.4 Installing the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
5.4.1 Setting up the Ethernet communication . . . . . . . . . . . . . . . . . . . . . . . . 48
5.4.2 Network integration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
5.5 Installing the measuring cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
5.6 Installing the cover of the NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . 51
5.7 Preparing the transflectance adapter . . . . . . . . . . . . . . . . . . . . . . . . . 52
5.7.1 Adjusting the pathlength of the transflectance adapter to the probe head . . . . . . . 52
5.7.2 Exchanging the spacer ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
5.7.3 Installing the transflectance adapter to perform measurements . . . . . . . . . . . . 54
5.8 Installing measurement equipment to the NIRFlex Fiber Optic SMA . . . . . . . . . . 55
5.9 Starting up the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
5.9.1 System Suitability Test. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
5.9.2 Temperature tests in detail. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
5.9.3 NIR linearity test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
5.9.4 Signal-to-noise ratio determination . . . . . . . . . . . . . . . . . . . . . . . . . . 57
5.9.5 Wavenumber stability test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
5.9.6 SST with NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . 57
5.10 Reference measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
6.1 General recommendations for measuring solids . . . . . . . . . . . . . . . . . . . . 59
6.2 General recommendations for measuring liquids . . . . . . . . . . . . . . . . . . . 60
6.3 Starting a measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
6.4 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
6.4.1 Reference measurement for the Petri dish add-on. . . . . . . . . . . . . . . . . . . 61
6.4.2 Reference measurement for the XL add-on . . . . . . . . . . . . . . . . . . . . . . 61
6.5 NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
6.6 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
6.7 NIRFlex Fiber Optics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
6.7.1 NIRFlex Fiber Optic Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
6.7.2 NIRFlex Fiber Optic Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
6.7.3 NIRFlex Fiber Optic SMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
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NIRFlex N-500 Operation Manual, Version E
Table of contents
7.1 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
7.2 Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
7.2.1 Optical surfaces and probes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
7.2.2 Cleaning of the External Reference . . . . . . . . . . . . . . . . . . . . . . . . . . 67
7.2.3 Cleaning of the Transflectance adapter . . . . . . . . . . . . . . . . . . . . . . . . 68
7.3 Advanced testing with NIRWare Automatic Diagnose . . . . . . . . . . . . . . . . . 69
7.4 Lamp module replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
7.5 Laser unit replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
7.6 Filter pad replacement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
7.7 Main fuse replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78
7.7.1 Measuring cell fuse replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . 78
7.8 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
7.9 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
7.10 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
8.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
8.2 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
9.1 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83
9.1.1 Interferometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83
9.1.2 Measuring cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84
9.1.3 Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
9.1.4 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
9.1.5 Optional accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87
9.2 NIRFlex spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90
9.3 NIRFlex Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
9.4 NIRFlex Solids Transmittance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
9.5 NIRFlex Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
9.6 NIRFlex Fiber Optic Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
9.7 NIRFlex Fiber Optic Solids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
9.8 NIRFlex Fiber Optic SMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
9.9 Transflectance adapter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
10.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . . 94
10.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
5 NIRFlex N-500 Operation Manual, Version E
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.
1 About this manual
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• NIRCal•
®
Kimwipes• Meliseptol•
1.2 Abbreviations
®
is a registered trademark of BÜCHI Labortechnik AG
is a registered trademark of BÜCHI Labortechnik AG
®
is a registered trademark of Kimberly Clark
®
is a registered trademark of B. Braun
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
6 NIRFlex N-500 Operation Manual, Version F
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 Safety
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 mate-•
rials and surfaces
7 NIRFlex N-500 Operation Manual, Version F
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.
2 Safety
★★★★
WARNING
CAUTION
NOTICE
no
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.
Table of supplementary safety information symbols The reference list below incorporates all safety information symbols used in this manual and their
meaning.
Symbol Meaning
Indicates a hazardous situation which, if not avoided, could result in death or serious injury.
Indicates a hazardous situation which, if not avoided, may result in minor or moderate injury.
Indicates possible property damage, but no practices related to personal injury.
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.• ...• ...•
★★★☆
★★☆☆
★☆☆☆
(property damage only)
General warning
Electrical hazard
LASER emission
8 NIRFlex N-500 Operation Manual, Version F
Symbol Meaning
Explosive gases, explosive environment
Hot item, hot surface
Device damage
Fragile components
2 Safety
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.
9 NIRFlex N-500 Operation Manual, Version F
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.
2 Safety
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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2 Safety
Risk of instrument damage by mechanical shocks.
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
NOTICE
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•
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.
11 NIRFlex N-500 Operation Manual, Version F
Sticker on top of the housing, near the Measure­ment Cell connector.
Device labels Meaning Location
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 Safety
LASER emission Sticker inside housing, at the LASER module
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.
12 NIRFlex N-500 Operation Manual, Version F
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
Polarizers Glass
Housing Polyurethane foam
Detector InGaAs
Magnets NdFeB
3 Technical data
2
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
Ambient temperature 5−35 °C ( 25 ± 5 °C recommended)
Pollution degree 2
Installation category II
Spectral range 800 - 2500 nm (default 1000 - 2500 nm)
Resolution 8 cm-1 (with boxcar apodisation)
Type of interferometer Polarisation interferometer with TeO
Wavenumber accuracy ± 0.2 cm
S/N 10000 (peak-to-peak noise of a linear corrected baseline
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
to 67 % at 35 °C, max. 2500 m, for indoor use only
-1
12‘500 - 4‘000 cm
(default 10‘000 - 4‘000 cm-1)
(if not specified otherwise for measuring cell)
wedges
-1
(measured with HF gascell at an ambient
2
temperature of 25 °C ± 5 °C)
-1
between 5600−6000 cm
, measured with NIRFlex
Liquids, 2 x 64 scans, Blackman apodisation)
13 NIRFlex N-500 Operation Manual, Version F
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)
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 Technical data
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)
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
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
Ambient temperature 5−35 °C ( 25 ± 5 °C recommended)
Pollution degree 2
Installation category II
Spectral range 12’500 - 6’000 cm
35 °C, max. 2500 m, for indoor use only
to 67 % at 35 °C, max. 2500 m, for indoor use only
-1
(recommended range 11’520 - 6000 cm-1)
800−1660 nm (recommended range 870 - 1660 nm)
Photometric dynamic range 0 - 6 AU
14 NIRFlex N-500 Operation Manual, Version F
3 Technical data
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
-7
T
Typical signal-to-noise ratio
series. The difference had been < 2 x 10 at 7’876 cm
-1
rms for spectral segments of 300 cm-1 in the range of 11’000 - 6’500 cm
-1
open beam
5 mm white standard
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
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
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-
Time needed to reach a stable control of the set temperature Ambient temperature to 65 °C: 15 min
mean 2 x 10-5 AU (16 scans; Blackman apodization)
-5
mean 10 x 10
AU (64 scans; Blackman apodization)
decreasing to 67 % at 35 °C, max. 2500 m, for indoor use only
± 0.5 °C
length of 2 mm, when spacers are used, 1, 5, 10 mm cuvettes can be inserted as well
15 NIRFlex N-500 Operation Manual, Version F
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
3 Technical data
Technical data Transflectance adapter (Fiber Optic Solids)
Max. operating temperature 120 °C
Material Transflectance sleeve material: Steel no. 1.4435
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
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
Spacer ring material: Steel no. 1.4305 Transflectance adapter window: Quartz glass (Infrasil 303) sealed with fluorine rubber O-rings
to 67 % at 35 °C, max. 2500 m, for indoor use only
16 NIRFlex N-500 Operation Manual, Version F
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
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.).
3 Technical data
to 67 % at 35 °C, max. 2500 m, for indoor use only
17 NIRFlex N-500 Operation Manual, Version F
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.
4 Description of function
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 tempera-• ture 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.
18 NIRFlex N-500 Operation Manual, Version F
4 Description of function
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.
H G
Effective NIR light path
A B
NIR light source assembly with spare lamp and motorized parabolic reflector
First polarizer
a
F + b
c
LASER – 633 nm
DE
B
f
Spare lamp
e
+ dC
A
C D E F G H
Reference laser signal path
a b c d e f
19 NIRFlex N-500 Operation Manual, Version F
Comparator (double refracting block)
Stationary double refracting wedge
Moving double refracting wedge
Second polarizer
Sample
Interferogram detector
Laser output window
Second polarizator (works as a beam splitter for the laser)
Laser output-power sensor
First polarizer
Laser feedback detector
Linear motor for wedge movement
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.
4 Description of function
Measuring cell matrix
Sample characteristics
(for NIR light)
Diffuse reflection 4.2.1 NIRFlex Solids;
Transmission 4.2.3 NIRFlex Liquids;
Section Measuring cell Typical application
Predominantly non-translucent NIRFlex Fiber Optic Solids; NIRFlex Fiber Optic SMA*
materials such as most tablets,
cereals and powders
Translucent and transparent liquids NIRFlex Fiber Optic Liquids NIRFlex Fiber Optic SMA*
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*
*Depending on the custom accessory
and measurement setup
Solids with weak diffuse reflection
and low transmission rate charac-
teristics
20 NIRFlex N-500 Operation Manual, Version F
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
4 Description of function
Sample cup / petri dish
NIR light
NIRFlex Fiber Optic Solids / SMA:
Small, defined gap for liquid samples
Detector
Fiber optics (example)
Small gap for liquid samples
Diffuse reflecting / reference plate
21 NIRFlex N-500 Operation Manual, Version F
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.
4 Description of function
Sample material
NIR light
Detector
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.
22 NIRFlex N-500 Operation Manual, Version F
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.
4 Description of function
pathlength
Cuvette
NIR light
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.
Sample
Detector
Collecting lens
23
NIR light
Detector
NIRFlex N-500 Operation Manual, Version F
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 Description of function
a b c
a Main switch b Primary fuses c Power supply socket d Type plate with serial number
4.3.1 Lamp unit
The lamp unit comprises two lamp modules:
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.
4
e
g
f
e Ethernet connection f Interfaces for service intervals (USB 1, USB 2, KBD, MS,
VGA, COM)
g Ventilation filter
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.•
24 NIRFlex N-500 Operation Manual, Version F
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
4 Description of function
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.
25
NIRFlex N-500 Operation Manual, Version F
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
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
4 Description of function
Basic Advanced
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.
26 NIRFlex N-500 Operation Manual, Version F
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 Description of function
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.
27 NIRFlex N-500 Operation Manual, Version F
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
4 Description of function
Each measuring cell is equipped with an operating panel:
a
b
c
a LED b START 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.
c STOP button
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.
28 NIRFlex N-500 Operation Manual, Version F
4.6.2 NIRFlex Solids
List of NIRFlex Solids add-ons
Max. number of samples per sequence
Measurement based on diffuse reflection
Measurement based on transflectance
Measurement with petri dishes
Measurement with vials - x - - -
Measurement of tablets - - x - -
Measurement using small plastic bags
Internal reference x - - x x
External Reference x x x x x
Sample dimensions Spinner 34 mm
Spinner / Petri dish
add-on
1 6 10 1 1
x x x x -
x - - - x
x - - - -
- - - x -
Petri dish 100 mm
4 Description of function
Vial add-on Tablet add-on XL add-on Flow cell
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.
29 NIRFlex N-500 Operation Manual, Version F
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