BUCHI N-500 User Manual

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Operation Manual

NIRFlex

N�500

093020

Table of contents

1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

1.1 Trademarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

1.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2 Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

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 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

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 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

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

3 NIRFlex N-500 Operation Manual, Version E

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 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

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 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

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

NIRFlex N-500 Operation Manual, Version E

Table of contents

7 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66

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 Storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81

8.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81

8.2 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81

9 Spare parts and accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83

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 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94

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 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

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•

10 NIRFlex N-500 Operation Manual, Version F

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

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

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

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

F + b

LASER – 633 nm

Spare lamp

+ dC

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

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.

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.

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 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

4 Description of function

a Detector b Magnet sensor c Status LED d START button e STOP button f Internal reference g Magnetic coding h Sample i Petri dish

Functional principle of the NIRFlex Solids

j Petri dish holder k Rotary plate l Motor m Optic 1 n Light barrier o Mirror 1 p Mirror 2 q Optic 2

4.6.3 Petri dish add-on for NIRFlex Solids

NIRFlex Solids with petri dish add-on

The NIRFlex Solids with the petri dish add-on is the ideal conﬁguration to measure solid samples in standard glass petri dishes. The petri dish add-on also enables to use a transﬂectance cover to analyze liquids (e.g. solvents, milk, etc.). The transﬂectance technique is a good compromise for customers, who only analyze liquids occasionally. To carry out the reference measurement, the user has to place the External Reference (see also section 5.10) onto the sample window.

30 NIRFlex N-500 Operation Manual, Version F

4.6.4 Vial add-on for NIRFlex Solids

NIRFlex Solids with vial add-on

The NIRFlex Solids with the vial add-on is the ideal conﬁguration to measure solid samples in glass vials. This special add-on is equipped with 6 positions for sample vials with a diameter of 10−15 mm. Buchi provides one type of glass vials as an optional accessory for this speciﬁc add-on. This built-in External Reference is measured automatically without any interaction of the operator. A measurement sequence consists of a measurement of the reference and afterwards the measurement of the sample positions (1−6), which have been pre-deﬁned in the NIRWare Operator. The actually measured spectrum is set against the last measured reference.

4 Description of function

4.6.5 Tablet add-on for NIRFlex Solids

NIRFlex Solids with tablet add-on

The NIRFlex Solids with the tablet add-on is the ideal conﬁguration to measure tablets in diffuse reﬂection mode. This special add-on is equipped with 10 sample positions for round tablets with a diameter between 5−10 mm. This built-in External Reference is measured automatically without any interaction of the operator. A measurement sequence consists of a measurement of the reference and afterwards the measurement of the sample positions (1−10), which have been pre-deﬁned in the NIRWare Operator.

31 NIRFlex N-500 Operation Manual, Version F

4.6.6 XL add-on for NIRFlex Solids

NIRFlex Solids with XL add-on

The NIRFlex Solids with the XL add-on is the ideal conﬁguration to measure solid sample in undeﬁned sample containers, like bags, beaker glasses, etc. The sample container is placed on the ﬂat add-on directly over sampling window. The sample holder will not rotate during the measurement. To carry out the reference measurement, the user has to place the External Reference (see also section 5.10) onto the sample window.

4 Description of function

4.6.7 XL add-on with iris aperture for NIRFlex Solids

The NIRFlex Solids with the XL add-on with iris aperture is the ideal conﬁguration to measure solid samples in bigger glass vials with an diameter of up to 39 mm. The sample holder will not rotate during the measurement. To carry out the reference measurement, the user has to place the External Reference (see also section 5.10) onto the sample window.

XL add-on with iris aperture

NIRFlex N-500 Operation Manual, Version F

4.6.8 XL add-on for B+L sample cups for NIRFlex Solids

The NIRFlex Solids with the XL add-on for B+L (Bran+Luebbe) sample cups is the ideal conﬁguration to measure solid sample in the B+L closed cup. The sample holder will not rotate during the measurement.

NOTE

For reference measurement remove the B+L cup ﬁrst. Place the centering ring and the External Reference onto the XL add-on and perform the measurement.

4 Description of function

XL add-on for B+L sample cups

4.6.9 External Reference for XL and petri dish add-on

External Reference

An External Reference is needed when the XL add-on or the petri dish add-on is used on the NIRFlex Solids. The reference holder is designed with an opening to insert the External Reference into the correct position.

NOTE

The reference holder is needed with the petri dish add-on only.

33 NIRFlex N-500 Operation Manual, Version F

4.6.10 Spinner add-on

NIRFlex Solids in combination with the Spinner add-on is the ideal conﬁguration to measure smaller solid samples whereas the volume of a petri dish is too big. This add-on can also be used with a transﬂectance cover to analyze liquids (e.g. solvents or milk). The transﬂectance technique is suitable for customers, who analyze liquids occasionally.

4 Description of function

Spinner add-on

Cuvettes (i.e. Hellma cuvette) or glass vials with a diameter of 34 mm can be used as sample vessel in the motor-driven Spinner. For reference measurement the Spinner can hold the External Reference.

4.6.11 Flow-cell adapter add-on

The NIRFlex Solids with ﬂow-cell adapter add-on is the ideal conﬁguration to measure liquids (e.g. solvents and milk.) in a quartz ﬂow-through cuvette with 1 mm pathlength.

Flow-cell adapter add-on

To connect the ﬂow-cell, silicone tubes with 4 mm inner and up to 7 mm outer diameter can be used. External referencing requires a clean and dry ﬂow-cell. In some applications, referencing can also be done with measurement solvent in the ﬂow-cell.

34 NIRFlex N-500 Operation Manual, Version F

4.6.12 NIRFlex Solids Transmittance

NIRFlex Solids Transmittance

It is a major request described in the pharmacopoeias to ensure consistency of dosage units; each unit in a batch should have active ingredient content within a narrow range around the label claim. Traditionally these analyses are made using HPLC determining only the active content, which is time consuming and very costly. The speed, efﬁciency, and cost situation can be very much improved by NIR spectroscopy.

4 Description of function

a Aperture 3 mm b Sample c Detector d Optic 3 e Sample plate f Magnetic coding g Magnetic sensor h Light barrier

Functional principle of NIRFlex Solids Transmittance

i Stepper motor j Optic 1 k Aperture l Mirror m Optic 2 n Status LED o START button p STOP button

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4 Description of function

Transmission measurements offer the advantage of collecting the information from the entire cross section of the samples. This is ideal, especially for coated or multilayer tablets. NIRFlex N-500 is optimized for transmission measurements of solid dosage forms, like tablets or capsules.

a Detector b Sample position

Sensor position and beam path

4.6.13 Sample plates for the NIRFlex Solids Transmittance

The autosampler accepts up to thirty samples with a diameter of 4 to 12 mm maximum. The picture shows an example of a 30-place sample plate.

For samples larger than 12 mm up to 30 mm, 10-place sample plates are available. The picture shows an example of a 10-place sample plate.

The picture shows the 10-place sample plate with iris aperture for method development.

36 NIRFlex N-500 Operation Manual, Version F

4 Description of function

The picture shows the SST sample plate.

The picture shows an examle of a 30-place sample plate for hard gelatin capsules.

Sample plates of the NIRFlex Solids Transmittance

4.6.14 NIRFlex Liquids

NIRFlex Liquids

The NIRFlex Liquids is the ideal conﬁguration to measure liquids like solvents, oils, etc. in transmission mode using glass cuvettes. The NIRFlex Liquids enables quantitative and qualitative analyses with thermostated conditions of the samples (from room temperature plus 10 °C up to 65 °C. The NIRFlex Liquids can accommodate up to six cuvettes with pathlengths up to 10 mm. Current and set temperatures are displayed in the user interface.

37 NIRFlex N-500 Operation Manual, Version F

4 Description of function

a STOP button b START button c Status LED d Detector e Optic 2 f Ventilation g Heating h Motor

Functional principle of the NIRFlex Liquids

i Optic 1 j Mirror k Aperture l Light barrier m Magnetic coding n Magnet sensor o Reference position

38 NIRFlex N-500 Operation Manual, Version F

4.6.15 NIRFlex Fiber Optic Solids

NIRFlex Fiber Optic Solids

The NIRFlex Fiber Optic Solids is the ideal conﬁguration to measure solid samples in their original container. The reﬂection probe operates with a ﬁber bundle. The reﬂection probe can accommodate a transﬂectance adapter to analyze liquids as well (e.g. solvents, milk, etc.). The transﬂectance technique is a good compromise for customers, who only analyze liquids occasionally. The handle is equipped with a remote control for initiating the measurements remotely and displaying the results using LEDs on the handle. The LEDs at the handle of the ﬁber optic probe indicate the status of the system and the results of the prediction in routine operation.

4 Description of function

Applications without calibration (just measuring spectra, e.g. acquisition of calibration spectra)

- green LED ﬂashing measuring

- green LED on measurement ﬁnished

red LED on green LED on message on monitor

Application with calibration (routine use for predictions)

- green LED ﬂashing measuring

red LED on green LED on message on monitor

- green LED on result conforms

red LED on - result does not conform

Because the ﬁber optic probe is used at a certain distance from the spectrometer, the length of the ﬁber optic cables between the measuring cell (spectrometer) and the probe tip is about 2 m (3 and 5 m versions are available as well).

39 NIRFlex N-500 Operation Manual, Version F

4 Description of function

a Magnet sensors b LEDs: OK, not OK c START button d Handle e Fiber bundle f Electrical connections probe g Light barrier h Holder for ﬁber optic i Internal reference

Functional principle of the NIRFlex Fiber Optic Solids

j Optic 3 k Detector l Motor m Optic 1 n Optic 2 o Directly reﬂected rays are invisible for the ﬁber optic p Transﬂectance adapter q Magnet r External Reference

40 NIRFlex N-500 Operation Manual, Version F

4.6.16 Transﬂectance adapter for NIRFlex Fiber Optic Solids

The transﬂectance adapter is an optional accessory for the NIRFlex Fiber Optic Solids and enables to measure liquid samples, pastes and transparent ﬁlms. The transﬂectance measurement principle is a combination of transmission and diffuse reﬂection: The light coming from the optical ﬁbers penetrates the liquid sample in the gap between the probe window and the transﬂectance adapter window (½ pathlength), is diffusely reﬂected at the white standard layer behind the adapter window, passes the sample liquid in the gap a second time and goes back into the optical ﬁbers. The transﬂectance adapter is suitable for the analysis of viscous, non-agressive liquids. Thanks to the reproducible, adjustable pathlength it is suitable both, for the meausurement of slightly and of strongly absorbing samples. The transﬂectance technique is a good compromise for customers, who only analyze liquids occasionally. As the measurements are carried out in the original sample containers, the probe head needs to be dipped into the sample.

4 Description of function

Transﬂectance adapter

4.6.17 NIRFlex Fiber Optic Liquids

NIRFlex Fiber Optic Liquids

The NIRFlex Fiber Optic Liquids is the ideal conﬁguration to measure liquid samples in their original container. The transmission probe operates with monoﬁbers. As the measurements are carried out in the original sample containers, the probe head needs to be dipped into the samples. The handle is equipped with a remote control for initiating the measurements remotely and displaying the results using LEDs on the handle.

41 NIRFlex N-500 Operation Manual, Version F

4 Description of function

The LEDs at the handle of the ﬁber optic probe indicate the status of the system and the results of the prediction in routine operation.

Applications without calibration (just measuring spectra, e.g. acquisition of calibration spectra)

- green LED ﬂashing measuring

- green LED on measurement ﬁnished

red LED on green LED on message on monitor

Application with calibration (routine use for predictions)

- green LED ﬂashing measuring

red LED on green LED on message on monitor

- green LED on result conforms

red LED on - result does not conform

12 13

a Protection cover b LEDs: OK, not OK c START button d Handle e Monoﬁber ﬁber optic 2 m f Electrical connections g Light barrier

Functional principle of the NIRFlex Fiber Optic Liquids

h Holder for ﬁber optic i Internal reference j Optic 3 k Detector l Motor m Optic 1 n Optic 2

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4.6.18 NIRFlex Fiber Optic SMA

The NIRFlex Fiber Optic SMA is the ideal conﬁguration to measure both, liquids and solids with external accessories. The SMA-cell can be used to connect mono or multi ﬁbers via its two SMA connectors. Laboratory and immersion process probes in transmission or diffuse reﬂection mode as well as ﬂow-through cells can be attached.

4 Description of function

NIRFlex Fiber Optic SMA

NOTE

Glas ﬁbers have to be handled with care. Do not bend, pull or twist the ﬁbers! Follow the supple-• mentary instructions of the ﬁber and accessories. See also section 5.8! Depending on the application, distances of up to 100 m can be realized.• External referencing has to be perfomed with clean and dry accessory!•

43 NIRFlex N-500 Operation Manual, Version F

5 Putting into operation

This section describes how the instrument is installed and gives instructions on initial startup.

To avoid damage by condensate moisture, special attention is needed when the instrument was delivered at cold temperatures. Do not remove the instrument from its plastic bag for at least two hours to let the instrument acclimatize to the ambient temperature!

5 Putting into operation

Risk of instrument damage by moisture condensate.

NOTE

Inspect the instrument package for damage immediately after delivery. If necessary, prepare a status report immediately and inform customer and your local Buchi representative. Keep the original packaging for future transportation.

5.1 Transportation lock

The NIRFlex N-500 is equipped with a mechanical transportation lock to avoid damage of the interferometer during transportation and shipping by shocks and vibrations. The transportation lock is in “Locked” position at initial delivery.

After system installation and prior use, the interferometer has to be unlocked! See following section for information about unlocking.

Risk of instrument damage at use with engaged transportation lock.

NOTICE

Let the instrument sufﬁciently acclimatize before unpacking•

NOTICE

Disengage the transportation lock prior use• Keep shocks and vibrations away•

44 NIRFlex N-500 Operation Manual, Version F

5 Putting into operation

In the front of the main cover of NIRFlex N-500 there is an opening which is hidden behind the “Locked - Unlocked” shield. For the operation

of the transportation lock pull out the shield ﬁrst. Insert the torx screwdriver supplied with the instrument and ﬂip the locking mechanism by moving it to the side.

a LOCKING movement b Output window of the interferometer

c UNLOCKING movement

The installation position of the shield depends on the locking status of the transportation lock. The label of the shield in this image indicates a locked transportation lock.

Operating the transportation lock

5.2 Requirements concerning the installation site

Basic installation conditions

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•

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5 Putting into operation

The instrument must be installed:

indoor only with a clearance of 15 cm minimum to walls and any other objects• without being exposed to heating or cooling source (e.g. direct sunlight or air conditioning)• with the transportation lock in unlocked posit• ion (see previous section) on a stable and horizontal position•

NOTE

Because of its weight it is recommended to carry the instrument with two persons.

If the instrument is installed on a laboratory cart, the cart should have large, soft wheels (approx. 10 cm diameter) for better shock absorption at transport on even ﬂoors. To avoid damage by condensate moisture, special attention is needed when the instrument is moved between environments with bigger temperature difference! When moving the instrument from a colder to a warmer environment, let it acclimatize to the ambient temperature before switching it on!

Risk of instrument damage by moisture condensate.

The electric plug on the measuring cell is only designed to plug-in the measuring cells. Do not connect any other item. The spectrometer must be placed onto a clean, level and stable support. It is recommended to set up the spectrometer so that it is easily accessible from all sides. The spectrometer is normally operated from the front. Make sure that ergonomic and back-friendly operation is insured.

NOTICE

Let the instrument sufﬁciently acclimatize at relocation•

5.3 Electrical connection requirements

After the pre-installation procedure (all internal connections have been established and transportation lock is in unlocked position) has been completed successfully, the power plug of the NIRFlex N-500 can be connected to mains.

The used mains circuit has to:

provide the voltage that is given on the type plate of the instrument.• be able to handle the load of the connected instruments.• be equipped with adequate fuses and electrical safety measures, in particular proper grounding.•

See also technical data of all components regarding the different minimum system requirements!

Risk of instrument damage by wrong mains supply.

46 NIRFlex N-500 Operation Manual, Version F

NOTICE

External mains supply must meet the voltage given on the type plate• Check for proper grounding• Exchange defective cabling instantly•

NOTE

To cut the power in case of an emergency by unplugging, the instrument or any other item must • not block the mains plug! The plug must be able to be pulled out instantly at all time. Additional electrical safety measures such as residual current breakers may be necessary to meet • local laws and regulations! External power switches (e.g. emergency stop switches) must meet IEC 60947-1 and IEC • 60947-3 requirements. Such devices must be clearly labeled and accessible at any time. External connections and extension lines must be provided with a grounded conductor lead • (3-pole couplings, cord or plug equipment). All used power cords must meet the input power requirements.

5.4 Installing the instrument

To install the instrument, proceed as follows:

Connect the NIRFlex N-500 to the PC using the supplied Ethernet cable.• Connect the mains cable to the socket.• Switch on the NIRFlex N-500 via the main switch on the rear of the instrument.• Start the PC, and install the NIRWare software.• Set up the communication between NIRFlex N-500 and the PC.•

5 Putting into operation

5.4.1 Setting up the Ethernet communication

The NIRFlex N-500 is equipped with one Ethernet (LAN) socket at the rear side.

LAN

LAN settings of the NIRFlex N-500 The primary network connector (LAN1) is predeﬁned for direct communication to a PC.

Standard conﬁguration of the Spectrometer:

Static IP-address 192.168.1.1• Subnet mask 255.255.255.0•

NOTE

The default IP-address of the spectrometer can be changed to a customer speciﬁc static • IP-address provided by the local IT. This conﬁguration is done within the Service Tools and described in the NIRWare Online Help and the corresponding PDF-ﬁle. The spectrometer‘s IP-address can be reset to default (192.168.1.1) by pushing and holding • both, START and STOP button, at the measuring cell during the power-up procedure of the NIRFlex N-500 for about 50 seconds.

47 NIRFlex N-500 Operation Manual, Version F

LAN setup of the PC To establish communication, set up the IP of the connected PC in accordance to the local network

environment or via direct link as listed below.

IP-conﬁguration of the connected PC (direct link):

Static IP-address 192.168.1.2• Subnet mask 255.255.255.0•

5.4.2 Network integration

There are various possibilities how the NIRFlex N-500 can be installed and used. In the following, two examples are given:

5 Putting into operation

All data on one PC via direct link

The PC with the NIRWare database is directly connected to the NIRFlex N-500. All data remain on that speciﬁc PC.

NIRWare database on central company server via indirect link

The NIRWare database runs on a central company server. The Administrator has access to the database on that server. The data measured by the Operator are collected on the database of the central company server.

NOTE

Other setups i.e. with the NIRFlex N-500 directly attached to a local network can also be realized.

48 NIRFlex N-500 Operation Manual, Version F

5.5 Installing the measuring cells

All different measuring cells are provided with a plug connection.

Installing a measuring cell

To install a measuring cell, proceed as follows:

Place the measuring cell vertically into the provided space.• Carefully applying pressure to the measuring cell, make sure that the plug connection catches.• Make sure it is seated well by means of the centerning pins at the NIRFlex N-500. • Subsequently, fasten the measuring cell with the ﬁxating screw at the bottom of the NIRFlex N-500. •

5 Putting into operation

NOTE

When using the NIRFlex Solids Transmittance cell, put the sample plate onto the cell by inserting the central hole into the shaft. The guiding pin must be inserted into the corresponding hole (next to the handle).

Risk of measurement interruption and data errors by communication loss.

NOTICE

Fixate the measuring cell to the basic instrument using the ﬁxing screw at the bottom plate of • the instrument.

49 NIRFlex N-500 Operation Manual, Version F

5.6 Installing the cover of the NIRFlex Solids Transmittance

5 Putting into operation

Insert the tilted cover a and hook its left hinge onto to the bushing pin (hinge counterpart) at the rear left hand side of the measuring cell. Tilt the cover back into a straight position b.

Keep the right hinge of the cover in a matching position with the bushing screw. Fasten the screw c with a few turns (the screwdriver is part of the scope of delivery). Open and close the cover several times to verify the correct installation.

Risk of mechanical damage at the hinges of the top cover.

50 NIRFlex N-500 Operation Manual, Version F

NOTICE

Keep the top cover closed when the measuring cell is not installed• Carefully open and close the top cover to avoid mechanical stress at the hinges•

Additional handling instructions

5 Putting into operation

Install the measuring cell with the top cover • closed to avoid mechanical stress at the hinges! Keep the top cover closed during a measure-• ment to keep out scattered ambient light. Open and close the top cover carefully.•

At closing:

A small bumper avoids hard impact to the cover.

At opening:

Do not release the top cover until it is in fully open position! The hinges might break-away.

Additional handling instructions

5.7 Preparing the transﬂectance adapter

5.7.1 Adjusting the pathlength of the transﬂectance adapter to the probe head

When you receive the transﬂectance adapter with a new instrument: When you receive your transﬂectance adpater together with a new NIRFlex N-500 instrument, the

pathlength has already been adjusted to the probe head by the manufacturer.

When you receive the transﬂectance adapter as additional accessory for an instrument already installed:

As the probe head dimensions may vary slightly you need to adjust the transﬂectance adapter to the probe head when you receive it as additional accessory for an instrument already installed. A correct adjustment is necessary for the portability of spectra. To adjust the pathlength of the transﬂectance adapter to the probe head, the spacer ring 1 mm is used. The other spacer rings have been manufactured to ﬁt accordingly.

Normally, the transﬂectance adapter is delivered with the adjustment ring and the spacer ring 1 mm mounted. If this is the case, proceed with section 5.7.2.

51 NIRFlex N-500 Operation Manual, Version F

If this is not the case, proceed as follows:

5 Putting into operation

Slide the adjustment ring over the transﬂectance sleeve and • turn it on the thread as far as possible.

Now slide the 1 mm spacer ring over the transﬂectance • sleeve, so that the pin on the inner surface of the spacer ring ﬁts into the groove in the adjustment ring.

Place the 1 mm spacer disk in the center of the transﬂec-• tance adapter window.

Slide the transﬂectance adapter over the probe head and • orient it so that the pin at the probe head is pushed into the groove of the spacer ring. Push the transﬂectance sleeve upwards until the spacer disk •

NOTE

It is very important that the spacer disk is located on the window center, otherwise it could get stuck between the metal edges during the adjustment procedure, damage the windows and fail to indicate the correct distance between probe and adapter window.

seats solidly between the transﬂectance adapter window and the probe window and exactly determines the distance between those two. Tighten the retaining screw • a.

52 NIRFlex N-500 Operation Manual, Version F

5 Putting into operation

Now turn the adjustment ring upwards until there is no • clearance between the adjustment ring and the spacer ring anymore. Tighten one of the three socket screws on the adjustment • ring by means of the allen key. Loosen the retaining screw and remove the transﬂectance • adapter from the probe head. Now tighten the remaining two socket screws on the adjust-• ment ring and the socket screw on the spacer ring.

Adjusting the pathlength

NOTE

The socket screw may be replaced by one of the knurled screws for easier exchange.

The pathlength of the transﬂectance adapter is now adjusted to this speciﬁc probe head, so that both form a functional unit. The pathlength now matches the engraving of the spacer ring in each case and no additional adjustment is necessary, when you change from one spacer ring to another.

5.7.2 Exchanging the spacer ring

To exchange the spacer ring in order to work with another pathlength, proceed as follows:

Loosen the screw on the spacer ring by means of the allen • key. Remove the spacer ring.• Take the new spacer ring you want to operate with, slide it • over the transﬂectance adapter and tighten the screw.

Exchanging the spacer ring

5.7.3 Installing the transﬂectance adapter to perform measurements

To perform a measurement, slide the transﬂectance adapter over the probe head and orient it so that the pin at the probe head is located in the groove of the spacer ring. Tighten the retaining screw.

NOTE

When performing measurements, make sure that there are no air bubbles in the measuring gap (pathlength) between probe and adapter window by carefully moving the probe head in the sample.

When you do not perform any measurements with the transﬂectance adapter, store it in the plastic box.

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5 Putting into operation

5.8 Installing measurement equipment to the NIRFlex Fiber Optic SMA

To install the instrument, proceed as follows:

left connector = short spring

right connector = long spring

To mount the SMA-adapter onto the optical ﬁber cable:

Put the spring onto the ﬁber connector • and secure the end of the connector with the threadened spacer nut.

NOTE

The spring must be freely movable after installation! Fasten the spacer nut handtight only!

Insert the optical ﬁber cable.• Place it into the cable-slot of the stress • relief and swivel the stress relief to match the screw heads at the SMA socket. Push the stress relief against the spring • of the optical ﬁber cable and swivel it into vertical position. Fasten the two ﬁxating screws of the • stress relief hand-tight.

Fixate the optical cable with cable ties.•

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5.9 Starting up the system

An automatic initialization process starts as soon as the NIRFlex N-500 and the PC are started up. The main components of the spectrometer are identiﬁed and its basic functions are checked during that initialization process, e.g. lamp unit, standard wheel, laser unit, measuring cell. The time needed for initialization is about 60 seconds.

5.9.1 System Suitability Test

The

System Suitability Test (SST) serves as an internal functionality and performance test of the

spectrometer. It is recommended to run an SST after each restart of the NIRFlex N-500 to monitor and verify the system performance.

The following SST values are tested:

Internal system temperatures (e.g. Laser, interferometer, detectors) • Linearity• Signal-to-noise ratio• Wavenumber stability•

5 Putting into operation

At the end of each SST a report protocol will be generated. The test results are compared to values ex factory and inform the user about the system condition.

➥ The report data are stored in the internal database for service and quality control.

NOTE

The time between two SST requests can be set with the NIRWare Application Designer. The recommended standard value between two tests is 24 hours, a test-run takes approximately 5 min. Test results can be exported and stored in XML-format, e.g. for service purpose.

If the instrument is used in continuous operation (e.g. several days of ON-time), a longer checking interval might be suitable. However, frequent tests should be performed to minimize the risk of erroneous measurement.

5.9.2 Temperature tests in detail

The system is equipped with numerous temperature sensors. Individual lower and upper temperature limits are predeﬁned for each sensor. ➡ To pass this test, all actual temperature values must be within the limits.

NOTE

Mind the ambient temperature data as listed in section 3, Technical data.

If temperature is too low • ➡ let system warm up sufﬁciently

If temperature is too high • ➡ clean ﬁlters and provide sufﬁcient airﬂow

5.9.3 NIR linearity test

With this test the linearity of the intensity scale of the spectrometer is being tested. The absorbance of a set of ﬁve gray ﬁlters in the standard wheel is measured sequentially and compared with reference values.

➡ To pass this test, all absorbance factors must be within the tolerance.

55 NIRFlex N-500 Operation Manual, Version F

5.9.4 Signal-to-noise ratio determination

With this test the ratio of signal power to noise power is determined. A high ﬂux (maximum intensity) and a low ﬂux (10% intensity) beam is being analyzed for a number of wavenumber intervals.

➡ To pass these tests, the average and the minimum values must be within the tolerance.

5.9.5 Wavenumber stability test

The wavenumber stability of the system is checked with the PMMA reference plate of the reference wheel. One absorption peak of the transmission spectrum is being analysed and compared to its reference value.

➡ To pass this test, the wavenumber accuracy must be within the tolerance.

5.9.6 SST with NIRFlex Solids Transmittance

The SST for the NIRFlex Solids Transmittance is extended in comparison to the SST for the other measuring cells. It is performed with the special SST sample plate, which is provided with every NIRFlex Solids Transmittance, and the internal standard wheel. Wavelength accuracy is measured in transmittance using a mixture of Rare Earth Oxides. Noise measurements are performed with open beam and with the 5 mm white standard disk both high and low ﬂux. The linearity tests are performed for open beam, 1 mm and 5 mm white standard disks together with the grey ﬁlters of the internal standard wheel covering the complete photometric dynamic range.

5 Putting into operation

5.10 Reference measurements

Frequent reference measurements compensate for environmental effects, which might inﬂuence the spectra. Each measuring cell offers a possibility for the reference measurement, the External Refer- ence. Some measuring cells additionally offer the possibility of an internal referencing.

External Reference In order to measure the transmittance or the reﬂectance of a sample, the measured intensity spectrum

of the sample is divided by a reference spectrum. This reference spectrum is either recorded without a sample (in case of transmittance) or with a white standard in the sample position (reﬂectance). We call this an External Reference. An External Reference is always required.

Internal reference While the acquisition of an External Reference can be automated in some cases (NIRFlex Liquids,

NIRFlex Solids Transmittance, Vial and Tablet add-on for NIRFlex Solids), in other cases the measurement of an External Reference requires user interaction (petri dish and XL add-on for NIRFlex Solids, NIRFlex Fiber Optic Solids, and NIRFlex Fiber Optic Liquids). In these cases internal referencing is used to minimize the need for external referencing and user interaction.

Internal and External Reference measurements provided by the measuring cells/add-ons

Measuring cell / Add-on Internal reference External Reference

NIRFlex Solids with petri dish add-on x manually

NIRFlex Solids with vial add-on - built-in

NIRFlex Solids with tablet add-on - built-in

NIRFlex Solids with XL add-on - manually

NIRFlex Solids with Flow Cell add-on - manually

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5 Putting into operation

Spectrum =

sample

ext. reference

Spectrum =

sample (recent) / int. reference (recent)

ext. reference (old) / int. reference (old)

Internal and External Reference measurements provided by the measuring cells/add-ons

Measuring cell / Add-on Internal reference External Reference

NIRFlex Solids with Spinner add-on - manually

NIRFlex Solids Transmittance - built-in

NIRFlex Fiber Optic Solids x manually

NIRFlex Fiber Optic Liquids x manually

NIRFlex Liquids - built-in

NIRFlex Fiber Optic SMA (+ individual accessories)

without internal reference:

with internal reference:

x manually

For more information on the reference measurements, see also section 6.

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6 Operation

This section describes how to start a measurement and how to prepare a reference measurement and gives recommendations on possible applications of the instrument.

6 Operation

Risk of instrument damage at use with engaged transportation lock.

NOTICE

Disengage the transportation lock prior use• Keep shocks and vibrations away•

6.1 General recommendations for measuring solids

The calibration wavelength range with a standard ﬁber optic probe goes from 4500 to 10000 cm-1. For quantitative applications the ﬁber optic probe should be ﬁxed. Hygroscopic samples show temperature dependency. The samples should either be measured at a constant temperature or the temperature inﬂuences must be considered during calibration. Coarse grained samples must be possibly milled before carrying out the measurement. Number of scans: Qualitative calibration: 4−16 (max. 32); quantitative calibration: 16−32; granules: 64. The spectral range of the NIRFlex Solids Transmittance is limited to 6000 cm-1. The number of scans should be 64 by default.

General recommendations for measuring solids

Sampling option Substance External Reference measurement Comment

NIRFlex Fiber Optic Solids Homogenous powder

(qualitative) solids with ﬂat surface

NIRFlex Solids with petri dish add-on

NIRFlex Solids with XL add-on Powder in containers

NIRFlex Solids with vial add-on

NIRFlex Solids with Spinner add-on

NIRFlex Solids Transmittance tablets, capsules,

Powder (quantitative) granules

pellets

Powder in small glass vials

Powder (quantitative), granules

powders in small plastic cups

White standard in the reference cap

White standard in a reference holder

White standard on XL add-on

White standard in vial add-on

White standard in a reference holder

Open beam (reference position in sample plate)

Make sure that there is enough sample in the dish so that all the light is reﬂected by the sample

Make sure that there is a constant bulk density, a constant sample container quality and a reproducible container position

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6.2 General recommendations for measuring liquids

For sample measurements with the NIRFlex Liquids, make sure that the cuvettes are placed in the direction of the centre of the cuvette holder. This is important to ensure optimal heat transfer to the sample. The calibration wavelength range with glass cuvettes goes from 4000 to 10000 cm-1.

The useable wavelength range for measurements with a ﬁber optic probe is 4500 – 10000 cm-1. Temperature differences can cause a spectral shift. The samples should either be measured at a constant temperature or the temperature inﬂuences must be considered during calibration. Avoid air bubbles. Number of scans: Qualitative calibration: 4−10; quantitative calibration: 16−32 (max 64)

General recommendation for measuring liquids

Sampling option Substance External Reference measurement Comment

NIRFlex Liquids Transparent liquids Built-in External Reference

(air)

NIRFlex Fiber Optic Liquids Transparent liquids

aggressive, trans-

parent liquids

NIRFlex Solids with petri dish add-on and transﬂectance cover

Clear liquids, turbid liquids

Clean probe head Max. temperature

Empty petri dish with transﬂectance cover

6 Operation

1, 2, 5, 10 mm cuvette with spacer

150 °C

avoid air bubbles

Avoid air bubbles

NIRFlex Solids with ﬂow-cell adapter add-on

NIRFlex Solids with Spinner add-on and transﬂectance cover

NIRFlex Fiber Optic Solids with transﬂectance adapter

6.3 Starting a measurement

The spectrometer needs a warm-up time of approx. 15 min. The lamp and the laser within the instrument will be switched on as soon as the NIRWare software is running.

When the instrument has warmed up and the sample is presented to the instrument, you can start the measurement.

Generally, you have two possibilities to do so:

Press the START button at the measuring cell.1. Click the Start icon (green arrow) in the NIRWare Operator.2.

NOTE

When you are working with the NIRFlex Fiber Optic Solids or NIRFlex Fiber Optic Liquids probe, you can also use the remote button on the handle to start a measurement.

Clear liquids, turbid liquids

Clean ﬂow cell Avoid air bubbles

Empty cuvette with transﬂectance cover

Clean probe head Make sure there

Avoid air bubbles

are no air bubbles in the gap

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6.4 NIRFlex Solids

6.4.1 Reference measurement for the Petri dish add-on

A pop-up will remind the operator to measure the External Reference as soon as a certain time window (predeﬁned in the Application Designer) has passed.

A new External Reference is mandatory

when a new application is selected• when an add-on or a new measuring cell is selected• every time the software is restarted•

To measure the External Reference, proceed as follows:

Remove any sample from the add-on and ensure that the glass window is clean.• Make sure that the bottom side of the External Reference and its holder is clean.• Place the holder with the External Reference on the petri dish add-on and measure the External • Reference.

6 Operation

6.4.2 Reference measurement for the XL add-on

A pop-up window will remind the operator to measure the External Reference as soon as a certain time window (predeﬁned in the Application Designer) has passed.

A new External Reference is mandatory

when a new application is selected,• when an add-on or a new measuring cell is selected, or• every time the software is restarted.•

To measure the External Reference, proceed as follows:

Remove any sample from the add-on and ensure that the sample glass window is clean.• Make sure that the bottom side of the External Reference and is clean.• Place the External Reference on the XL add-on, rotate it until the mark on the reference is next to • the hole in the XL add-on, and measure the External Reference.

6.5 NIRFlex Solids Transmittance

Diffuse transmission measurements are very demanding applications, because only a very small part of the incident light is transmitted. Therefore care must be taken for good signal-to-noise ratio. The design of the NIRFlex Solids Transmittance and its optimized detector ensure best performance. NIRFlex Solids Transmittance uses a low energy source, which avoids any overheating of the samples and therefore enables the analysis of temperature sensitive active ingredients. Emissions e.g. from ﬂuorescent tubes can cause artifacts in the sample spectrum. Therefore the cover of NIRFlex Solids Transmittance must be closed during measurements.

Risk of incorrect measurement results by ambient light

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NOTICE

Keep the top cover closed during a measurement•

6 Operation

Typical samples for the NIRFlex Solids Transmittance include tablets, hard gelatin capsules, powders or soft gelatin capsules including semi-liquids or oily liquids, which requires a very high dynamic photometric range of the system. The design of the measuring cell takes this requirement into account. Without any special settings the user will generate spectra with optimized signal-to-noise ratio for his speciﬁc samples. For reproducible and accurate results in tablet transmission measurements, it is essential to prevent stray light caused by light passing around the side of the tablets. Therefore the sample plates are individually customized in order to ﬁt perfectly for your tablets and to ensure the optimal performance. Additionally the sample plates exhibit a specially selected coating to prevent reﬂection and light leakage.

All sample plates include an External Reference position. By default reference measurements are performed automatically before every measurement sequence.

6.6 NIRFlex Liquids

System preparation The liquid cell must reach a stable working temperature before a measurement can be performed. The

heat-up time depends on the ambient temperature.

Starting at standard ambient temperature of 25 °C the measurement cell needs:

approximately 15 minutes to stabilize at 35 °C.• approximately 30 minutes to stabilize at 60 – 65 °C.•

Depending on the heat distribution and the positioning of the cuvettes the temperature difference between probe and liquid temperature is about 2 °C at a measurement temperature of 65 °C.

Risk of damage at the coating of the sample plate

Risk of measurement errors by unsufﬁcient heat-up time

NOTICE

Do not cleat the sample plate in a dishwasher• Clean the sample plate with Ethanol and a soft, lint-free tissue•

NOTICE

Cuvettes and sample material must be completely heated-up at measurement•

NIRFlex Liquids measurement cell

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6 Operation

CAUTION

Minor or medium burns by hot surfaces

Do not touch the cell chambers•

NOTE

The software does not prevent measurements in case of incorrect temperatures. The operator is responsible, that the current temperature corresponds with the set temperature. A reproducible temperature of the samples is crucial when carrying out measurements in transmission mode. The heat-up time of the sample material must be sufﬁcient to reach the measurement cell temperature.

Working with different types of cuvettes

For most of the applications running with the NIRFlex Liquids, the use of 2 mm cuvettes is recommended. However, the cell is designed to use 1, 5 and 10 mm cuvettes as well. If doing so, the spacers, which ﬁx the cuvettes in the measurement position, must be changed. A set of different spacers is included in the scope of delivery.

For quadratic cuvettes :

No spacers are required.

For rectangular cuvettes:

All rectangular cuvette types must be installed in pairs with a matching spacer!

The cuvette must be aligned to the turning • hub (inner circle of the cell). A matching spacer must be aligned to the • outer circle of the cell.

Handling of different cuvette types

NOTE

Quartz glass cuvettes are recommended when working with the NIRFlex Liquids. Most plastic cuvettes show a signiﬁcantly higher light absorption rate which can reduce the determination performance. This also has direct inﬂuence onto calibration and reproducibility. Make sure that the radiated surfaces of the cuvettes are placed perpendicular to the beam of light.

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Risk of ﬁre by highly ﬂammable materials

Do not insert highly ﬂammable materials or samples into the measurment cell•

6.7 NIRFlex Fiber Optics

All ﬁber optics must be treated with special care to avoid breaks and other damages of the glass ﬁbers and optical surfaces! Cleaning should always be done manually with a soft, lint free damp cloth with mild soapy water. Optical surfaces can be cleaned with Kimwipes.

WARNING

6 Operation

Risk of damage at the ﬁber optics

Do not bend the ﬁber optics to a radius smaller than 15 cm• Do not overstrech or twist the ﬁber optics• Do not expose the ﬁber optics to heavy impacts or punctual pressure• Do not bring the ﬁber optics into contact with organic solvents, acids or alkaline solutions• Do not bring the white standard into contact with furanes, acids and other oxidizing agents•

6.7.1 NIRFlex Fiber Optic Solids

The handle is equipped with a remote control for initiating the measurements remotely and displaying the results using LEDs on the handle. Because the ﬁber optic probe is used at a certain distance from the spectrometer, the length of the ﬁber optic cables between the measuring cell (spectrometer) and the probe tip is about 2 m (special versions with longer ﬁber optic cables are available on request).

Risk of damage at the white standard

Do not bring the white standard into contact with furanes, acids and other oxidizing agents•

NOTE

The software automatically detects the presence of a transﬂectance adapter but not the path-• length in use, so make sure to use the appropriate pathlength. It is not possible to start a reference measurement if the reference cap has not been detected by • the system.

NOTICE

Reference measurement

For correct measurements and correct results, it is necessary to record a reference spectrum regularly. For this purpose, use the reference cap. In order to avoid false results, the reference cap is detected automatically if installed.

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6.7.2 NIRFlex Fiber Optic Liquids

For most of the applications a pathlength of 1 or 2 mm is the best choice. Many samples will contain water or alcohol, which cause strong NIR absorptions. Therefore for the standard NIRFlex Fiber Optic Liquids a pathlength of 2 mm will be sufﬁcient (special versions with other pathlengths are available). For sample measurements with the NIRFlex Fiber Optic Liquids make sure that the quartz window in the probe head is in full contact with the sample to be analyzed. Despite its rugged design, the transmission probe requires careful treatment.

6.7.3 NIRFlex Fiber Optic SMA

This measurement setup is suitable for continuous online measurements. Special settings can be found in the NIRWare manual.

NOTE

Respect handling and operation information provided by the manufacturer of your custom optics / accessories.

6 Operation

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7 Maintenance

This section gives instructions on all maintenance work to be performed in order to keep the instrument in good working condition. In addition to this, adjustment jobs the operator can carry out by himself/herself are explained.

7 Maintenance and repairs

CAUTION

Risk of dangerous device status or defects and malfunctions when serviced by untrained personnel

Service and maintenance actions which require to open the device housing must be • performed by trained personnel only Switch off the device and disconnect the mains cable before any service, maintenance or • cleaning Do not touch live parts• Close the housing before reconnecting the device to mains•

7.1 Cleaning

To avoid cross-contamination and germ dissemination (e.g. by bacteria) the operator is advised to attend common laboratory biosafety measures in accordance the chosen application and environment. The “Laboratory Biosafety Manual” of the World Health Organization can be used as a practical guidance.

7.2 Housing

Clean the housing with a soft, lint free damp cloth with mild soapy water. For hygienic reasons, use surface disinfectant wipes in combination with similar disinfectant spray on alcohol basis. If the sample window on top of the instrument is dirty, clean it with an antimicrobial wipe (e.g. Melisptol® wipes).

WARNING

Risk of cross-contamination and germ dissemination at use

Exchange ﬁlter regularly• Keep the housing and the working area clean• Keep all surfaces in contact with sample material clean and free of germs• Use disinfectant to avoid germ dissemination• Do not reuse sample material•

Risk of damage at the housing

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NOTICE

Do not use any objects for cleaning which might scratch the optical surfaces or add-ons•

Do not clean coated optical surfaces in a washer.•

In order to avoid contamination by sample material between the measurements, clean the surfaces in direct contact with the sample after each measurement.

NOTE

Switch off the NIRFlex N-500 and all directly connected eletronic devices i.e. monitors before • cleaning the housing. Avoid scratches on optical surfaces as they can inﬂuence a measurement!• For coated optical surfaces, use abrasion-resistant precision cloths such as Kimwipes from • Kimberly-Clark. Primary cleaning can be done with disinfectant wipes on alcohol basis. Avoid ﬁngerprints on any optical surface!•

7.2.1 Optical surfaces and probes

All optical surfaces must be handled with care i.e. must not be scrached, cleaned with unproper cleaning medium. Do not apply excessive force to any part of the device or its accessories!

If the connectors for the measuring cell on the instrument are dirty, clean them with a soft cloth moistened with alcohol. In order to avoid contamination by sample material between the measurements, clean the surfaces in direct contact with the sample after each measurement. For this purpose, use abrasion-resistant precision cloths such as Kimwipes from Kimberly-Clark. Loose dust can be removed by blowing with clean and oil-free compressed air. If substances still adhere, you may additionally rinse the surfaces with acetone or alcohol.

7 Maintenance and repairs

Due to the limited resistance of the adhesive between metal and quartz glass, the ﬁber optic probe must not be in prolonged direct contact with organic solvents nor acids and alkaline solutions. Take it out of the liquid directly after completing the scans. To prevent contamination of the white standard reference make sure that it is always applied to a clean measuring cell.

Risk of damage at the coating of the sample plate

7.2.2 Cleaning of the External Reference

For dependable reference measurements the External Reference and Transﬂectance adapter must be clean and damage free. sary precautions, rinse it with pure acetone. Make sure to remove all cleaning residue.

NOTICE

Do not cleat the sample plate in a dishwasher• Clean the sample plate with Ethanol and a soft, lint-free tissue•

In case the External Reference is strongly contaminated despite the neces-

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7 Maintenance and repairs

Risk of damage at the External Reference

After treating the External Reference with pure acetone, always make sure that the acetone adsorbed by the reference material evaporates completely. For this purpose, you can place the External Reference in an oven for a few minutes at a maximum of 60 °C. The reference material adsorbs oils and fats.

7.2.3 Cleaning of the Transﬂectance adapter

The transﬂectance adapter should be cleaned regularly after each measurement in order to avoid a sample cross contamination during the next measurement. To clean the transﬂectance adapter you can rinse it with solvents suited for use with the materials of the adapter and probe (stainless steel, quartz glass, ﬂuorine rubber). After rinsing, dry the adapter thoroughly and carefully inspect it for remaining contaminations. Suited cleaning solvents are water, acetone, and alcohols.

NOTICE

Do not drop the External Reference•

Do not scratch the surface•

Never bring it in contact with hard objects.•

Do not use any cleaning media with abrasive character which might scratch the surface.•

Do not use item for reference measurement when damaged or scratched. •

Do not use any compressed air for blowing off dirt from the External Reference, as it often • contains oil and is not sufﬁciently pure.

Risk of damage at the Transﬂectance adapter

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NOTICE

Do not bring any part of the adapter into contact with Furanes, acids and other oxidizing • agents

NOTE

Exact cleaning procedures tailored to the indiviudal sample composition have to be developed by • the customer. When you analyze liquids of medium or high viscosity, sample residues may accumulate in the • measuring gap and all other gaps between the adapter and the probe. In this case, remove the transﬂectance adapter from the probe head to clean it thoroughly in order to avoid a sample cross-contamination during the next measurement.

7.3 Advanced testing with NIRWare Automatic Diagnose

In addition to the SST NIRWare 1.x includes the NIRWare Automatic Diagnose (NADIA). NADIA is a tool which enables Buchi service personnel to judge the condition of the NIRFlex N-500 or to do a performance check of the instrument as part of a service contract.

To start NADIA select Start > Programs > Buchi NIRSolutions > NIRWare > Nadia

7 Maintenance and repairs

Close the NIRWare Operator before starting NADIA. The Control System Service must be stopped during the test. NADIA will prompt you for permission to stop the Control System Service, if it detects a running Control System Service.

Click ‘Start’ to execute the Nadia test and follow the instructions on the screen. Once the test is ﬁnished, the following information is displayed:

Test result Nadia

The result is saved in an *.xml ﬁle, which is stored in the folder shown below:

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MyNadiaFiles

7 Maintenance and repairs

Send this ﬁle to your customer service organisation for evaluation. To archive the ﬁle, copy it to a different folder.

7.4 Lamp module replacement

The primary lamp module needs to be replaced quickly after failure. This action can be performed by a trained operator.

After failure of the primary lamp module, the following instructive message appears:

NOTE

When the primary lamp is broken the instrument automatically switches to the secondary lamp. In this case make sure to replace the primary lamp as soon as possible as the instrument does not work anymore in case of failure of the secondary lamp and this lamp has to be replaced by a Buchi service engineer.

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CAUTION

Risk of minor burns by hot lamp module.

Switch off the device ﬁrst and unplug the mains cable• Do not touch hot parts or surfaces• Let the lamp module cool down safely• Do not touch the bulb glass•

To replace a defective lamp module, proceed as follows:

• Switch off the instrument and unplug the mains cable. Let it

cool down safely! Loosen the two screws on the left rear of the instrument • approximately 3-5 turns. Remove the cover.•

For easy release of the housing slightly tilt the back part away from the screws. Then pull out the housing towards the rear side of the instrument. There is a built-in sensor to record the opening of the housing. A safety tack ensures that the lamp remains in the correct position.

Slide the safety tack to the upright position (counterclock-• wise). Pull the metallic housing with the primary lamp out of the • lamp unit. Exchange the primary lamp source with a new lamp by • removing it from the gray plug and connect the new primary lamp source to this plug.

7 Maintenance and repairs

Replacing the lamp module

Insert the new lamp into the lamp unit and slide the safety • tack back to the horizontal position until a metallic click sound is audible, which indicates the right position. Make sure that the gray plastic plug is in a vertical position.

Secure the housing of the lamp unit with the two screws on • the back side of the unit.

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7 Maintenance and repairs

NOTICE

Risk of instrument damage by ingress of particles.

Check proper seating of all housing parts before use• Do not operate instrument when housing is open or unlocked•

Resetting the lamp lifetime counter After lamp module exchange, the following message appears at power on:

Message concerning required instrument setup

Click the OK icon • to conﬁrm the message. Now click the Service icon • (Operator) and double-click ‘Assembly’.

NOTE

To correctly monitor the lamp lifetime the software hour counter has to be reset after each lamp replacement. At lamp exchange, the secondary lamp module is active.

The following dialog opens:

Assembly setup dialog

Click the icon next to the Lamp row • to reset the “housing open” status.

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Workﬂow to reset the lifetime counter of the primary lamp module

To establish the standard working conditions of the NIRFlex N-500:

7 Maintenance and repairs

Start the Operator software• Switch from “secondary lamp” • a to “primary lamp” Resetting the hour • b counter will bring up a prompt for conﬁrmation Conﬁrm the message • c to ﬁnally set the lamp lifetime counter to zero

➡ After this procedure, reboot the NIRFlex N-500 and restart the Operator software.

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7.5 Laser unit replacement

The LASER unit needs to be replaced at failure. This action can be performed by a trained operator or (preferably) by a service technician.

WARNING

Risk electric shock and burns by remaining high-voltage load at the LASER module

Do not disconnect the white plug from the laser power supply•

7 Maintenance and repairs

White plug at laser power supply

Risk of optical misalignment and damage at the LASER module.

To replace the laser, proceed as follows:

NOTICE

Do not touch the optical surfaces of the module• Handle the module with care i.e. do not expose the module to heavy impacts• Handle the module at the base plate only•

Loosen the two screws on the left rear of the • instrument approximately 3-5 turns.

Remove the cover.•

For easy release of the laser housing it is recommended to slightly tilt the housing and then pull it horizontally away from the instrument. There is a built-in sensor to record the opening of the housing.

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7 Maintenance and repairs

Disconnect the electric lasers power supply • plug.

Loosen the two screws which are on the laser • unit bottom plate. For easy release of the laser it is recommended to lift it upright and than pull the laser unit backwards.

Removing the LASER unit

For installation proceed in reverse order.

Risk of instrument damage by ingress of particles.

NOTICE

Check proper seating of all housing parts before use• Do not operate instrument when housing is open or unlocked•

Now take the new laser unit, insert it and make • sure that its base plate is correctly placed into the bolts. Fix the new laser unit with the two screws and • connect the electric plug. Close the housing of the laser unit. This can • easily be done by ﬁrst positioning the slits over the screws. When the instrument and the PC is switched on again and the NIRWare Operator is started, a corresponding message will be displayed and inform you that this change in hardware conﬁguration must be added into the database.

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Resetting the laser lifetime counter After LASER unit replacement the following message appears:

Message concerning required instrument setup

Click the OK icon • to conﬁrm the message. Now click the Service icon • (Operator).

The following dialog opens:

7 Maintenance and repairs

Assembly setup dialog

Click the icon next to the Laser Module row • . The following dialog appears:

Exchange sequence dialog for the laser

Activate the watch icon next to the line • Laser hours of operation .

The following message box is displayed:

Message

Conﬁrm the message by clicking the OK icon • .

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The following screen indicates the laser lifetime counter is set to zero:

Hours of operation of the laser

Now click the Go Back icon • to ﬁnish the procedure.

7.6 Filter pad replacement

7 Maintenance and repairs

When the ﬁlter pads at the rear of the instrument and the measuring cell are dirty, ventilation and thermal stability of the instrument will no longer be ensured. Replace the pad after 6 month of use at the latest. An earlier exchange might be necessary, when the instrument is operated in a dusty environment.

Replacing the ﬁlter pads

Risk of instrument damage by ingress of particles.

Risk of instrument damage by overheating.

To replace the ventilation ﬁlter, proceed as follows:

Remove the ﬁlter cover.• Remove the old ﬁlter pad.• Insert the new ﬁlter pad.• Reinstall the ﬁlter cover.•

NOTICE

Check proper seating of the ﬁlter and ﬁlter bracket before use• Do not operate instrument without ﬁlter•

NOTICE

Do not block the cooling openings of the instrument• Do not operate instrument with a clogged ﬁlter•

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7.7 Main fuse replacement

The primary fuses are located at the rear of the instrument next to the power supply socket. They are accessible from the outside.

To replace the primary fuses, proceed as follows:

7 Maintenance and repairs

Unplug the power cord!• Remove the defective fuses from the holder and replace them • with new fuses of the same rating (T 10 A, L 250 V). Reconnect the power supply connector and switch on the • instrument.

Replacing the primary fuses

7.7.1 Measuring cell fuse replacement

Each measuring cell is provided with two fuses located at the bottom. To replace them, proceed as follows:

Location of the fuses at the bottom of the measuring cell

Remove all add-ons, petri dishes, vials, etc. • from the measuring cell. Remove the measuring cell from the instru-• ment. Turn the cell, in a way that you see the • bottom side. The two black fuse holders are located as indicated by the arrow on the picture to the left. Replace the 2.0 AT fuses with two new ones. •

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7.8 NIRFlex Solids

It is possible that solids or pasty samples are spilled into the sample holder of the NIRFlex Solids. In this case it is recommended to start the cleaning process as soon as possible to prevent any damage of the instrument. Special attention is needed on that point, if aggressive media are spilled over the instrument.

To clean the measuring cell, proceed as follows:

Remove the add-on from the measuring cell.• If some solid residues are left in its sample holder, remove the cell from the instrument and turn it, • so that the residues fall off. If some pasty residues are left in the sample holder, remove them with a soft tissue and clean the • sample holder with a non-aggressive liquid (water or alcohol).

Special attention is needed to prevent the glass window from getting any scratches by using optical tissues.

7.9 NIRFlex Liquids

7 Maintenance and repairs

To clean the measuring cell, proceed as follows:

Take the measuring cell out of the basic instrument.• Remove the cuvettes that might still be in the openings.• Remove the sample holder from the measuring cell by loosening the screws in sample position 1, 3 • and 5. Clean the sample holder and the corresponding opening of the measuring cell. Make sure that • there are no residuals of sample anymore. Place the sample holder back into the measuring cell and retighten the three screws.•

CAUTION

Minor or medium burns by hot surfaces

Let the cell chambers cool down sufﬁciently ﬁrst• Do not touch hot cell chambers or cuvettes•

NIRFlex Liquids measurement cell

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7.10 Customer service

Only authorised service personnel is allowed to perform repair work at the instrument. These persons have a comprehensive technical training and knowledge of possible dangers which might arise from the instrument. Addresses of ofﬁcial Buchi customer service ofﬁces are given on the Buchi website under: www.buchi.com. If malfunctions occur at your instrument or you have technical questions or application problems, contact one of these ofﬁces.

The customer service offers the following:

Spare part delivery• Repairs• Technical advice•

7 Maintenance and repairs

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8 Storage, transport and disposal

This section instructs how to handle the instrument for storage or transport, and gives advice on disposal.

8 Storage, transport and disposal

Risk of instrument damage at storage and transport

Engage the transportation lock before storing, transport and re-packaging• Only store and transport the instrument in original packaging• Keep shocks and vibrations away • Safely store and transport accessories separately•

8.1 Storage and transport

The NIRFlex N-500 is equipped with a mechanical transportation lock to avoid damage of the interferometer during transportation and shipping by shocks and vibrations. For storage and transportation, the transportation lock must be in “Locked” position. Manual handling of the instrument requires a second person!

NOTE

Because of its weight it is recommended to carry the instrument with two persons.•

• Clean the instrument thoroughly before storage or transport. When returning the instrument to BUCHI ﬁll out a copy of the „Health and Safety Clearance“ form • and safely attach it at the outside of the transport box.

NOTICE

8.2 Disposal

For instrument disposal in an environmentally friendly manner, a list of materials is given in section 3.1. This helps to ensure that the components can be separated and recycled correctly by a specialist for disposal.

You have to follow valid regional and local laws concerning disposal. For help, please contact your local authorities!

NOTE

When returning the instrument to the manufacturer for repair work, please copy and complete the health and safety clearance form on the following page and enclose it with the instrument.

CAUTION

Risk of poisoning by improper decomposing and recycling of the device

Do not dispose of the device as unsorted household waste• Recycle all materials according to local directives and laws •

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8 Storage, transport and disposal

Health and Safety Clearance

Health and Safety Clearance_20081110.doc_20081110 Version 1.0 Page 1/1

Declaration concerning safety, potential hazards and safe disposal of waste.

For the safety and health of our staff, laws and regulations regarding the handling of dangerous goods, occupational health and safety regulations, safety at work laws and regulations regarding safe disposal of waste, e.g. chemical waste, chemical residue or solvent, require that this form must be duly completed and signed when equipment or defective parts were delivered to our premises.

Instruments or parts will not be accepted if this declaration is not present.

Equipment

Model: Part/Instrument no.:

1.A Declaration for non dangerous goods

We assure that the returned equipment

has not been used in the laboratory and is new was not in contact with toxic, corrosive, biologically active, explosive, radioactive or

other dangerous matters.

is free of contamination. The solvents or residues of pumped media have been

drained.

1.B Declaration for dangerous goods

List of dangerous substances in contact with the equipment:

Chemical, substance Danger classification

We assure for the returned equipment that

all substances, toxic, corrosive, biologically active, explosive, radioactive or

dangerous in any way which have pumped or been in contact with the equipment are listed above.

the equipment has been cleaned, decontaminated, sterilized inside and outside and

all inlet and outlet ports of the equipment have been sealed.

2. Final Declaration

We hereby declare that

- we know all about the substances which have been in contact with the equipment and all questions have been answered correctly

- we have taken all measures to prevent any potential risks with the delivered equipment.

Company name or stamp:

Place, date:

Name (print), job title (print):

Signature:

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9 Spare parts and accessories

This section lists spare parts, accessories and options of the instrument including their ordering information. Order the spare parts from Buchi. Always state the product designation and the order number when ordering spare parts. Use only genuine consumables and genuine spare parts for maintenance and repair to assure good system performance and reliability. Any modiﬁcations to the spare parts used is allowed only with the prior written permission of the manufacturer.

CAUTION

Risk of device damage and dangerous system status by unauthorized spare parts

Only use original spare parts•

9 Spare parts

9.1 Scope of delivery

9.1.1 Interferometer

Interferometer

Product Order number

NIRFlex N-500 Polarization Interferometer 100-230 V, 50/60 Hz

N505-000

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9.1.2 Measuring cells

9 Spare parts

NIRFlex Solids

Product Order number

For measurements in diffuse reﬂection

N510-000

mode with rotating sample desk

Petri dish add-on N510-001

Vial add-on N510-002

XL add-on N510-003

Tablet add-on N510-004

XL add-on with iris aperture N510-005

XL add-on accepting B+L sample cups N510-006

Spinner add-on N510-012

Flow-cell adapter add-on N510-013

NIRFlex Solids Transmittance

Product Order number

For measurements in diffuse transmission

N514-000

mode with rotating sample plates

Sample plate for 30 tablets with a

N514-002

diameter of 4 - 12 mm

Sample plate for 10 tablets with a

N514-001

diameter of 12 - 30 mm

Sample plate for 10 tablets with iris

N514-003

apertures

Table 3-4: NIRFlex Liquids

Product Order number

For measurements in transmission mode

N511-000

using cuvettes

83 NIRFlex N-500 Operation Manual, Version F

9 Spare parts

N IR S o ft war e Sui te

N IR War e + NI RCal

NIRFlex Fiber Optic Solids

Product Order number

For measurements in diffuse reﬂection

2 m ﬁber length N512-000

3 m ﬁber length N512-004

5 m ﬁber length N512-005

NIRFlex Fiber Optic Liquids

Product Order number

For measurements in transmission mode

N513-000 using a ﬁber optic probe (default length 2 m, custom-made lengths up to 7 m available)

NIRFlex Fiber Optic SMA

Product Order number

For measurements in transmission or

N515-000 diffuse reﬂection mode. External optical probes or and measuring cells can be connected through ﬁber optic via SMAconnector

Monoﬁber without SMA connectors, 1m A515-020

SMA connectors with tailoring A515-021

Transmission immersion probe A510-020

Transmission ﬂow cell A510-010

9.1.3 Software

Software

Product Order number

NIRWare Basic N550-011

NIRWare Advanced N550-013

NIRCal N550-021

84 NIRFlex N-500 Operation Manual, Version F

9.1.4 Standard accessories

Example

93124

NIRWare

Quick Guide

9 Spare parts

Standard accessories

Product Order number

1 Power supply cable

Type CH 10010

Type Schuko 10016

Type GB 17835

Type USA 10020

Type AUS 17836

1 Ethernet connection cable NIRFlex

48457

N-500/PC

Operation Manual NIRFlex N-500

English 93020

German 93019

French 93021

Italian 93022

Spanish 93023

Quick Guide NIRWare 1.2

English 93124

German 93125

French 93126

Italian 93127

Quick Guide NIRWare 1.4

English 11593434

German 11593435

French 11593436

Italian 11593437

Spanish 11593438

Chinese 11593439

Japanese 11593440

Quick Guide NIRCal 5.2 with Toolbox

English 93119

German 93120

French 93121

Italian 93122

Quick Guide NIRCal 5.4 with Toolbox

English 11593441

German 11593442

French 11593443

Italian 11593444

Spanish 11593445

Chinese 11593446

Japanese 11593447

85 NIRFlex N-500 Operation Manual, Version F

9.1.5 Optional accessories

9 Spare parts

Optional accessories

Product Order number

Set of 2 quartz glass cuvettes with 2 mm pathlength for NIRFlex Liquids

1 spacer for 5 mm cuvettes

1 spacer for 2 mm cuvettes

1 spacer for 1 mm cuvettes

Set of spacers (6 pieces of each)

Set of 100 glass vials to be used with NIRFlex Solids with the vial add-on

46266

45430

45431

45432

N560-013

N560-015

Vial adapter for NIRFlex Liquids with a diameter of 8 mm, including 100 vials

Set of 10 glass petri dishes (inner diameter 100 mm) for NIRFlex Solids with the petri dish add-on

N511-001

41583

86 NIRFlex N-500 Operation Manual, Version F

9 Spare parts

Optional accessories (cont.)

Product Order number

Transﬂectance cover or high performance cup using 100 mm petri dishes

XL add-on for NIRFlex Solids with iris aperture

XL add-on for NIRFlex Solids accepting B+L cups

High performance sample cup for NIRFlex Solids

Exchange glass bottom 46246

41636

N510-005

N510-006

46259

Transﬂectance adapter for NIRFlex Fiber Optic Solids

The transﬂectance adapter is supplied in a plastic box containing the following parts:

a Adjustment ring

b Spacer rings for pathlength 0.5 mm,

1 mm and 1.5 mm

c 3 knurled screws

d 1 mm spacer disk

e Allen key

f Transﬂectance sleeve

N512-001

87 NIRFlex N-500 Operation Manual, Version F

9 Spare parts

Optional accessories (cont.)

Product Order number

Holder for ﬁber optic probe 46273

Barcode reader 42762

Special Vials, set of 6 11056492

Unbreakable Sample Cup for NIRFlex

11055058

Solids

Transﬂectance cover for Unbreakable Cup 11055998

Spinner add-on 11055087

Transﬂectance cover for Hellma cuvettes 11056376

88 NIRFlex N-500 Operation Manual, Version F

9 Spare parts

Optional accessories (cont.)

Product Order number

Stamp for Hellma cuvettes 11056459

Flow add-on 11055051

Flow Through cuvettes 11055911

9.2 NIRFlex spectrometer

Spare parts NIRFlex spectrometer

Product Order number

Primary lamp module N560-001

Laser unit N560-002

Fuse (T 10 A slow blow, L 250 V) 02009

Filter cover and ﬁlter pad N560-004

1 Ethernet connection cable NIRFlex N-500/PC 48457

Power supply cable 33748

10 ﬁlter pads 42779

89 NIRFlex N-500 Operation Manual, Version F

9.3 NIRFlex Solids

Spare parts NIRFlex Solids

Product Order number

Fuse 2.0 AT 02998

External Reference N560-003

Vial add-on N510-002

XL add-on N510-003

Petri dish add-on N510-001

Tablet add-on N510-004

Spinner add-on N510-012

Flow-cell adapter add-on N510-013

Set of 10 glass petri dishes, 10 mm 41583

Set of 100 glass vials for vial add-on N560-015

10 ﬁlter pads 42778

XL add-on with iris aperture N510-005

XL add-on accepting B+L sample cup N510-006

High performance sample cup 046259

Exchange glass bottom for high performance sample cup 046246

Transﬂectance cover 041636

Set of 6 special vials for Vial add-on 11056492

Unbreakable sample cup 11055058

Transﬂectance cover for Unbreakable sample cup 11055998

Spinner add-on 11055087

Transﬂectance cover for Hellma cuvette 11056376

Flow cell add-on 11055051

Flow-through cuvette 11055911

9 Spare parts

90 NIRFlex N-500 Operation Manual, Version F

9.4 NIRFlex Solids Transmittance

Spare parts NIRFlex Solids Transmittance

Product Order number

Fuse 2.0 AT 02998

10 ﬁlter pads 42778

Window, complete 48961

Tweezers 48959

Cover for NIRFlex Solids Transmittance 48955

9.5 NIRFlex Liquids

Spare parts NIRFlex Liquids

Product Order number

Fuse 2.0 AT 02998

Cuvette holder complete N560-010

Set of 2 quartz glass cuvettes, 2 mm 46266

1 spacer for 5 mm cuvettes 45430

1 spacer for 2 mm cuvettes 45431

1 spacer for 1 mm cuvettes 45432

10 ﬁlter pads 42778

Vial adapter for 8 mm vials including 100 vials N511-001

9 Spare parts

9.6 NIRFlex Fiber Optic Liquids

Spare parts NIRFlex Fiber Optic Liquids

Product Order number

Fuse 2.0 AT 02998

10 ﬁlter pads 42778

9.7 NIRFlex Fiber Optic Solids

Spare parts Fiber Optic Solids

Product Order number

Fuse 2.0 AT 02998

Sample probe head 48400

10 ﬁlter pads 42778

91 NIRFlex N-500 Operation Manual, Version F

9.8 NIRFlex Fiber Optic SMA

Spare parts Fiber Optic Solids

Product Order number

Fuse 2.0 AT 02998

10 ﬁlter pads 42778

Packing parts SMA 11056060

9.9 Transﬂectance adapter

Spare parts transﬂectance adatper

Product Order number

Spacer ring 0.5 mm 48994

Spacer ring 1 mm 48995

Spacer ring 1.5 mm 48996

Knurled screw 44311

9 Spare parts

92 NIRFlex N-500 Operation Manual, Version F

10 Declarations and requirements

10.1 FCC requirements (for USA and Canada)

English: This equipment has been tested and found to comply with the limits for a Class A digital device,

pursuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment. This equipment generates, uses and can radiate radio frequency energy and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio communications. Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at his own expense.

Français: Cet appareil a été testé et s'est avéré conforme aux limites prévues pour les appareils numériques

de classe A et à la partie 15 des réglementations FCC ainsi qu’à la réglementation des interférences radio du Canadian Department of Communications. Ces limites sont destinées à fournir une protection adéquate contre les interférences néfastes lorsque l’appareil est utilisé dans un environnement commercial. Cet appareil génère, utilise et peut irradier une énergie à fréquence radioélectrique, il est en outre susceptible d’engendrer des interférences avec les communications radio, s’il n’est pas installé et utilisé conformément aux instructions du mode d’emploi. L’utilisation de cet appareil dans les zones résidentielles peut causer des interférences néfastes, auquel cas l’exploitant sera amené à prendre les dispositions utiles pour palier aux interférences à ses propres frais.

10 Declarations and requirements

93 NIRFlex N-500 Operation Manual, Version F

10.2 Declaration of conformity

10 Declarations and requirements

94 NIRFlex N-500 Operation Manual, Version F

BÜCHI Labortechnik AG CH-9230 T +41 71 394 63 63 F +41 71 394 65 65

Flawil 1 / Switzerland

www.buchi.com Quality in your hands

BUCHI N-500 User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual