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76 

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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 
Configure, Account Policy. 

A 21 CFR Verification Document is 
available for users who wish to verify 
key features. This document is 
included with Vision installation 
materials, on the same CD, starting 
with Vision 3.50, SP1.  

Please contact your local distributor 
for information, or if you cannot 
locate this document. 

 

Содержание NIRS

Страница 1: ...NIRS XDS RapidLiquid Analyzer Manual 8 921 8005EN...

Страница 2: ......

Страница 3: ...Metrohm AG CH 9100 Herisau Switzerland Phone 41 71 353 85 85 Fax 41 71 353 89 01 info metrohm com www metrohm com NIRS XDS RapidLiquid Analyzer Manual 8 921 8005EN 03 2013 fpe...

Страница 4: ...entation 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 an...

Страница 5: ...n opening closing drawer to main body of manual Removed flow through cuvettes from manual Added information of flow through bulkhead fittings Moved Wavelength Linearization ahead of Instrument Calibra...

Страница 6: ...blems 15 3 6 1 Network Troubleshooting Overview 16 3 6 2 Direct Connection Troubleshooting Overview 20 4 Assembly of the Instrument 21 5 Rapid Liquid Module 26 5 1 Wavelength Calibration of the Rapid...

Страница 7: ...strument Test Guide and Results 72 9 1 2 Installation and Operating Qualification Documents 73 9 1 3 NIRStandards for Instrument Performance Verification 73 9 1 4 Instrument Performance Certification...

Страница 8: ...ses various patented algorithms to provide superior accuracy and transferability between like instruments This instrument uses near infrared NIR spectral energy to illuminate the sample By measuring t...

Страница 9: ...t communication is through RJ 45 network connections which eliminates issues involved with long runs of RS 232 cable An Internet Protocol IP address is dynamically requested upon connection This addre...

Страница 10: ...m the instrument Replace the filter If dust has accumulated on the fans carefully wipe them clean with a moist soft cloth Do not distort or damage the fan blades or fins as this will impede cooling Do...

Страница 11: ...ull instructions are given in section 3 0 2 6 Instrument Dimensions and Weight XDS Rapid Liquid Analyzer dimensions are Width 18 0 457 mm Leave about 6 152mm on the right side for ease of sample loadi...

Страница 12: ...cannot be responsible for software and instrument problems resulting from the use of two network cards in the host computer This information is correct as of the time of original publication Changes...

Страница 13: ...n may result in lost commands lost data and unsatisfactory software operation Metrohm cannot be responsible for software and instrument problems resulting from the use of two network cards in the host...

Страница 14: ...n internally stored default IP address This address 169 254 0 2 is used for local free standing communication only In such cases a crossover cable or a hub with two patch cables should be used to conn...

Страница 15: ...e Dynamic Host Configuration Protocol DHCP is an Internet protocol for automating the configuration of computers that use TCP IP DNS Server A Domain Name Server DNS Servers run special purpose softwar...

Страница 16: ...ight NIRSystems XDS series Instrument Driver as shown then click on Configure Information At this point Vision requests any XDS instrument on the local area network LAN to report connection status Thi...

Страница 17: ...ms Vista is good also but may impose user security restrictions Windows 2000 is almost as simple but may require an extra step or two as discussed If your computer uses Windows 95 98 or NT 4 0 for the...

Страница 18: ...tting which should be changed It may be necessary to contact your IT department for assistance with these issues First verify that the network has a DHCP Server If no DHCP server is available the inst...

Страница 19: ...y When finished click OK Close all other boxes opened for this verification If the settings were not set properly it may be necessary to exit Windows XP then re enter XP to have the correct settings t...

Страница 20: ...it may be necessary to verify that the XDS instrument is installed within the IP address range of the computer Network Solution 3 Verify network has full IPv4 compatibility Some networks have moved t...

Страница 21: ...inished click OK Network Retry XP and Vista Windows XP and Vista users should click on Retry Only This command resets the communication port and allows Vision to find the instrument if connected prope...

Страница 22: ...ame IP range as the XDS instrument The XDS instrument default IP address is 169 254 0 2 as shown This address calculator gives the allowable computer IP address range as 169 254 0 1 through 169 254 2...

Страница 23: ...Analysis Software Spare Lamp in Accessory Kit Accessory Kit containing cords cables and other required items Safety Manual for CE certification Instrument Test Results Packet XC 1300 Wavelength Calibr...

Страница 24: ...el opens to about a 45 degree angle for access to connectors and for filter inspection Avoid scratches or damage 4 Gently thread the AC power cable and network cable through the lower right corner of...

Страница 25: ...it is a UTP crossover cable and will not work with a network Use a network cable as described in section 3 0 7 Close the outer cover of the instrument Push gently to the final closed position It shoul...

Страница 26: ...e instrument The final assembly is as shown Note that the sample drawer is closed It will open upon power up Do not attempt to open the drawer manually 11 Plug the AC power cord into a grounded AC out...

Страница 27: ...es will be heard as items find their initial positions This is normal 14 Once the instrument has initialized the sample drawer will quietly open as shown Do not attempt to push or force the drawer It...

Страница 28: ...nd Technology NIST transmission standard This assures that wavelength registration of each Liquid Analyzer is set to known standards Instrument Calibration is required for transferability between inst...

Страница 29: ...mpounds where the constituents will remain in solution for the duration of analysis and evaporation is not an issue Compounds with volatile ingredients should be analyzed in sealable cuvettes to preve...

Страница 30: ...size cuvettes The cuvette size is stamped on top of the spacer The spacers are designed to thread into a 10 32 tapped hole inside the sample drawer to keep the spacer in the proper position Insert th...

Страница 31: ...sample drawer is in the desired position disconnect from Vision 5 9 Liquid Sampling Considerations The XDS Rapid Liquid Analyzer is capable of detecting low levels of analytes in liquids A brief over...

Страница 32: ...ighlight the 2 propanol absorbances at 1690nm and 2310nm Absorbance at 1690mm using a 1mm cuvette appears too low to be of much use Absorbance at 1690nm is about 0 55 absorbance units using a 2mm cuve...

Страница 33: ...n box appears on the opening screen Enter the default User ID NIRS It is not case sensitive Tab or mouse to the Password box and enter the default password NIRS Note that you should set up specific Us...

Страница 34: ...ts up communication parameters for the instrument The XDS instrument has a unique driver Highlight this box and click on Configure This box allows the user to set the COM port and select the instrumen...

Страница 35: ...project and DCM must be created to allow the change in data collection Do not use Blank Correction during Diagnostics It does not apply during Diagnostics To enable Blank Correction cancel out of Data...

Страница 36: ...e set for the number of seconds required for samples to reach the desired temperature setting Measure several typical samples to determine this time then enter it into the DCM Add several seconds to b...

Страница 37: ...ion the sample drawer will quietly open Do not manually force the sample drawer to either an open or closed position It is under software control Next select this DCM from the selection box Click OK t...

Страница 38: ...t right is the default set of selections A brief explanation follows Instrument must stabilize before data acquisition This prevents spectral acquisition if the instrument is cold Performance Test mus...

Страница 39: ...brations and are used to apply corrections to the instrument to minimize differences between units of the same configuration The correction programs are accessed from the Diagnostics menu bar shown at...

Страница 40: ...in these raw spectra due to detector crossover and other spectroscopic reasons After linearization these artifacts are minimal or not evident some being beyond the usable range of the instrument This...

Страница 41: ...this message confirms the transfer Click OK to proceed 7 1 3 Blank Correction The Rapid Liquid Analyzer has the option of Blank Correction to provide an optimum photometric match between instruments...

Страница 42: ...sample area After the sample area is scanned a dialog box prompts that Vision is ready to plot the Blank Correction Click OK to proceed The spectrum at the right is a Blank Correction and is a typica...

Страница 43: ...was later determined that better transferability between instruments could be achieved if each standard was calibrated on the Metrohm NIRSystems master transmission instrument Since that time each WS...

Страница 44: ...trum The method has been proven by comparing SRM 2035 sample scans on multiple instruments with Instrument Calibration turned off then on The resulting scans are most consistent with Instrument Calibr...

Страница 45: ...tion to proceed A dialog box will appear and the user should click Yes to proceed to the next step Continue until this step is completed The user must confirm the linearization to proceed A dialog box...

Страница 46: ...ion between instruments At the same time bandwidth bandpass is measured and is iteratively adjusted to an optimum value This is performed to assure good agreement from instrument to instrument should...

Страница 47: ...later run Photometric Test to check the repeatability of instrument performance This is detailed later in this manual in Evaluation Diagnostics Photometric Test compares the current performance of the...

Страница 48: ...ndards spectra for stability For Number of Replicates retain the default setting of 1 Click on OK Vision will begin to take an instrument reference scan The red progress bar at the bottom of the scree...

Страница 49: ...ick on Diagnostics Wavelength Certification Run Wavelength Certification The Number of Samples should be 10 as shown Recent Vision software defaults to the Trans Cal Std XC 1300 which gives more infor...

Страница 50: ...is shown in the upper right quadrant of the screen A tabular report is shown giving each peak its nominal position and its measured position The difference from nominal peak position and the repeatabi...

Страница 51: ...for each instrument Note that Bandwidth is only computed on the XC 1300 WST3Wxxx Trans Cal Std which is the same standard used in Instrument Calibration Shown on left The printout above is for WST3W01...

Страница 52: ...the external standard As discussed under Performance Test the internal reference materials are not traceable and are only used as an internal method of maintaining correct wavelength measurement on t...

Страница 53: ...successful and this dialog box is displayed Before clicking Close All Reports the user is directed to the tabular display To view the tabular display of results place cursor over the tabular display a...

Страница 54: ...may proceed with sample analysis The XDS instrument contains internal wavelength reference materials which are used as a means to maintain monochromator wavelength measurement These internal wavelengt...

Страница 55: ...service Because the calibrated photometric standards are the link to previous photometric performance the standards should always be stored in their wooden box and protected from fingerprints droppin...

Страница 56: ...S Rapid Liquid Analyzer remain the same in all versions Vision displays the wavelength regions for test For Rapid Liquid instruments these regions give a good overall picture of instrument performance...

Страница 57: ...use the same set with the labeled mini CD Position the standard in the sample drawer with the label facing the user When the T01 standard has been scanned the result will be plotted as shown In this...

Страница 58: ...2 4 Gain Test The Gain Adjust feature can be a useful diagnostic tool though it is not required for normal operation Technically gain is never adjusted on the XDS Rapid Liquid Analyzer The name of the...

Страница 59: ...al 10 transmission standard in the sample position A noise test is run using this standard Because the transmission value is less than the instrument standard the test is considered a good method for...

Страница 60: ...o run the Low Flux Test when using an external sample standard If the user clicks No to the external standard then Vision will automatically trigger the 10 internal screen for this test No user action...

Страница 61: ...value This photo shows the set point as 27 0 degrees C and the actual sample temperature as 26 1 degrees C approaching the set point An equilibration delay may be set in Vision to permit the samples...

Страница 62: ...ifference between ambient temperature and set point temperature In practice it is best to check the equilibration time with a temperature probe in the cuvette to determine the actual time required Whe...

Страница 63: ...Metrohm service personnel The instrument should be kept clean at all times If it becomes dusty or dirty wipe it with a damp soft cloth to restore the finish Sampling areas should be kept clean to prev...

Страница 64: ...ould release allowing the door to open as shown Lower the door as shown to expose the filter material Using a 1 4 nut driver remove the four 4 40 nuts that hold the filter frame in place Lift the filt...

Страница 65: ...carefully over the screws as shown The screws should penetrate the filter material fully Install the filter frame Install the 4 40 nuts and tighten hand tight as shown Gently close the instrument doo...

Страница 66: ...and unplug AC power cord from AC receptacle or supply The O position is OFF Allow the instrument to cool for about 15 20 minutes before attempting to change the lamp 2 On the back side of the instrum...

Страница 67: ...to release the retaining ring from the shoulder screws 5 This photo shows the lamp retaining ring in the removal position The spring will tend it push the retaining ring outwards when the shoulder scr...

Страница 68: ...ge Always keep a spare lamp in stock to avoid last minute emergencies The part number is XA 3000 8 Unpack the new lamp from the protective box Place the new lamp carefully onto the bench and place the...

Страница 69: ...own Note the shoulder screws holding the lamp retaining ring The black arrow on the lamp should point straight upward as shown This is required for proper wavelength registration in Instrument Calibra...

Страница 70: ...spare lamp after changing this lamp order one from your Metrohm distributor immediately NOTE The lamp is a very special assembly and should never be replaced with any substitutes Special features of...

Страница 71: ...t from AC power Open the side cover Remove the AC power plug from the AC power block of the instrument Use a tool such as an Allen wrench to pull the housing open There is a small slot where the tool...

Страница 72: ...the AC power cord in Plug the RJ 45 cable in if it was removed Turn on AC power and re establish instrument communication 8 5 Maintenance Log Vision provides a Maintenance Log in the Diagnostic Datab...

Страница 73: ...s shown in the screen below In addition the user may enter text comments which are saved as part of the log Enter the text then click on OK This screen shows entries sorted by record number To re sort...

Страница 74: ...rmly enforced with analytical instrumentation There are many reasons for this including assessor familiarity with NIR instrumentation However the enforcement is beginning to be applied more commonly I...

Страница 75: ...ular testing of NIR instrumentation to verify continuing stability of photometric and wavelength response These transmission standards operate with Vision Software Vision records first use instrument...

Страница 76: ...s 9 2 1 Installation and Operating Qualification Documents Software Installation Qualification IQ and Operating Qualification OQ Documents are included as part of the Vision Spectral Analysis Software...

Страница 77: ...s will apply Escrow agreements for source code are available 9 2 3 21 CFR Part 11 Compliance Vision meets the strict requirements of 21 CFR Code of Federal Regulations Part 11 covering Electronic Reco...

Страница 78: ...creen click on Configure Account Policy A 21 CFR Verification Document is available for users who wish to verify key features This document is included with Vision installation materials on the same C...

Страница 79: ...al energy have been evaluated The instrument design is meant to dissipate any thermal energy A circuit interlock is provided as a backup to primary thermal controls The instrument has been tested at m...

Страница 80: ...on For minor problems this guide should be consulted While some recommendations are quite basic some of the suggestions may be helpful in avoiding oversights or problems Follow the recommendations and...

Страница 81: ...ot damaged crushed or distorted in any way Wires should be firmly clinched by the connectors 3 Lamp does not come on when instrument is connected 1 Verify communication with instrument Click on Acquir...

Страница 82: ...ate it to another part of the laboratory or place it on isolated supports away from the XDS Analyzer 4 A weak lamp will exhibit higher noise near the end of its life This may also show up as one or tw...

Страница 83: ...76 102mm space in by fan exhaust for proper airflow 4 Check ambient temperature in area where instrument is used If temperature is near the maximum fan flow will be high 9 Instrument cooling fans not...

Страница 84: ...nees not with the back Lift unit up move to a cart and lower gently Do not lift from below waist level as the unit may be awkward to control Ask for assistance when lifting from lower levels to bench...

Страница 85: ...0 IP Address 15 18 32 IPV Setup 45 46 53 55 Lamp 3 7 21 63 68 79 Lamp Replacement 3 63 Low Flux Test 57 58 Maintenance 61 70 71 Module 9 21 24 26 27 37 Monochromator 9 21 Network Connection 10 NIRStan...

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