Metrohm NIRS Analyzer PRO User Manual

NIRS
Analyzer PRO

Manual

8.928.8004EN

Metrohm AG
CH-9100 Herisau
Switzerland
Phone [phone]
Fax [phone]

[e-mail]
www.metrohm.com

NIRS
Analyzer PRO

Manual

8.928.8004EN 03.2013 fpe

Teachware
Metrohm AG
CH-9100 Herisau

[e-mail]

This documentation is protected by copyright. All rights reserved.

Although all the information given in this documentation has been checked with great care, errors
cannot be entirely excluded. Should you notice any mistakes please send us your comments using the
address given above.

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Change Control

Version

Date

Summary of Changes

1.0

Dec. 2,
2012

Document first release, initiated change control

Change control on this document is as follows:

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Table of contents

1 Introduction ................................................................................................................... 5

1.1 Information Disclaimer ................................................................................. 7

2 Hardware Familiarization .............................................................................................. 8

2.1 Lamp Housing .............................................................................................. 8

2.2 Optical Switch .............................................................................................. 8

2.3 Diode Array Spectrometer ............................................................................ 9

3 Specifications............................................................................................................... 11

3.1 Window Reflectance .................................................................................. 12

3.2 MicroBundle Fiber Optic Interface .............................................................. 12

3.3 Direct Light ................................................................................................ 13

4 Mounting Information ................................................................................................. 14

4.1 4.1 Mounting Frame, U-Bolts Secured to Mounting Flanges ...................... 14

4.2 Mounting by straps to blind plates ............................................................ 19

4.3 Weld Flange ............................................................................................... 20

5 Mounting Dimensions .................................................................................................. 22

6 Electrical Connection ................................................................................................... 23

7 Air Cooling Connection Kit........................................................................................... 30

8 Air Purge Connection (Used with “Spoon Probe”) ....................................................... 32

9 Fiber Optic Probe Mounting ........................................................................................ 34

10 Ethernet Connection .................................................................................. 35

11 Safety and Power-up .................................................................................. 37

12 Connection to Vision Software ................................................................... 38

13 Diagnostics ................................................................................................. 43

13.1 Window Reflection ..................................................................................... 43

13.1.1 Performance Test ................................................................................................. 43

13.1.2 Reference Standardization .................................................................................... 46

13.1.3 Wavelength Certification ...................................................................................... 50

13.2 MicroBundle Fiber Optic Sensing ............................................................... 52

13.2.1 Performance Test ................................................................................................. 52

13.2.2 Reference Standardization .................................................................................... 55

13.2.3 Wavelength Certification ...................................................................................... 59

13.3 Direct Light Sampling ................................................................................. 60

13.3.1 Performance Test ................................................................................................. 61

13.3.2 Reference Standardization (External Reference Correction) .................................... 64

14 Sampling .................................................................................................... 65

15 Standards and Approvals ........................................................................... 66

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1 Introduction

Analyzer PRO is a rugged, compact Near-Infrared Process

Instrument, designed for the wavelength range from 1100-1650
nanometers. This is an excellent region for process analysis,
containing many second and third overtones of molecular
vibrations which can be measured.

The instrument is based upon high-resolution diode array
technology. The InGaAs diode array, with spectral dispersion of

1.1 nm/pixel, is a stable, intrinsically accurate method of NIR
absorbance measurement. It offers excellent peak shape
resolution, and contains no moving parts. Therefore, no
wavelength accuracy adjustment is needed, as there is no
measurable drift.

Sampling systems are as follows:

• Window Reflectance, where the sample passes in contact with the window on the side of the
instrument

• Reflectance Probe, using a 1” (25.4mm) diameter stainless steel probe

• Direct Light Reflectance, where the sample passes at a distance of 4-10 inches

(approximately 100-250mm) from the window

The analyzer is housed in a robust cabinet, designed for easy, reliable mounting at the desired
location in the production area. Mounting is simplified by use of industry-standard stainless steel
clamps, which facilitate installation and removal, as well as good positioning of the analyzer to the
sample.

The instrument may be mounted in any orientation, as long as the sample window is in the proper
location. The sample interface is normally placed at a point of production where the product is
pumped through a pipe, dryer, blender, or other feed mechanism. There should be no (or very few)
gaps or voids in the product flow, as these will cause measurement instability.

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The Analyzer PRO vides non-destructive analysis of

chemical and pharmaceutical products directly in
the process line, without use of a bypass loop.
Because most materials can be measured directly,
with no need for sample dilution or preparation,
the material can be measured as produced, with
no loss of end product.

Operation of the Analyzer PRO is through
Metrohm Vision™ software, which is robust,
powerful, and easy to use. This validated software
package meets all 21 CFR Part 11 requirements,
and comes with a test script to prove compliance
for internal regulatory personnel. Combined with
normal customer procedures for network and user
access, all 21 CFR Part 11 requirements are met.

Vision provides excellent tools by which to develop an analytical model for sample prediction. The
NIR sample information is correlated with quantitative lab data from the primary analysis method,
and a predictive model is used to report values for ongoing sample analysis.

Communication between instrument and computer is by Ethernet line, using standard connectors.
Commands use a proprietary, encrypted language which is not susceptible to hacking, support of
viruses, or other means of hacking. Only authorized operators may communicate with the Analyzer
PRO instrument, and only by valid entry through Vision.

Measurements may be displayed in a control room area on the computer screen as they are reported
in the Routine Analysis section of Vision. Provision is made for digital electronic transfer to most
supported plant controller languages.

Use of the Analyzer PRO helps to optimize the use of raw materials by ongoing measurement in real
time. This permits adjustment and correction of the process to target values, eliminating or
minimizing waste product. The Analyzer PRO fits into Process Analytical Technology (PAT) planning,
in support of recent FDA process initiatives.

Precise instrument matching enhances method development, minimizes implementation efforts, and
ensures straightforward calibration model transferability between analyzers.

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1.1 Information Disclaimer

This manual and the information herein are correct as of the time of publication, based upon the best
information available at the time. Configuration, options, and software information may change over
time, in keeping with the corporate philosophy of continuous improvement.

Metrohm NIRSystems and its distributors cannot be liable for changes to the customer process based
upon information contained in this manual which is subject to revision and update. Additionally, the
information and steps in this manual are not meant to serve as template standard operating
procedures for use in regulation industries. Customers should supply their own procedures for
internal users, based upon the specific samples, methods, and needs of the application.

Metrohm offers optional training and field support to assist in the technical aspects of calibration and
library development. The final responsibility lies with the user, who has access to calibration samples,
lab data, and other information required to build and maintain methods using this instrument.

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2 Hardware Familiarization

Analyzer PRO is built into a rugged, sealed stainless steel housing which is designed to withstand the
harsh production environment, including washdown.

Fiber optics are used with the Reflectance Probe design, and should always be protected from
damage and abuse. In particular, fiber bend radius should never be less than 6” (150mm). It is
strongly recommended that fibers be mounted in enclosed cable trays to minimize handling,
movement, and possible accidents.

The inside view of the instrument is as shown.

Primary components are as follows:

2.1 Lamp Housing

This contains two halogen lamps. Only one lamp is active at a time. If a lamp fails, the other is
automatically switched on, and a motor moves the Sample Illumination or “light-output” fiber to the
operating lamp. The Sample Illumination Fiber carries the light energy to the sampling point.
Note that the Lamp Housing also has a Reference Fiber for each lamp, which are routed to the
optical switch. These fibers are used to measure the background (reference) energy for each lamp.
The Optical Switch automatically moves to the correct position, based upon which lamp is in use.

2.2 Optical Switch

The Optical Switch receives the light reflected back from the sample, which has been modified by
interaction with the sample material. The other inputs to the Optical Switch are the two Reference
fibers from Lamps #1 and #2, along with a “Dark Signal” reference. The Optical Switch, under control
of the on-board electronics, measures the energy returning from the sample, compares this with the
energy level sent to the sample, and scales the signal to create an absorbance spectrum over the

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wavelength range from 1100-1650 nm. (The optical switch may be heard moving when instrument

The diode-array spectrometer is composed of 512

scans are taken, if the ambient noise level is low enough.)

2.3 Diode Array Spectrometer

discrete InGAs detector diodes. It has no moving
parts.

The wavelength accuracy is intrinsically stable, and
requires no adjustment. Temperature is maintained
internally to assure consistent and accurate
response.

NOTE: There are no user-serviceable parts in the
Diode Array Assembly. Do not attempt to open,
disassemble, or service this unit. Any attempt at
service or opening will immediately void the
warranty.

Power Supply

This takes the incoming AC Mains voltage and steps it down to 24 VDC, as used by the instrument.

Cooling Fan

The fan circulates air internally to maintain consistent, controlled temperature to the spectrometer
and all internal components. This assures repeatable optical response.

Sampling Point

This may be either a Window Reflectance system (as shown here), a Fiber Optic Probe, or Direct
Light. The internal instrument interface is the same for all styles. A fiber optic bundle carries the light
to the sample. A small bundle carries the returning energy from the sample to the Optical Switch.

AC Mains Block

This is explained in the section on electrical Connection. All connections should be made in
compliance with local codes, by a qualified electrician. Always use safety lockout procedures when
performing electrical wiring.

Ethernet RJ-45 Connector

The Ethernet cable is plugged in on the instrument motherboard.

Control PCB

Instrument functions are controlled from this PC board. There are no user-serviceable items or
procedures in connection with this board.

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The internal light paths of the Analyzer PRO are

Block Diagram

shown.

The sample is illuminated with white light. The
resulting signal is sent back (through the optical
switch) to the Diode Array Spectrometer for
analysis.

Both dark and light reference signals are used to
set the scale of absorbance. Vision uses the
resulting information to produce sample spectra.
The formula (shown only for information) is as
follows:

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3 Specifications

Overall Analyzer PRO instrument specifications are as follows:

Item Specification

Ambient Temperature

Ambient Humidity 10-90% Relative Humidity, non-condensing

Electrical Supply 100-240 VAC, 50-60 Hz, 2.0 A, 150 W

Protection IP69k according to IEC 60529 and DIN 40050 part 9, NT ELEC 023

Dimensions

Weight 33.0 pounds (15 Kg)

Pressurized Air Cooling
(Ambient Temperature 45­65 Degrees C)

Pressurized Air – Spoon
Probe

Network Connections Local Area Network (LAN) – Ethernet, RJ-45 connection

23 to 104° F (-5 to 40° C)
With Air Cooling: 23 to 149° F (-5 to 65° C)

Width: 17.0” (42 cm)
Height: 17.0” (42 cm)
Depth: 5.0” (13 cm)

Cooling air flow rate minimum 5 Liters/min
>99.9% water free
>99.9% free of oil and fine particles down to 0.3 micrometers

Purge air: 3-5 bar

Sample Temperature,
Reflectance Window

Sample Temperature,
Spoon Probe

Computer Requirements See Vision computer requirements

Wavelength Range 1100-1650 nm

Analysis Time:

Wavelength Accuracy 0.5 nm

Wavelength Precision < 0.02 nm

Wavelength Stability < 0.01 nm/°C

Specifications for each type of sample interface follow:

302 degrees F (150° C)

248 degrees F (120° C)

5 – 50 ms / integration time; depends upon sample. Typical result
time: 3-15 sec.

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3.1 Window Reflectance

In-line analysis of paste, granulates, slurry, powdered products and similar materials in pipes or fluid
transport systems can be performed without need for bypass streams. The sample material must pass
over the sample interface window.

The window reflection interface may easily be installed into the production line using standard GEA
Tuchenhagen flowcell mountings, or by welding an interface flange into the wall of the
pipe/transport system. GEA Tuchenhagen is well known for innovative, hygienic components for
operation in the process stream.

• Temperature: 150°C (302°F)

• Pressure: Vacuum > 1 Torr (approximately 1 mm Hg), Pressure < 3000 PSI

• Lens: Sapphire; diameter 45 mm (1.8”), thickness 12 mm (0.5”), with

EPDM O-ring seal for reliable, temperature resistant sealing

• Pipe flowcells: Fits directly into GEA Tuchenhagen Varinline Access units (DN40 to
DN150 with 68 mm [2.7”] opening). This mounting method facilitates
implementation of CIP (clean in place) and SIP (sterilize in place) methods.

• Transport System: Stainless steel welding flange

3.2 MicroBundle Fiber Optic Interface

Direct in-line measurement with microbundle fiber optic probe interface, optimized for process
streams of clear to opaque liquids, slurries, suspensions, and powders. The analyzer may be
configured with a reflectance or immersion probe based upon sample type.

316 Stainless Steel or Hastalloy Probes (custom materials also available)

• Micro Interactance Reflectance Probe

• Micro Interactance Immersion Probe

• Micro Interactance Reflectance with purge on collection tip

(requires clean air or nitrogen for purge)

• Optimized Micro Reflectance (45-degree) Probe with 3 meters of fiber
(Angled face for optimized sample collection)

Window: Sapphire

Temperature: 300°C (572°F)

Pressure: 5000 PSI (344 Bar)

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Diameter: 1” (25.4 mm) Standard

Length: 12” (305 mm) Standard

Installation: 1” Swagelok® crimp fitting

Cleaning: Wash in water, hot or cold depending upon product

Fiber: Interactance Micro Fiber Optic Bundle (3m) with Metal or Nylon Cladding,

SMA connection to the Analyzer PRO

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3.3 Direct Light

In-line analysis of products where direct contact with the product is not technically feasible, such as
product transported on a conveyor belt or similar means of movement.

Lens: Sapphire; diameter 45 mm (1.8”), thickness 12 mm (0.5”), with EPDM O-ring

seal for reliable, temperature resistant sealing

Distance: 100-250 mm to sample surface (4 to 10”)

Scanning Area: 20 - 85 mm (0.8 to 3.3”) diameter, depending upon distance to sample

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4 Mounting Information

Analyzer PRO is provided with an innovative, rugged integral flange-mounting system that permits
easy installation and service. There are two mounting flanges, top and bottom, to which are
mounted “blind plates” using a rugged, industry-standard tri-clamping mechanism. This approach
eliminates bolt holes or other entry points for contaminants.

The mounting flanges are sized to attach directly to 3” (76.2 mm) diameter stainless steel piping,
which is widely used in sanitary installation areas. To mount using pipe, determine where the window
or fiber will be positioned, and install pipes in the corresponding positions for supporting and
mounting the enclosure. The pipes should have the proper flange ends to accept the clamps to lock
the Analyzer PRO instrument in place.

Two alternative methods are shown. This first is preferred in most cases.

4.1 4.1 Mounting Frame, U-Bolts Secured to Mounting Flanges

Many installations will be performed using a fabricated mounting frame which can be bolted to a
solid surface in the plant. This mounting method should be well-planned, so the sample window (or
fiber optic probe) is in the right location upon final installation. In this case a Analyzer PRO Fiber Optic
Probe system is being installed.

This sequence shows mounting the frame to the Analyzer PRO instrument first, then bolting the
frame (with Analyzer PRO installed) to the mounting bolts.

We advise using a cart or frame to support the instrument during mounting, to avoid damage. Use
lab jacks as shown, to make height adjustment easy. Protect the fiber optic cable, as well as the
power and communications cables. Do not kink, bend, or otherwise stress the fiber optic cable in any
way, as this may damage the internal fibers and cause loss of energy.

Safety NOTE: Please follow all site safety rules regarding lifting and physical exertion while mounting
the Analyzer PRO.

In addition, use of a rolling cart provides an easy way to protect the fiber optic cable, power cable,
and communications cable – they are carefully coiled on the lower shelf of the cart, to avoid damage.

1. Remove the locking clamps and blind
mounting plate from each mounting
flange. Remove the gasket as well.

Keep all these parts in a safe place, in
case they are needed at some point in
the future.

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2. Fabricate the mounting frame as

shown. It may be larger if required. In

Note that the Analyzer PRO instrument is on a cart for positioning. We use lab jacks to

3. Use 3” (76.2 mm) inside-diameter

this installation we purchased pre-cut
channel from McMaster Carr. We used
four (4) lengths of Steel Strut Channel,
Slotted, 1-5/8” x 1-5/8”, zinc-plated, 2
foot length, part number 3310T53.

The brackets each measure 24” (610
mm) in length. The upright brackets
are bolted so the centerline of the
slotted holes is 17.25” (about 439 mm)
apart. Use 3/8” (or 10mm) bolts.

The brackets should be capable of
supporting the full Analyzer PRO
weight, plus an ample safety margin.
We suggest a minimum capacity be
100 pounds, or roughly 45 kilograms.

raise it to the final mounting height, to avoid difficult lifting. The installer is shown
checking the size and slot pattern for fit.

stainless U-Bolts with extended-length
legs, like that shown.

(This is a McMaster-Carr Extended­Length Type 316 SS U-Bolt 3/8”-16
Thread, part number 29605T7 -- as of
time of publication.)

Remove the nuts from the U-Bolt and
gently place it over the flange as
shown. Verify that the mounting
height is correct, and that the U-Bolt
will be in the correct position to bolt
onto the brackets. Use additional
wooden blocks to reach the proper
mounting height. Check both sides.

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4. Adjust height with the lab jacks, so the

5. When the height is correct, push the

U-Bolts align properly with the frame
slots. Adjust each side equally, to keep
the Analyzer PRO aligned with the
bracket.

U-Bolt through the slots.

Do this on both sides of the Analyzer
PRO instrument, in preparation for
securing with washers and nuts.

6. Install large washers, lock washers,
and nuts on the ends of the U-Bolts.
Do not tighten until all four sets of
washers and nuts are in place.

When all four sets of hardware are in
place, gently tighten each nut, using
care not to distort the U-Bolts or
frame.

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If preferred, nylon-insert locking nuts
may be used in place of normal lock
washers and hex nuts.

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7. The Analyzer PRO instrument is now

securely mounted to the fabricated

8. Mounting studs should be placed in

9. Roll the cart so the mounting frame is

frame. It is ready to be mounted to the
final process location.

Verify that all hardware is secure.
Protect the fiber (if so equipped) as
well as the power and
communications cables.

Carefully move the Analyzer PRO
instrument and mounting frame to the
final location.

the correct positions to hold the frame
in place.

We installed 3/8” studs in the
mounting area as shown. These are

21.75” (552mm ) apart, which
corresponds with the slot holes in our
mounting frame. The lower studs are
mounted 22” (560mm) below, at the
same width.

These studs should be capable of
supporting the weight of the Analyzer
PRO instrument and frame, with a
large margin of safety. Be sure to
measure for the frame used, and

directly in front of the mounting studs.

Using the lab jacks, raise the Analyzer
PRO instrument (on the mounting
frame as shown) to the correct
position. When the studs align with
the mounting frame, gently ease the
mounting frame over the studs as
shown.

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10. Install a large washer, a lock washer,

11. When all four sets of washers and nuts

12. When all hardware is tight, the lab

and a hex nut onto each stud.

Do not tighten until all four sets of
hardware are in place.

Continue to protect the fiber optic
cable, as shown here.

are threaded on, begin tightening each
set. Do not damage or distort the
mounting frame.

If nylon-insert nuts are preferred, those
may be used in place of standard hex
nuts.

jacks may be lowered and removed.
This may be done gently, to verify that
the mountings support the weight,
and that all hardware is properly
tightened.

This photo shows the final mounting,
with all bolts installed and tightened.

As before, continue to protect the
fiber optic cable, as well as the power
and communications cables. The cart is
still shown at the bottom of this
photo, immediately after removing lab
jacks. The cables are on the bottom
shelf, ready for the next stages of
installation.

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4.2 Mounting by straps to blind plates

The blind plates are 15mm stainless steel,

The mounting flange of the instrument is shown at

and are equipped with a special gasket to
properly affix the blind plate to the flange on
the instrument.

The blind plates may be welded or machined
in any way to properly affix and support the
instrument in the desired position.

Do not distort or weaken the blind plates, as
they support the full weight of the Analyzer
PRO. Weight is 33 pounds, or 15 Kg.

the top.

The “blind plate” and gasket are shown at right.

The clamp is a “Tri-Clover” style. It is an ISO Clamp,

76.1mm. This style of clamp is used in sanitary

installations, and is known for ruggedness as well as
ease of installation and removal.

Do not attempt to drill mounting holes through the
cabinet or cover, as this will compromise the
protective sealing of the instrument enclosure. Any
holes drilled in the cabinet will invalidate the
instrument warranty.

Before mounting, determine the optimal desired position of the sampling window, and arrange for
the blind plate positions to correspond to that desired sampling position. (With a fiber optic probe
this position may be less critical.)

Before mounting the instrument, verify that the blind plates are in the correct locations, and that the
fabricated mounting arrangement will support the full weight of the instrument. When mounted, the
distance from the outside flat of the top blind plate, to the outside flat of the bottom blind plate is

19.25” (384mm). Leave some provision for movement of the mounting brackets (such as slotted

holes) to ease mounting and final positioning. At least ¼” (6mm) of movement is recommended. The
gaskets have a molded ridge on each surface, and the mounting must accommodate this ridge
during assembly.

The blind plate, gasket, and mounting flange should be securely clamped in place, top and bottom.
There should be no play in the clamp or mounting mechanism. This method of mounting provides for
easy mounting and dismounting, if required. The cover, secured by 32 bolts and sealed by a
compressive gasket, has two handles which allow lifting. Please wear protective gloves when lifting.

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