Metrohm NIRS XDS Interactance OptiProbe Analyzer User Manual

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Summary of Contents

Page 1 - Analyzer

NIRS XDS Interactance OptiProbe Analyzer Manual 8.921.8006EN / 2013-12-16

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8 ▪▪▪▪▪▪▪ instrument detects network capability and optimizes communication speed. The computer that operates the instrument must have clear access t

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▪▪▪▪▪▪▪ 9 3 Instrument Connection The XDS instrument may be connected to the host computer in one of two ways: If the XDS Instrument will be used as

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10 ▪▪▪▪▪▪▪ • The XDS instrument appears just like a network printer (or other peripheral device) on the LAN system. It generates no signals, and onl

Page 5 - Table of contents

▪▪▪▪▪▪▪ 11 3. Upon being powered up on a LAN, the XDS instrument requests a “dynamic” IP address from the DHCP server which controls the LAN. This I

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12 ▪▪▪▪▪▪▪ • Enter Control Panel, Security Center. • On the “General” Tab, be sure that “exceptions” are allowed. (Un-click “Don’t allow exception

Page 7 - 1 Introduction

▪▪▪▪▪▪▪ 13 LAN: A local area network (LAN) is a computer network covering a small physical area, like a home, office, or small group of buildings, su

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14 ▪▪▪▪▪▪▪ 2. Highlight “NIRSystems XDS-series Instrument Driver” as shown, then click on “Configure”. Information: At this point, Vision requests a

Page 9 - 2 Site Readiness

▪▪▪▪▪▪▪ 15 1. Vision cannot see any instrument on the connection path. Click on the “down arrow” at the right side of the empty field to see if inst

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16 ▪▪▪▪▪▪▪ • Click on Start, then Control Panel • Double-click on Network Connections • Double-click on Local Area Connection • Click on Local Ar

Page 11 - 3 Instrument Connection

▪▪▪▪▪▪▪ 17 Network Solution 2: Returning to the Local Area Connection Status dialog box, note these items for the computer: • Address Type: (should

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18 ▪▪▪▪▪▪▪ Network Solution 4: Verify that the Firewall on the computer has Vision loaded as an “exception”. This is located under “Control Panel”,

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▪▪▪▪▪▪▪ 19 assistance with these issues. First, verify the following: • The instrument is free-standing not connected to a network with DHCP server

Page 15 - 3.2.5 Connection in Vision

20 ▪▪▪▪▪▪▪ 4 Assembly of the Instrument The XDS Analyzer will be assembled and installed by a trained representative of Metrohm. This person will pe

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▪▪▪▪▪▪▪ 21 1. Load Vision Spectral Analysis Software onto the computer designated to operate the XDS instrument. 2. Place the monochromator on the

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22 ▪▪▪▪▪▪▪ 5. Insert the AC power cable into the AC power block as shown. 6. Attach the RJ-45 cable to the network connector on the instrument. If

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▪▪▪▪▪▪▪ 23 9. Lift the release handle on the monochromator and engage the module “catches” to the locking togs on the monochromator. (Module not sho

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24 ▪▪▪▪▪▪▪ 13. Install the ferrite onto the RJ-45 cable as shown. This is detailed in the sheet attached to the ferrite. This ferrite is required fo

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▪▪▪▪▪▪▪ 25 5 OptiProbe Module The XDS™ OptiProbe Analyzer is designed for sampling of many types of customer samples. This section describes removal

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26 ▪▪▪▪▪▪▪ 5.1 Interactance Reflectance Configuration The Interactance Reflectance barrel should be screwed onto the probe for reflectance sampling.

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▪▪▪▪▪▪▪ 27 The probe barrel can be rinsed in a cleaning solution, then rinsed with distilled (or de-ionized) water to prevent sample carry-over from

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Metrohm AG CH-9100 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 [email protected] www.metrohm.com NIRS XDS Interactance Opt

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28 ▪▪▪▪▪▪▪ Reference Standardization requires use of an XC-1200 Calibrated 99% Reflectance Reference. Do not attempt to perform this with the R99 fr

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▪▪▪▪▪▪▪ 29 Spacers are available for 2, 4, 5 and 10mm. Note that the pathlength through the liquid sample is 2X that of the spacer, since the energy

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30 ▪▪▪▪▪▪▪ When finished sampling, the probe should be stored in the reference position. The probe end is protected from ambient light in this positi

Page 27 - 5 OptiProbe Module

▪▪▪▪▪▪▪ 31 5.2.1 Cleaning the Probe End Following analysis, the probe end should be cleaned to prevent sample carryover, which could affect analysis

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32 ▪▪▪▪▪▪▪ It is important to always clean the OptiProbe tip before placing into the reference position. Never leave any sample material on the end.

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▪▪▪▪▪▪▪ 33 6. Using a large flat-bladed screwdriver, loosen the large (3/4”) threaded plug inside the instrument opening. A larger screwdriver than

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34 ▪▪▪▪▪▪▪ 11. To re-install the reflectance standard and the threaded plug, gently turn the OptiProbe over onto the face of the module. Place a to

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▪▪▪▪▪▪▪ 35 18. Run Reference Standardization to create a new calibration for the newly-cleaned internal reflectance reference. (See section 7.1.2 fo

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36 ▪▪▪▪▪▪▪ 6 Vision Software: Connection to the Instrument This section describes communication between the computer (with Vision Software loaded) a

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▪▪▪▪▪▪▪ 37 Vision asks if the default directory location is acceptable. Click on “Yes”. Vision creates a directory for the project as shown. Vision

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Teachware Metrohm AG CH-9100 Herisau [email protected] This documentation is protected by copyright. All rights reserved. Although all

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38 ▪▪▪▪▪▪▪ Click on “Acquire”,” Connect” to initiate instrument connection. This screen sets up communication parameters for the instrument. The XDS

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▪▪▪▪▪▪▪ 39 A Data Collection Method (DCM) must be established to communicate with the instrument. There are no Data Collection Methods available upon

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40 ▪▪▪▪▪▪▪ Next, select this DCM from the selection box. Click “OK” to connect to the instrument. Once connected, verify that the amber “Communicatio

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▪▪▪▪▪▪▪ 41 7 Instrument Diagnostics Vision provides diagnostics for instrument setup, which must be performed before use of the instrument for analy

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42 ▪▪▪▪▪▪▪ This is used only on certain XDS Process Instruments. Do not select for XDS OptiProbe. When method transfer (between instruments) is antic

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▪▪▪▪▪▪▪ 43 The “visible” portion of the spectrum is similar. A linearization is applied to this portion of the spectrum. Minor artifacts appear in th

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44 ▪▪▪▪▪▪▪ Vision acquires spectra needed to perform Wavelength Linearization. No operator action is required at this point – this screen is for info

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▪▪▪▪▪▪▪ 45 7.1.2 Reference Standardization Reference Standardization is a method to provide a virtual 100% reflectance reference at each data point

Page 43 - 7 Instrument Diagnostics

46 ▪▪▪▪▪▪▪ Place the probe in this position. Click “OK” in the dialog box. The status bar indicates scan progress. Next, Vision requests that the C

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▪▪▪▪▪▪▪ 47 Vision averages the spectra of the Certified 99% Reflectance Reference, as indicated by the status bar on screen. When finished, Vision pl

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▪▪▪▪▪▪▪ 3 Table of contents 1 Introduction ...

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48 ▪▪▪▪▪▪▪ A final spectrum (green when plotted on-screen) is plotted to verify that the corrected spectrum produces the same results as the Certifie

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▪▪▪▪▪▪▪ 49 Instrument Calibration uses a stable rare-earth standard, of known wavelength response, as a method to establish wavelength scale response

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50 ▪▪▪▪▪▪▪ Next a sample scan is taken (on the reference) and this box is displayed. This takes about 20-30 seconds. Wavelength Linearization is per

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▪▪▪▪▪▪▪ 51 At the end of the test this dialog box is displayed. Click “OK” to exit Instrument Calibration. Information about the wavelength standard

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52 ▪▪▪▪▪▪▪ NOTE: The response of the WSR Wavelength Standard may vary slightly with temperature. This is typically in the range a few hundredths of a

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▪▪▪▪▪▪▪ 53 Vision requests a “Standard File”. This is provided on a mini-CD, packed in the wooden box with the standards. Insert this mini-CD into th

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54 ▪▪▪▪▪▪▪ Place the 99% standard in the sample drawer as shown. Note the position, so that it can be rotated as directed. The standards should have

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▪▪▪▪▪▪▪ 55 7.2.1 Performance Test Performance Test is a comprehensive test of instrumental performance, and is the final assurance that the instrume

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56 ▪▪▪▪▪▪▪ At the end of Performance Test, all measured values are compared with acceptance criteria stored in Vision. If all results meet acceptanc

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▪▪▪▪▪▪▪ 57 The OpQual tab brings up the display shown. This shows results of the Noise Test for each of the four wavelength regions. These regions ar

Page 56 - 7.2 Evaluation Diagnostics

4 ▪▪▪▪▪▪▪ 8.3 Lamp Replacement ... 71 8.4 Fuse Replacement ...

Page 57 - 7.2.1 Performance Test

58 ▪▪▪▪▪▪▪ The Number of Samples should be 10, as shown. The wavelength standard for reflectance is the “SRM-1920 with talc”. This is the same cell u

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▪▪▪▪▪▪▪ 59 Gently position the probe in contact with the WSR wavelength standard as shown. Do not press the probe on the quartz window, as this may

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60 ▪▪▪▪▪▪▪ If the test has passed, the user should click the cursor on the tabular display, go to the File menu, and click Print to keep a copy of t

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▪▪▪▪▪▪▪ 61 consistent over time. Note that both tests use the wavelength standard at the sample plane, where actual sample measurement is done. Perfo

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62 ▪▪▪▪▪▪▪ Vision requests a “Standard File”. For Photometric Test, use the RSSVxxxx.da file stored in the Vision directory. This file was created du

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▪▪▪▪▪▪▪ 63 Vision requests “Position Reference”. The OptiProbe should be placed in the top opening, gently resting against the Spectralon instrument

Page 63 - 7.2.3 Photometric Test

64 ▪▪▪▪▪▪▪ When the 99% standard has been scanned, the result will be plotted as shown. In this picture, the upper and lower spectra are tolerances

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▪▪▪▪▪▪▪ 65 In some cases, Photometric Test may fail and display the message shown. This indicates that the photometric scale of the instrument has sh

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66 ▪▪▪▪▪▪▪ This view shows a fairly typical OptiProbe Analyzer instrument. The gain program requires that the Interactance Reflectance probe be in th

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▪▪▪▪▪▪▪ 67 Vision asks if the user wishes to use an external sample (standard) for the test. Click “Yes” to use an external 10% reflectance standard.

Page 67 - 7.2.4 Gain Test

▪▪▪▪▪▪▪ 5 1 Introduction Thank you for selecting the XDS™ OptiProbe Analyzer, manufactured by FOSS. This instrument is the third generation in a ser

Page 68 - 7.2.5 Low Flux Test

68 ▪▪▪▪▪▪▪ Click on the tab marked “Summary” to see the summarized results as compared to acceptance specifications. Vision reports a pass or fail b

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▪▪▪▪▪▪▪ 69 8 Instrument Maintenance Instrument maintenance is quite simple on the XDS OptiProbe Analyzer. The optical enclosure is sealed to prevent

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70 ▪▪▪▪▪▪▪ Turn off power at the power switch located on the back panel. The power cord may be removed for easier access to the filter, if desired. T

Page 71 - 8 Instrument Maintenance

▪▪▪▪▪▪▪ 71 Be sure the filter material is positioned correctly, and is not wrinkled or folded. There should be no gaps at the edges. Starting at the

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72 ▪▪▪▪▪▪▪ Unplug the power cord. While this is not essential, it makes access easier. Remove the communications cable too. Loosen the six (6) capti

Page 73 - 8.3 Lamp Replacement

▪▪▪▪▪▪▪ 73 This orientation photo shows the area inside the back cover. The lamp box is at the lower left. The fan and heat sinks, shown to the right

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74 ▪▪▪▪▪▪▪ Gently grasp the corners of the lamp mounting plate. Push in about 1mm, then rotate clock-wise (to the right) about 5 mm. The lamp mountin

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▪▪▪▪▪▪▪ 75 Position the lamp with the black arrow up as shown. Gently insert the lamp and mounting plate into the lamp housing as shown. Engage the h

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76 ▪▪▪▪▪▪▪ Carefully re-install the back cover, lining up the captive screws with the mating threaded holes. Tighten gently by hand. Do not over-tig

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▪▪▪▪▪▪▪ 77 Perform tests as specified in the prior sections of this manual. These normally include the following: • Wavelength Linearization • Perf

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6 ▪▪▪▪▪▪▪ Green when stable operating temperature is reached Green when module is properly attached Vision Software™ offers an easy user interface,

Page 79 - 8.4 Fuse Replacement

78 ▪▪▪▪▪▪▪ Remove the power cord for access to the fuse. Use a tool (such as an Allen wrench) to pull the housing open. There is a small slot, unde

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▪▪▪▪▪▪▪ 79 When finished, re-install the power cord. Turn on AC power and re-establish instrument communication. 8.5 Maintenance Log Vision provide

Page 81 - 8.5 Maintenance Log

80 ▪▪▪▪▪▪▪ This screen shows entries, sorted by record number. To re-sort by another parameter, click on the column heading.

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▪▪▪▪▪▪▪ 81 9 Validation Tools Validation is an overriding concern in the pharmaceutical marketplace. In the United States, manufacturers must follow

Page 83 - 9 Validation Tools

82 ▪▪▪▪▪▪▪ customer testing. Included with your instrument are results from Performance Test, Photometric Certification, and Wavelength Certification

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▪▪▪▪▪▪▪ 83 • Independent assessment, not performed by instrument user Meets independent test requirements of CFR 21 and most auditing methods. • Fu

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84 ▪▪▪▪▪▪▪ tested product for use in the pharmaceutical industry. Documents were selected (from the enormous quantity of records in our logs) based u

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▪▪▪▪▪▪▪ 85 This screen shows many of the setup items to be set by the System Manager for 21 CFR Part 11 Compliance. To access this screen, click on C

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86 ▪▪▪▪▪▪▪ 10 Safety and Electrical Certification The XDS OptiProbe Analyzer and all associated components have been tested for CE (Communite Europe

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▪▪▪▪▪▪▪ 87 11 Troubleshooting The XDS OptiProbe Analyzer is a dependable, trouble-free instrument, designed for many years of service in your labora

Page 89 - 11 Troubleshooting

▪▪▪▪▪▪▪ 7 2 Site Readiness Like most precision instruments, the OptiProbe Analyzer is sensitive to environmental conditions that can affect its perf

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88 ▪▪▪▪▪▪▪ 2 No communication between Vision and the instrument. 1. Verify that the RJ-45 cable is plugged in at both the instrument and at the netw

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▪▪▪▪▪▪▪ 89 4 Instrument fails Wavelength Linearization 1. Verify that the Interactance Reflectance probe is positioned in the top opening, against t

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90 ▪▪▪▪▪▪▪ 6 Instrument fails Instrument Calibration. 1. Verify that the Interactance Reflectance probe is positioned in the top opening, against th

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▪▪▪▪▪▪▪ 91 9 Instrument cooling fans not operating. 1. Instrument may not be warmed up. Fans do not operate until the instrument is near operating t

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92 ▪▪▪▪▪▪▪ 12 Lifting and transporting the Metrohm instrument 1. Always separate the module from the monochromator (shown) before lifting or transp

Page 95 - 13 Index

▪▪▪▪▪▪▪ 93 13 Index Accessory Kit ............ 20 Bias ...............

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