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You can make a request for the operating manual by completing the adjoining form. Subsequently, you will receive the operating manual as pdf-file. Visit our Shop Request a PDF Therefore, you will receive offers and information about relevant topics by e-mail or post. You can unsubscribe from this notification at any time. Dionex ICS-3000 (Ion Chromatography, no peak detected. Hi All, After our preventive maintenance, when running standards, we can no longer see fluoride, chloride, bromide, nitrate, sulfate and phosphate peaks in our chromatogram. Although the EGC KOH cartridge has just expired last April 2016, we checked the pH of the waste coming out from the column line and it is pink or basic. Personnel who used the equipment last time also reported that he was able to use an expired EGC KOH cartridge, Id like to ask why are we not seeing sample signals during our run. Have you experienced this. The service personnel calibrated the detector via a meter and checked it by bypassing the column and directly injecting 10ppm HNO3 to the conductivity detector to check if a signal will appear. A signal did appeared, however was it proper. What are the risks? Please help! Best Regards! Ion Chromatography Chromatographic Techniques Analytical Chemistry Instrumentation Share Facebook Twitter LinkedIn Reddit Most recent answer 2nd May, 2019 Tien Do Van Ulan national institute science and technology Hi, I am setting up an IC version ICS3000. There is a Na peak in blank (DI water). I already checked blanks by another IC but it did not show Na peak like ICS3000 (using the same eluent and DI water). Then I changed new column and suppressor but it still showed Na peak in blank (same eluent and blank). I checked Dtector and Pump also. They did not have any problem. Do you know any posible problem in my case. Turn off the suppressor and re-inject again after the background conducitivity is very high, in case water dip is not visible.
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Re-check all the correct plumbing from the injector onwards till the suppressor and the end of the detector. Most probably the system is not injecting anything. Secondly, what is your background conductivity. Cite 3rd Jun, 2016 Rey Sanjorjo Gyeongsang National University Hello Professor Wahab. Apparently I am still on the process of building expertise in my IC, can you give me a description what is a water dip. Where can we see it and how will it look like. We always make sure that our background conductivity when running samples is always below 1uSv. Currently the system is running at and below 0.01uSv. We did a check on the autosampler and we can see a flow in the line after that. We can check it again for clogs and possible injection problems as we have only checked it once. Cite Deleted profile Water dip, refers to the disturbance in the IC chromatogram due to a decrease in the conductivity of the baseline. It is an indication of the dead time of the system. Turn off the suppressor and check if the conducitivity is rising or not. Inject pure deionized water. You should see a dip in the baseline. If you don't see a dip, autosampler, or injection lines are clogged. Cite 1 Recommendation 20th Sep, 2016 Greg Malek Thermo Fisher Scientific Hi Rey, I'm an ion chromatography specialist. The water dip refers to the negative peak experienced directly before fluoride in the chromatogram. What does your chromatogram look like when you don't get any peaks. From your information, it appears the conductivity detector itself is functioning correctly. Have you tried a different EGC or manually preparing the eluent. Have you tried doing manual injection into the sample loop to eliminate issues with the autosampler. Are you using the autosampler to inject onto two systems? If so, that requires a diverter valve and its position needs to be set correctly in order to properly fill the sample loop. When was the last time the column was used successfully.
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Cite Can you help by adding an answer. Answer Add your answer Similar questions and discussions How to calculate limit of detection, limit of quantification and signal to noise ratio. Question 99 answers Asked 16th May, 2014 Praveen Dhyani Reg. Hplc standard curve calculation. Please tell me how to calculate limit of detection, limit of quantification and signal to noise ratio. Please also explain what is the relation of these parameters with each other. Usually in papers it is mentioned that LOD and LOQ were measured based on signal to noise ratio at about 3 and 10, respectively. View Is there any possibility to resolve high conductivity problem with Cationic Ion chromatographic system. Question 3 answers Asked 19th Apr, 2015 Yerabham Praveenkumarreddy Even though i tried to hydrate the suppressor with NaoH and milli q, i couldn't decrease the conductivity to less than 2 even retention times are effecting due to the high conductivity. Can someone please help me to resolve the problem. Thank you. View Has anybody already encountered negative peaks on IC. Question 5 answers Asked 27th Aug, 2015 Catherine Signoretty I run IC with high ionic concentration of mobile phase. I started to get negative peaks at my defined RT. They become deeper and deeper. I cleaned the lines, made fresh solutions, nothing works. I noticed my back pressure is getting slowly higher and higher. Any advice around? Is BP related to these dips. What could be the cause of the BP. View How to fix the pressure increase in ion chromatography. Question 8 answers Asked 24th Jan, 2018 Vijetha Mogilireddy Hi all. I'm having troubles with Ion chromatrography (Metrohm 881). As soon as I start the stabilisation, pressure increases rapidly and the pump stops working as it reaches the maximum pressure (defined in the method). Thank you. View Can anyone help with problem regarding overlapping peaks of sodium and ammonium during standardization.
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Question 14 answers Asked 23rd Jul, 2014 Arindam Roy We are getting overlapping peak of sodium and ammonium during standardization in ion chromatography. We use 1PPM 3PPM 5PPM and 10PPM as standard. The problem is mostly happening in case of 3,5,10 ppm of samples. Does any one have a clue about it. View DIONEX ICS-3000 Throuble shooting Question 28 answers Asked 1st Aug, 2017 Carlos Ezquer Hi. I am working now with a DIONEX ICS-3000 HPLC system. Chamshaft 145 ?. Excessive Drive Current. Anybody knows any idea about how to solve this problem please. Question 5 answers Asked 15th May, 2016 Nor Laili Azua Jamari Hi all. I need your suggestion. Thanks!! View Could anyone help me to improve separation between chlorides peak and nitrites peak in water anlysis by IC. Question 2 answers Asked 3rd Oct, 2013 Silvia Frati I work with DIONEX ICS 5000, the column is AS 9HC; after 2000 runs in two months the chlorides and nitrites peaks are nearly overlap, I lose resolution. How could I restore the column efficiency. Thanks View What cause shifting of retention time of a peak forward. Question 9 answers Asked 3rd Nov, 2016 Medhat Emad 1- I have problem in shifting of retention time of a peak: During analysis of rebamipide, the peak of rebamipide shift forward. NASA SP5083 Article J. S. Whittick Rosaria Francesca Muraca L. A. Cavanagh View An RC Active Filter Design Handbook. Analytical Chemistry Instrumentation: A Survey. NASA SP5104 Article Gordon J. Deboo View Got a technical question. Get high-quality answers from experts. Keep me logged in Log in or Continue with LinkedIn Continue with Google Welcome back. Keep me logged in Log in or Continue with LinkedIn Continue with Google No account. All rights reserved. Terms Privacy Copyright Imprint. By fully integrating eluent generation (RFIC-EG) technology the Dionex Aquion RFIC system uses proven and reliable technologies to deliver results you can count on.
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The system is designed for ease of use, providing fast start-up times and reliable, stable performance for demanding applications in environmental, food safety, and academic laboratories. In addition, it is compatible with all Dionex suppressor technologies and column formats from 2 mm to 5 mm. An ion chromatography system typically consists of a liquid eluent, a high-pressure pump, a sample injector, a guard and separator column, a chemical suppressor, a conductivity cell, and a data collection system. By comparing the data obtained from a sample to that obtained from the known standard, sample ions can be identified and quantitated. The data collection system, typically a computer running chromatography software, produces a chromatogram (a plot of the detector output vs. time). The chromatography software converts each peak in the chromatogram to a sample concentration and produces a printout of the results. The Ion Chromatography components consist of: Among the advantages of electrolytic suppression are fast startup times, superior sensitivity for both cation and anion analysis, reduced background conductivity and enhanced day-to-day consistency. The temperature-controlled, high-performance conductivity cell is unaffected by ambient temperature variations. In addition, digital control offers a wide dynamic range for detecting analytes with large concentration variations within the same sample. With eluent generation, gradient separations can be as easy as isocratic applications. This line of trap columns removes contaminants, thereby eliminating trace ionic impurities, such as carbonate, from the eluent stream. Control, status, and diagnostics are provided with the Chromeleon CDS software. Compared to manual eluent preparation RFIC-EG provides superior results by preventing baseline shift, increasing sensitivity, improving resolution, and ensuring consistent peak integration. It also makes your system more reliable.
The features of the Chromeleon CDS software make system control and setup fast and easy. Overall system and method consistency is accomplished with minimal effort using easy-to-follow screens and setup wizards. The CD20 manual recommends using a DS3 Detection Stabilizer containing the flow cell. There is a DS4 Stabilizer available - I'm assuming this is a newer version of the DS3. Does anyone know if the DS4 can be used with the CD20 detector? ThanksBest regards. If you continue browsing the site, you agree to the use of cookies on this website. See our User Agreement and Privacy Policy.If you continue browsing the site, you agree to the use of cookies on this website. See our Privacy Policy and User Agreement for details.If you wish to opt out, please close your SlideShare account. Learn more. You can change your ad preferences anytime. I don't have enough time write it by myself.A Problem Tree (Page 2). An Overview (Pages 3-7). An Overview of the Anion-Exchange Chromatography system. Problems Section (pages 8-14)Running the Ion Chromatography System (Pages 15-27)Flushing the SystemYeIs there a problem with theIs the pressure tooIs there very high background. Noise?Pump ProblemsIs the syringe leaking,Blockage in Needle. Injection or Diverter. Valve (Page 13). Blockage of the. Halide Trap (PageThis section is a brief overview of the entire chromatographyIt will also allowSection 1: AS-AP Auto sampler. This is the first section of theThe carousel is divided into three sections labelled with different colours (Red, GreenThe carousel can be shut for protection againstThrough Chromeleon, another command can come in use for mixing, which allowsTab.
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The needle injects theJust like the carouselThe dual pump section may look confusing, but inThe sectionThe pumps then send the eluent or deionised water through diverter valves all acrossBut it can also have a great affect on the overallUnderneath the pumps lies a gradient mixer, this contains a small filter that theAs the eluent types, ratios andThe section when opened contains various parts that can beThe eluent cartridge contains a specific eluent, thisAbove the CRTC is a degasser, the eluent that isJust like the dual pump section the rest of the system it is readyThis is the main section of the Ion chromatographySample Cartridges. The Ion Chromatographer currently contains a set of a trap column,The sample then travels through the. InGuard cartridges which work together to remove the chloride fromThe final stage is the concentrator, the concentrator allows the sample to be retainedFigure 7: InGuard Cartridge. ATC-HC Trap ColumnProblems SectionFigure 10: Suppressor Method. Figure 11: an example of a ChromatogramAt the top of the page, there willContinue toPress closeProblems with the Pump; Low pressure, (signals alarm and redYou can also check the pressure onYou can then release the black valveOnce you have done this youThen switch it back on andIf it’s jumping 10-20psi, then this is an indication ofIt should only vary around 1-2psi at most, as thisBackground Noise and Eluent ConcentrationChromeleon starts to show, huge levels of background noise then, this canEluent will be going over the suppressor.The build up should be reduced by this and should settle down back to normal.High Pressure Build up in the Halide TrapIn order to remove this build up similar the steps are very similar to thoseWhilst it’s running theFigure 17: Eluent Generator Programme pageWhen the noise remainsIf this doesn’t workBlockage in Needle, Injection or Diverter ValveChromeleon data, sampler page.
This line is the final point before the sampleIf it isn’t then on the samplerASAP on the right hand side of the page, this should allow you to executePerform a flushOnce all these haveRunning the Ion Chromatography System. Creating a new sequenceThe data can be removed and replaced, but it is a good way to compareBut if you’re creating a sequence from scratch, use the following steps;Carbohydrates). Select the one you need and then click next.You can also select the number ofClick Finish. (Name it, recommended as date. Troubleshooting GuideIt can also be used to run a start up programme in theN.B Remember to turn off any injections that are labelled as blanks, as these willThis date and time can be changed, soFigure 21: Sequence Queue PageClick Create Instrument method. (ToIt will also ask youOnce these have both been chosen, click next.Generator Cartridge). The concentration mode can be changed and theClick Finish.Creating an Eluent GradientIC is on standby.You want to save as much water as possible as if it’s empty, it can causeFigure 24: Eluent Concentration PageAs the eluent concentration is brought down,The suppressorUsing the Virtual Column Separation SimulatorIt will display theColumn QA conditions.Figure 25: Virtual Column Separation Simulator. How to Analyse Chromatogram ResultsThe Results tab when clicked will bringThis is the bestTo move the baseline backCreating a Calibration CurveFigure 27: Results PageUsing the calibration plot it will compare the results toThis is very important if you are retesting a sample asThis can be relatively tricky for someone new to the instrument so a diagramConcentrator attachments, as well as using both systems and a switch betweenThis difference can be seenWhen open click on configure instrument and it will take you to the commandClick on file and load upTo begin with, reattach the TrapPosition 4 and 1 shouldThis device can also remain attached when changing methods.
Position 2 isSystem 2 6-port diverter valve and capped off to prevent drying out.Figure 31: Sulphite ConfigurationNow customize the name of a clipboard to store your clips. J Page 230 and 231: ED40 Electrochemical Detector Detec Page 232 and 233: ED40 Electrochemical Detector Modes Page 234: ED40 Electrochemical Detector Index show all Thank you, for helping us keep this platform clean. The editors will have a look at it as soon as possible. The Dionex Integrion system’s flexible detector configurations meet your analysis needs for today and tomorrow. Its high-pressure capabilities enable faster analysis without compromising data quality. Use the system’s automated eluent generation (EG) to eliminate error-prone manual eluent preparation and achieve better method reproducibility. No 22153-60203) Please use our contact formular in the section “contact” or check out the responsible person under “Team”. For more details, please see our Privacy Policy. I Accept For more details, please see our Privacy Policy. I Accept For more details, please see our Privacy Policy. I Accept Read about. The analytical method is based on ion exchange between a mobile phase consisting of the eluant, which transports the sample, and a stationary phase at the solid-state (ion-exchange resins). The negative or positive (active center) ions are fixed to aromatic rings. In order to construct the calibration curves, at least 6 calibration levels, with different concentrations, are used. It is therefore possible to determine the calibration curve for each species. It represents a control of the quality of analyses. EG40, EG50 Eluent. Generator. Operational Manual: Bookkeeping. Guide. Swaziland Commercial Agricultural Production And. Marketing Project. Khan (Bangladesh) for Text contribution. Surapong Monmano (Thailand) for. QED 6 Defibrillator Analyzer is manufactured in Everett, Washington by Fluke BioIntroduction. 1. My quick guide to great D300 photos.
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Qualification Software Templates for IC and BioLC Instruments, revision 5.11. This publication is protected by federal copyright law. No part of this publication may be copied or distributed, transmitted, transcribed, stored in a retrieval system, or transmitted into any human or computer language, in any form or by any means, electronic, mechanical, magnetic, manual, or otherwise, or disclosed to third parties without the express written permission of Dionex Corporation, 1228 Titan Way, Sunnyvale, California 94085-4015 USA.Documented evidence must be provided to demonstrate the integrity of data collected and qualify the results obtained on laboratory instrumentation. The following institutes set and control industry instrumentation standards: NIST. The National Institute of Standards and Technology is an administrative body of the US Department of Commerce. Together with the industry, the NIST develops new technologies and sets technological standards countrywide. These standards are written in broad terms to make them as widely applicable as possible. All stipulate general requirements specifying instruments must be fit for purpose, technically checked in defined periods, calibrated and make sure that test results are documented according to international quality standards. For example, direct sunlight and close proximity to air conditioning ducts will cause thermal irregularities that will affect baseline drift on conductivity detectors. In these cases, it may happen that the manufacturer’s specifications are not met, and the specifications may have to be adjusted accordingly. Module name, type and serial number. Software and firmware version. This will help keep track of what steps to follow during system setup and preparation. It will also aid in selecting the appropriate sequences to run the tests. 2. For the DX500, DX600, and ICS2500 systems, electrochemistry cells are not used for any qualification tests apart from noise and drift qualification.
If a customer uses amperometry methods, a conductivity cell must be used in its place to perform injector and gradient pump tests. 3. For the ICS-3000 system, electrochemistry cells in Integrated Amperometry mode are supported for qualification tests. If using Integrated Amperometry detection, a conductivity detector must be used in its place to perform a gradient pump test (pump flow test and EG test should also be run in conductivity mode). For a system with only electrochemical detectors, it is suggested that a complete system qualification be performed with a conductivity detector (including pump gradient accuracy, flow rate, and EG), after the system has been qualified with the conductivity detector, the detector should be exchanged for an ED detector. The ED tests (noise and drift, detector linearity) can be executed as described in this manual. The ICS-3000 electrochemistry detector DC amperometry and cyclic voltametry modes are not supported. When qualifying Integrated Amperometry detection a disposable gold working electrode is use. In his specification, the supplier has therefore to define exactly the conditions that must be observed. OQ should be performed after initial system installation or when an additional new module is added to an existing system. A system is subject to wear when being operated. Thus, it may happen that the supplier’s specification is no longer met. This means: The test procedures used for OQ are also used for PQ, but the tolerances of PQ are less restrictive than those for OQ. Using the same test procedures simplifies the handling. PQ should be performed at regular intervals after the initial installation and OQ. Dionex recommends performing PQ every six months. It is the responsibility of the qualification engineer to determine the most up to date revision of the templates available and ensure that revision is used before proceeding with this qualification.
It is recommended that the qualification be performed using the most current Chromeleon service pack version (Contact Dionex Technical Support for current version). It is recommended that the qualification be performed using the most current firmware version for each system or module (Contact Dionex Technical Support for current version). As described in section 1.1, OQ and PQ are system-specific test procedures. The procedures described below are valid for IC systems comprising of the following equipment (only one type of detector and one pump can be qualified concurrently): Pump: IP20, IP25, IS25, DX120, IC20, IC25, IC25A, GP40, GP50, GS50, ICS-90, ICS-1000, ICS1500, ICS-2000, ICS-3000 SP, ICS-3000 DP. Sampler: Manual injection: AS, AS40, AS50, TSP AS3500. Absorbance detector: AD20, AD25, UVD-170U, PDA-100, UVD-340U, ICS Series VWD, ICS Series PDA. Conductivity detector: CD20, CD25, CD25A, DX120, IC20, IC25, IC25A, ED40, ED50, ED50A, ICS-90, ICS-1000, ICS-1500, ICS-2000, ICS-3000 CD. Electrochemical detector: ED40, ED50, ED50A, ICS-3000 ED. Fluorescence detector: RF-2000 with UCI-50, UCI-100 or UI20 interface. Such modifications are not within the scope of this document. It is not possible to qualify multiple detectors on a single system, with the following exceptions: An RF-2000 detector must be qualified in series with a conductivity detector. For the ICS-3000, it is not possible to qualify multiple pumps on a single system. Instrument All conductivity detectors. CD20, CD25, CD25A, ED40, ED50, ED50A, IC20, IC25, IC25A, DX-120, ICS-90, ICS-1000, ICS-1500, ICS-2000, ICS-3000 CD AD20 and AD25, ICS Series VWD. Parameter Baseline Noise. Concentration and peak height are represented on a graph. Wavelength Accuracy. Holmium oxide maxima are compared with the theoretical maxima. Baseline Drift. Electrochemical detectors. ED40, ED50, ED50A. ICS-3000 ED Limits OQ Baseline Drift. UVD-170U, UVD-340U Description Baseline Drift. RF-2000 All injectors and samplers.
AS, AS50 and TSP AS3500 Automated Sampler. Parameter Description Limits OQ PQ Baseline Noise. Emission Wavelength is changed from 450 to 394 nm to give a response of between 40 and 80 mV. Change the name or directory if required. These sequences will be copied to the corresponding datasource. Click “Finish”. 8. When the installation is complete the “Specification” page opens in the report. Instrument names and test limits will be filled in automatically into the report if it is opened after the “Warm Up” sample is run. During the copying this is not the case. Click on the “Default Panel Tabset”. Turn the cell voltage to “On”. 1. Open the “Qualification” menu in the Browser. 2. Select “Instruments OQ” or “Instruments PQ”. A wizard opens and assists you in copying the sequences. Click on the sequences required for the tests. A copy is made and the batch list of the respective timebase is automatically updated and opened. Click on Ready Check to confirm the program and method files contained in the sequence are compatible with the configured system. Make modifications to the program files if necessary. Note: If an Eluent Generator is configured on the system, the following message may occur at the Ready Check: “Flow rate not specified at time 0.0, using a flow setting 1.00.” This refers to the Eluent Generator flow rate, not the pump flow rate. It is not necessary to take any action since the Eluent Generator is not used for this part of the qualification. Proceed with starting the batch. If qualifying an AD20 absorbance detector, close the Start Batch dialog box by clicking on the Cancel button. Otherwise, start the batch to process the sequences. Note: For systems with a shared auto sampler there might be a number of informational messages indicating that “Exclusive Access” has not be acquired or released. Do not change this report (exceptions; step 9, Section 2.6 and below). In the report, many references are used between the individual data sheets.
When lines or columns are deleted or inserted, those references may be lost so the calculations may be wrong. Open the Printer Layout (View menu) and select the Specification page from the tabs at the bottom of the report. Make sure the report is in Layout Mode (Edit menu). If the Moduleware Versions are not recorded, enter Moduleware Versions into the Moduleware Version column of the Instruments section as well as any Descriptions, Lot and Serial Numbers and Expiration Dates in the accessories section. For ECD and IC systems the columns will contain amount values for the nitrate standards, for Abs systems it will contain amount values for caffeine standards and for ICS-3000 ED systems it will contain amount values for threonine standards. These values should be modified to match the exact reported amounts listed on the certificate of analysis that came with your standards kit. Select the sequence for which to print the report, ensure that no sample is marked, select “Batch Report” in the “File” menu and start printing by clicking “ok”. It is possible to highlight all completed sequences and print all the reports at once. 2.7.2 Repeating Individual Tests It may be necessary to repeat individual tests. If so, review Section 5 where problems are described according to which individual tests might fail. According to Good Laboratory Practice, all tests following the one that failed must be repeated. If this is the case release the “Exclusive Access” command before proceeding. Once the qualification sequences begin, the system being qualified will gain and retain exclusive access to the autosampler, column TC and compartment TC until the “Stop” sequence is run and “Exclusive Access” is released. “Exclusive Access” can be released by going to the command function (F8), choosing the module from the list, and executing the “ReleaseExclusiveAccess” command. The wavelength accuracy test for AD20 absorbance detectors is the only tests performed manually.
The wavelength accuracy test for AD20 absorbance detectors must be completed before starting the main qualification. Set the detector wavelength to 354 nm and then press Enter on the front panel. Locate the row of sheet names at the bottom of the report. Print the sheet. This will allow for manual recording of test results. Test results can also be directly entered into the report (see Step 10). Allow the detector to equilibrate for approximately 20 seconds. Record the offset absorbance value as the measured absorbance for 354 nm. This value should be approximately 0.0000 AU. 6. Manually change the wavelength setting on the front panel of the AD20 to 355 nm and press Enter on the front panel. Go to Edit and turn Layout Mode on. Update the SPECIFICATION page with the correct information. Enter today’s date in the Additional Information section. Enter all previously recorded values in the table on the sheet. In some cases a cell value may need to be modified (i.e. change the detector serial number), for this modification Chromeleon Report Publisher is required. If Chromeleon Report Publisher is not available, the cell can be modified by clearing the value of the cell and typing in the new value. Print the sheet. Click on Edit and turn Layout Mode off. Choose the same datasource and directory used for the main part of the qualification. 11. If any part of the test does not pass, refer to Section 5 for troubleshooting assistance. 3.3.2 Flow Rate Accuracy and Precision Qualification The Flow Rate Accuracy and Precision test is designed to qualify the flow-rate accuracy and precision of all pumps, with the exception of the ICS-90 and DX-120. No flow-rate test is required for ICS-90 and DX-120 systems. Systems equipped with an AS3500 autosampler cannot be qualified automatically by this procedure. Dionex does however suggest the use of alternative protocols to verify flow rate measurement.