Carbonate Removal Device CRD 180 and 200 Manual
Contents
1. Product Manual for Dionex CRD Carbonate Removal Device 180 CRD 180 0 4 mm P N 079960 Dionex CRD Carbonate Removal Device 200 CRD 200 4 mm P N 062983 CRD 200 2 mm P N 062986 CRD 200 0 4 mm P N 072054 Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 2 of 29 065068 06 2013 Thermo Fisher Scientific Inc All rights reserved All trademarks are the property of Thermo Fisher Scientific Inc and its subsidiaries Thermo Fisher Scientific Inc provides this document to its customers with a product purchase to use in the product operation This document is copyright protected and any reproduction of the whole or any part of this document is strictly prohibited except with the written authorization of Thermo Fisher Scientific Inc The contents of this document are subject to change without notice All technical information in this document is for reference purposes only System configurations and specifications in this document supersede all previous information received by the purchaser Thermo Fisher Scientific Inc makes no representations that this document is complete accurate or error free and assumes no responsibility and will not be liable for any errors omissions damage or loss that might result from any use of this document even if the information in the document is followed properly This document is not part of any sales contract between Thermo Fisher Scientific Inc and a purchaser This d2. 6 7 Howto Check for Leaks a Visually inspect for liquid drops or leakage at the Dionex CRD 180 or CRD 200 eluent and regen ports Reconnect the lines and tighten the fittings if needed Do not over tighten as damage may occur b Disconnect the lines from the regen ports of the Dionex CRD 200 and with the eluent flowing in the eluent channel of the Dionex CRD 200 observe for fluid flow out of the regen channel A continuous flow of liquid from the regen ports of the Dionex CRD 200 indicates an internal leak Replace the device For assistance contact Technical Support for Dionex Products In the U S call 1 800 346 6390 Outside the U S call the nearest Thermo Fisher Scientific office Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 28 of 29 065068 06 Appendix Quality Assurance Report QAR Appendix Quality Assurance Report QAR Eluent Eluent Source Flow Rate Temperature Detection Suppressor Applied Current Injection Volume Storage Solution Carbonate Removal Device CRD 4 mm Date Product No 062983 23 mM KOH EGC II KOH Cartridge 1 00 mL min 30 C Suppressed Conductivity using a CD25 Anion Self Regenerating Suppressor ASRS 300 4mm AutoSuppression Recycle Mode 300 mA 20 uL Deionized Water Serial No 12 0 Serial No 1012 uS Sulfate J Chloride 4 5 04 l i ken Carbonate 1 0
3. Dionex CRD 200 into the chromatography module An example of a typical installation of a Dionex CRD 200 in a chromatography module is shown in Figure 8 i The Dionex CRD 200 installation is now completed Before using the Dionex CRD 200 for analysis proceed to Section 3 3 Dionex CRD 200 Backpressure Measurement Figure 7 CRD 200 Plumbing Schematic EG CRTC A Pump i Injection valve Ly To CR TC and EG degas R IN REEN Column Backpressure Coils 4 3 4 3 sICRD q a_ ASRS f 1 Eluent in 2 Eluent out cu 3 Regen in 4 Regen out Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 17 of 29 065068 06 3 Installation Figure8 Dionex CRD 200 Installed in the System i D b b w po b w ve CONDUCTIVITY DETECTOR P N 061830 SN 13050767 inermo IENTIFIC AA D Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 18 of 29 065068 06 3 Installation 3 1 3 External Water Setup When pursuing the external water the Dionex CRD 200 is plumbed similar to what was previously described However in Step e the fluid from the cell outlet port is diverted to waste and the suppressor REGEN IN port is plumbed to the external water source It is recommended that the external water flow rate is 1 2 ml min for 2 or 3 mm applications and 3 5 ml min for 4 or 5 mm applications 3 1 4 Ch
4. the Capillary IC System Do not attempt to plug the Dionex CRD 180 or CRD 200 Capillary into any receptacle other than the CRD receptacle See the system manual for details Step 3 Ensure the suppressor and EG Degas cartridges are in place install dummy units if these devices are not available Using a 1 cc disposable syringe and a 10 32 Luer adapter push approximately 2 mL of degassed DI water through the REGEN IN port of the suppressor This will flush the regenerant chambers of the suppressor Dionex CRD 180 or CRD 200 and EG Degas cartridges simultaneously Step 4 Allow the Dionex CRD 180 or CRD 200 to sit for approximately 10 minutes to fully hydrate the membrane 2 1 3 Backpressure Instructions A WARNING Thermo Scientific 065068 06 The total backpressure to the suppressor eluent channel should be less than 100 psi This includes the Dionex CRD 180 or CRD 200 the cell and the backpressure coil Trim the backpressure coil if required to achieve lt 100 psi total backpressure Refer to Section 3 3 for backpressure measurement instructions Total backpressure amounts exceeding gt 100 psi may cause irreversible damage to the Dionex CRD 180 or CRD 200 and the suppressor Product Manual for Dionex CRD 180 and 200 Page 14 of 29 3 Installation 3 Installation 3 1 Installing the Dionex CRD 200 4 mm and 2 mm versions between the Suppressor and the Detection Cell 3 1 1 Mounting the Dionex CRD 200 to the Suppre
5. 200 should be installed in the IC System 2 To begin plumbing the Dionex CRD 180 or CRD 200 refer to the plumbing schematic shown in Figure 6 3 Turn off the pump and Dionex ACES 300 before making any connections 4 Remove the plugs from the Dionex CRD 180 or CRD 200 ports 5 Connect the Outlet tubing from the Dionex ACES 300 to the ELUENT IN port of the Dionex CRD 180 or CRD 200 Red label 6 Connect the Outlet tubing from the Dionex CRD 180 or CRD 200 Yellow label to the conductivity cell inlet 7 Connect the suppressor REGEN IN line to the outlet of the conductivity cell 8 Dionex CRD 180 or CRD 200 installation is now complete Regenerant connections are established when the Dionex CRD 180 or CRD 200 is plugged into its receptacle in the capillary system 3 2 3 External Water setup Thermo Scientific 065068 06 When using the external water mode of operation for the suppressor the Dionex CRD 180 or CRD 200 Capillary is plumbed similar to what was previously described However in step 7 the fluid from the conductivity cell outlet is diverted to waste and the suppressor REGEN IN line is plumbed to an external water source It is recommended that the external water mode be set to 0 1 mL min Product Manual for Dionex CRD 180 and 200 Page 21 of 29 3 Installation 3 3 Dionex CRD 180 or CRD 200 Backpressure Measurement The backpressure to the suppressor module may need to be measured and adjusted This will ensure opt
6. 4 mm is also recommended for the minimizing CO from acidic samples prior to injection or analysis Samples that have relatively high concentrations of CO such as carbonated beverages can out gas causing issues with reproducibility of both retention time and peak response Trapped bubbles in the system can affect the system operation and performance and overall chromatography It is therefore desirable to remove these bubbles from the sample prior to injection The Dionex CRD 200 4 mm is particularly useful for analyzing carbonated beverages such as cola As a sample pretreatment tool the Dionex CRD 200 4 mm is not recommended for basic or neutral samples since CO is no longer a volatile component rather it exists as bicarbonate and or carbonate anion in solution The Dionex CRD 200 is also recommended for anion analysis in ammoniated waters The CRD 200 is operated in the vacuum mode for the above application Product Manual for Dionex CRD 180 and 200 Page 23 of 29 4 Applications 4 2 Negative Dip at the Carbonate Peak Location A WARNING gt NOTE AN NOTE Thermo Scientific 065068 06 A negative peak may be observed at the location where the peak resulting from carbonate is removed It is hypothesize that the trace level of carbonic acid at the carbonate peak location consumes the trace hydroxide in the background and this lowers the background response at that location Some applications may not benefit from the Di
7. D and a Reagent Free Ion Chromatography System has more details on operating the Dionex NOTE CRD 200 in this mode 3 2 Installing the Dionex CRD 180 or CRD 200 Capillary between the suppressor and conductivity cell 3 2 1 Mounting the Dionex CRD 180 or CRD 200 Capillary in the IC System The Dionex CRD 180 and CRD 200 Capillary are a cartridge design and are plugged into their receptacle in the Capillary system for example the IC Cube in a Dionex ICS 5000 DC If the Dionex CRD 200 is not already installed l Thermo Scientific 065068 06 Remove the plugs from the REGEN ports at the rear of the Dionex CRD 180 or CRD 200 cartridge If a dummy cartridge or used Dionex CRD 180 or CRD 200 Capillary is installed in the CRD 200 receptacle loosen the thumb screws of the dummy cartridge or used device and pull it out Plug the new Dionex CRD 180 or CRD 200 into the CRD receptacle so the regenerant ports at the rear of the cartridge seat correctly Tighten the thumb screws to ensure a firm fit Product Manual for Dionex CRD 180 and 200 Page 20 of 29 3 Installation 3 2 2 Plumbing the Dionex CRD 180 or CRD 200 between the suppressor and the detection cell A NOTE Always use the precut tubing included with the suppressor and Dionex CRD 180 or CRD 200 Capillary to make connections Do not cut or alter this tubing the tubing is factory cut for an extremely low dead volume interface 1 The Dionex CRD 180 or CRD
8. Out In lt rom Eluent Out Port Cell Inlet Port co gas of the Suppressor Regen Regen h Out Cco carbonate Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 10 of 29 065068 06 1 Introduction 1 2 Dionex CRD 200 Configuration The Dionex CRD 200 is available in capillary 0 4 mm 2 mm and 4 mm formats for use with 0 25 0 4 2 3 4 and 5 mm Ion chromatography columns The 4 mm Dionex CRD 200 has a typical delay volume of 200 uL and is recommended for 4 or 5 mm column applications and for installation between the autosampler and injection valve The 2 mm CRD 200 has a typical delay volume of 40 uL and is recommended for 2 or 3 mm column applications it is not recommended for installation between the autosampler and injection valve The capillary Dionex CRD 200 has a typical delay volume of 2 uL and is recommended for 0 25 or 0 4 mm capillary column applications it is not recommended for installation between the autosampler and injection valve 1 3 Dionex CRD 180 Configuration Thermo Scientific 065068 06 The Dionex CRD 180 is only available in capillary 0 4 mm format for use with 0 25 and 0 4 mm Jon chromatography columns The CRD 180 has a typical delay volume of 1 uL and is recommended for 0 25 or 0 4 mm capillary column applications it is not recommended for installation between the autosampler and injection valve The Dionex CRD 180 is recommended for use with columns using 4 um bead sizes it i
9. RD 180 and CRD 200 with a Reagent Free Ion Chromatography RFIC system comprised of a Dionex Ion Chromatograph IC system equipped with an Eluent Generator Cartridge EGC Continuously Regenerated Anion Trap Column CR ATC and a hydroxide eluent compatible column such as IonSwift MAX 100 IonPac AS11 AS15 AS16 AS17 AS18 AS19 AS20 or AS21 The Dionex CRD 200 can also be used with RFIC systems pursuing borate chemistry with AS4A AS14 or AS14A chemistries The Dionex CRD 200 can also be operated under a vacuum mode of operation and this is recommended for samples such as ammoniated waters Product Manual for Dionex CRD 180 and 200 Page 7 of 29 1 Introduction Figure 1 Dionex CRD 200 Basic Plumbing CRD 200 REGEN IN CRD 200 REGEN OUT Orange Blue Base from Suppressor To CR TC Regen Out Regenerant In CRD 200 ELUENT IN Red From Suppressor Eluent Out CRD 200 ELUENT OUT Yellow To the Conductivity Cell Inlet Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 8 of 29 065068 06 1 Introduction CRD 180 and CRD 200 REGEN IN and OUT ports not shown connection automatically established when cartridge is installed in CRD receptacle Figure 2 Dionex CRD 180 and CRD 200 Capillary Basic Plumbing CRD 180 and CRD 200 ELUENT IN Red From Suppressor Eluent Out CRD 180 and CRD 200 ELUENT OUT Yellow To the Conductivity Cell Inlet 1 1 Dionex CRD 180 and CRD 200 Design and Operation T
10. al efficiency Equation 2 The Dionex CRD 180 has less capacity for the removal of carbonate with gt 80 apparent removal efficiency When plumbed between the suppressor and the cell it should be noted that high levels of CO carbonate in the sample may affect chromatographic peak shapes and recovery When plumbed between the autosampler and injection valve the sample must be acidic in order to facilitate efficient carbonic acid removal Equation 2 Apparent Removal Efficiency Response crp X 100 Apparent Removal Efficiency 100 Response crp Responseycrp Peak area or height with Dionex CRD 180 or CRD 200 installed Responsey ocrp Peak area or height without Dionex CRD 180 or CRD 200 installed It should be noted that the true CO removal efficiency is based on the chemical equilibrium outlined in Equation 1 In Equation 2 it shows underestimating this removal efficiency and therefore is the apparent removal efficiency It is included here for reference purpose only For example using a known level of carbonate for a peak height of 23 uS cm when the peak is reduced to 2 3 uS cm the true removal efficiency based on the chemical equilibrium described in Equation 1 is calculated as 99 whereas Equation 2 calculates this removal efficiency as 90 Figure3 Dionex CRD 180 and CRD 200 Design and Operation Regen In Regen Out Base from Suppressor co To CR TC 3 carbonate Eluent 2 Eluent bof uen uen To the Conductivity 4
11. d Figure4 Hydrating the Dionex CRD 200 gt 45 0 cc syringe 5 mL DI Water y REGEN OUT Luer adaptor 016640 5 cc plastic syringe i 5 0 cc syringe l Luer adaptor _ _ 024305 1 4 28 Luer Adaptor 046888 10 32 Luer Adaptor 3 mL DI Water ELUENT IN Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 13 of 29 065068 06 2 Getting Started 2 1 2 Hydrating the Dionex CRD 180 or CRD 200 Capillary gt NOTE gt NOTE Step 1 Using a 1 cc disposable syringe P N 016640 and a 10 32 Luer adapter P N 046888 very slowly push approximately 0 3 mL of degassed DI water through the ELUENT IN port The entire process should take no less than one minute Step 2 Install the Dionex CRD 180 or CRD 200 in the Capillary IC System 1 Remove the plugs from the REGEN ports at the rear of the Dionex CRD 180 or CRD 200 cartridge 2 Ifa dummy cartridge or used Dionex CRD 180 or CRD 200 capillary is installed in the CRD receptacle loosen the thumb screws of the dummy cartridge or used device and pull it out 3 Plug the new Dionex CRD 180 or CRD 200 into the CRD receptacle so the regenerant ports at the rear of the cartridge seat firmly 4 Tighten the thumb screws to ensure a firm fit Remove the plugs from the REGEN ports at the rear of the Dionex CRD 180 or CRD 200 before inserting the cartridge into the receptacle Failure to remove the plugs may cause damage to
12. ecceescesceeeseeeneeeeeetseeaecseceseenseens 28 6 7 How to Check for Leak ss 53s caccecova tsc5id os shlen ava clegd sehews yates Sedans a vavedaan sds E e sda a a Se 28 Appendix Quality Assurance Report QAR esssessseseessessoesoossossoesoossoesoesooesossoeseossoosseesossossse 29 Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 6 of 29 065068 06 1 Introduction 1 Introduction NOTE Thermo Scientific 065068 06 The Thermo Scientific Dionex Carbonate Removal Device 180 and 200 Dionex CRD 180 and CRD 200 is a membrane based module that transports CO from the suppressed eluent stream into the outer regenerant waste stream for removal Figure 1 Typically the Dionex CRD 180 and CRD 200 is installed between the suppressor and the detector cell e g conductivity cell This placement reduces the carbonate peak contributed by the sample during anion analysis by suppressed anion chromatography with hydroxide eluents Alternatively the Dionex CRD 180 and CRD 200 can be installed between the autosampler and injection valve when the sample is acidic e g carbonated beverages This placement reduces the carbonate peak contributed by the sample and eliminates out gassing of CO3 The Dionex CRD 180 and CRD 200 Capillary are not compatible with placement between the autosampler and injection valve The Dionex CRD 200 4 mm is recommended For optimal performance Thermo Scientific recommends using the Dionex C
13. emical Regenerant Mode If operating the suppressors in the conventional chemical regeneration mode or the Displacement Chemical Regeneration DCR mode the Dionex CRD 200 installation is similar to what was described previous However in step e the fluid from the cell is diverted to waste in conventional mode or to the DCR bottle DCR mode An external reservoir of 200 mM base NaOH is used as a regenerant in place of the suppressor effluent a Connect a 6 piece of 0 01 ID PEEK tubing black to the REGEN OUT port on the Dionex CRD Then connect a waste line using 1 8 OD opaque tubing and a coupler b Connect a 1 8 OD opaque tubing 18 to the REGEN IN port on the Dionex CRD and then connect the other end to a reservoir containing 200mM base c Pressurize the reservoir containing 200 mM base and adjust the gas pressure to regenerate a flow of 1 to 2 ml min through the regenerant channel of the Dionex CRD 200 It is also possible to use a displacement approach to supply the base to the Dionex CRD 200 regenerant channel The cell effluent will be used in this mode to displace the base from the DCR container into the Dionex CRD 200 regenerant channel 6699 To achieve this follow step a from Section 3 1 4 and then connect the line coming from the top of the 2 L DCR bottle P N 056882 to the cell out port on the cell The line coming from the bottom of the DCR bottle should be connected to the REGEN IN po
14. fate 75 Phosphate 15 20557 E Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 26 of 29 065068 06 6 Troubleshooting 6 Troubleshooting High backpressure may cause irreversible damage to the Dionex CRD 180 CRD 200 and suppressors The total backpressure from the cell the CRD and the backpressure coil WARNING should not exceed 100 psi 6 1 Leakage Due to High Backpressure a b c d High backpressure will cause irreversible damage to the Dionex CRD 180 and CRD 200 Measure the backpressure to the suppressor i e cell Dionex CRD 180 or CRD 200 the backpressure coil following the instructions in Section 3 3 The backpressure should not exceed 100 psi Trim the backpressure coil if needed Check the waste lines and ensure these do not contribute to the overall backpressure Replace and trim tubing s if needed When operating in external water mode ensure that the external water flow is 1 2 mL min for 2 mm and 3 mm applications and 3 5 mL min for 4 mm and 5 mm applications Lower the external water flow rate if recommended rates were exceeded 6 2 Poor CO2 Removal Efficiency a b 6 3 No Peaks a b c Thermo Scientific 065068 06 Ensure that the Dionex CRD 180 or CRD 200 is installed correctly with suppressor waste base flowing into the regenerant channel Check for leaks and reconnect Ensure that the Dionex CRD 180 or CRD 200 is connected as outlined in the pl
15. hermo Scientific 065068 06 The Dionex CRD 180 and CRD 200 consist of a gas permeable membrane with a silicone coating that is selective to CO Figure 2 In a typical system the Dionex CRD 180 or CRD 200 is plumbed between the suppressor module and the detector cell Alternatively the Dionex CRD 200 can be installed between the autosampler and injection valve The regenerant channel that encloses the Dionex CRD 180 and CRD 200 membrane is flushed with the suppressor waste base and aids removal of the CO as carbonate Suppression of the carbonate peak results in conversion to carbonic acid Carbonic acid is in equilibrium with carbon dioxide gas dissolved in water The Dionex CRD 180 and CRD 200 remove the carbonate peak as CO from the suppressed eluent Equation 1 Carbonic acid Carbon dioxide Equilibrium H CO gt H20 CO As the CO peak is removed by the Dionex CRD 180 or CRD 200 membrane the equilibrium shifts to the right thereby facilitating further removal of the CO and reducing the net carbonic acid concentration Additionally the basic environment in the regenerant channel allows a quick conversion of the removed CO to carbonate anion The net result of the above steps is a reduction of the peak resulting from carbonate Product Manual for Dionex CRD 180 and 200 Page 9 of 29 1 Introduction The Dionex CRD 200 can remove high levels of the peak resulting from carbonate gt 1000 mg L of carbonate with gt 90 apparent remov
16. imal performance of the system Failure to complete the following steps may result in a leaking suppressor and or Dionex CRD 80 or CRD 200 a After installing the Dionex CRD 180 or CRD 200 measure the total system pressure P1 b Remove the line from the ELUENT OUT port of the suppressor and measure the system pressure P2 P1 P2 P3 lt 100 c IfP3 is higher than 100 psi then trim the backpressure coil line out of the conductivity cell to achieve a total pressure of less than 100 psi A Total backpressure exceeding gt 100 psi may cause irreversibly damage to the Dionex CRD 180 or CRD 200 and or suppressor WARNING Always use 1 8 tubing when connecting lines for the regenerant side of the Dionex ERS 500 Suppressor or Dionex Atlas Electrolytic Suppressor ERS AES Dionex Carbonate Removal Device 200 CRD 200 Dionex Continuously Regenerated Trap Column CR NOTE TC and Eluent Generator EG Degas modules Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 22 of 29 065068 06 4 Applications 4 Applications The Dionex Carbonate Removal Device CRD 180 or CRD 200 has been optimized for removing the peak resulting from carbonate as CO3 in ion chromatography systems for anion analysis using Eluent Generation modules 4 1 Recommended Applications Thermo Scientific 065068 06 The Dionex CRD 180 and CRD 200 are recommended for both routine and trace level work with hydroxide and borate elue
17. m 0 0 2 0 4 0 6 0 8 0 10 0 QA Results Test Parameter Specification Results Leak Pass Fail Passed Eluent Back Pressure Pass Fail Passed Regen Back Pressure Pass Fail Passed CO2 Removal Pass Fail Passed Production Reference Datasource SPD_local Sequence Sample No 63 Thermo Scientific 065068 06 C62983 VAL 02_CRD_4mm 04 Jun 05 09 49 001012 6 60 SP3 Build 1485 Demo Installation Chromeleon Dionex Corp 1996 2003 Product Manual for Dionex CRD 180 and 200 Page 29 of 29
18. nts when the presence of CO carbonate from the sample interferes with the anion analytes By simply being exposed to carbon dioxide in the air samples can become contaminated with carbonate In some samples depending on the column and separation conditions the presence of high levels of carbonate originating from dissolved carbon dioxide interferes with the accurate determination of analytes of interest such as sulfate and nitrite Under the above conditions minimizing carbonate using the Dionex CRD 180 or CRD 200 leads to improved peak integration and quantification for analytes such as sulfate and nitrite in hydroxide RFIC systems The Dionex CRD 180 and CRD 200 are particularly useful for analyzing drinking water groundwater wastewater ultra pure water and caustic solutions where carbonate is a major component in the samples especially when pursuing large volume injections or preconcentration techniques The Dionex CRD 180 is a version of the CRD that has reduced internal volume This facilitates operation in conjunction with 4 um resin packed capillary columns without unacceptable loss of peak efficiency However the Dionex CRD 180 has less capacity for the removal of carbonate and is therefore not recommended for use with columns packed with resin larger than 4 um The Dionex CRD 180 is available only in capillary format Microbore and standard bore systems using 4 um resin packed columns should use the Dionex CRD 200 The Dionex CRD 200
19. ocument shall in no way govern or modify any Terms and Conditions of Sale which Terms and Conditions of Sale shall govern all conflicting information between the two documents For Research Use Only Not for Use in Diagnostic Procedures Revision History Revision 06 June 2013 Rebranded for Thermo Scientific Added CRD 180 Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 3 of 29 065068 06 Safety and Special Notices Make sure you follow the precautionary statements presented in this guide The safety and other special notices appear in boxes Safety and special notices include the following Indicates a potentially hazardous situation which if not avoided could result in death or serious injury gt SAFETY Indicates a potentially hazardous situation which if not avoided could result in damage to equipment gt WARNING Indicates a potentially hazardous situation which if not avoided may result in minor or moderate injury Also used to identify a situation or practice that may seriously damage the CAUTION instrument but will not cause injury gt Indicates information of general interest Z Q Highlights information necessary to prevent damage to software loss of data or invalid test ee results or might contain information that is critical for optimal performance of the system Tip Highlights helpful information that can make a task easier Thermo Scientific Product Manual f
20. onex CRD 180 or CRD 200 module due to the following reasons a Even after CO removal the peaks of interest continue to co elute with the residual CO3 peak If possible it is recommended under these conditions to investigate other columns or eluent conditions that exhibit different selectivity for the peaks of interest b The presence of CO does not interfere with peaks of interest Under these conditions there is no need for a Dionex CRD 180 or CRD 200 device The Dionex CRD 180 and CRD 200 are designed to perform optimally with hydroxide and borate eluents only It is not recommended for carbonate and or bicarbonate or cation applications The CRD 300 is recommended for carbonate and or bicarbonate eluents The Dionex CRD 180 and CRD 200 will remove CO2 from the carbonate peak thus minimizing the peak but complete removal of CO2 may not occur Due to the added delay volume of the device the early eluting peaks will show a decline in peak efficiency and all peaks will show a small change in retention time Product Manual for Dionex CRD 180 and 200 Page 24 of 29 5 Operation 5 Operation 5 1 Example Chromatograms Analysis using borate eluents is typically pursued in the nuclear power industry for analyzing borated waters In the example below the Dionex CRD 200 is useful in reducing the carbonate peak and improving the quantitation of chloride Figure9 Dionex CRD 200 with AS4A Borate Chemistry CRD Application with AS4A B
21. or Dionex CRD 180 and 200 Page 4 of 29 065068 06 Contents Contents Ls CU CHON PRAE A E A E ennai 1 1 Dionex CRD 180 and CRD 200 Design and Operation ccccccsseesseceseceeceeceseeneeeeeeeseeeeneeesaees 9 1 2 Dionex CRD 200 Configuration cccccccccsccsseceseceseceseceseeseseseeeseseseneeeaeeeaeecseecauecaeceaeceaeeneeneenaes 11 1 3 Dionex CRD 180 Co nfigut ti n ss seeeecessouienn oiii a e A a i a E E 11 2 Getting Started sosacecisciccecsvcntiacassarwnsswinasacesdsaneudeasanasccedausducidenesncsdsuceseuunasscabivcaicummeesechuaneaeniae LA 2 1 Dionex CRD 180 and CRD 200 Quick Start ccccccccccceseceesseceeseecsseeeesseseessecsseeeessessesseceeseeens 12 2 1 1 Hydrating the Dionex CRD 200 4 mm and 2 mm versions eee eseeseeseeeecneeeecseeeecaecaeenecaeeeeeneens 12 2 1 2 Hydrating the Dionex CRD 180 or CRD 200 Capillary 0 cecccecccesecsseeneeeeeeeeeeeeeeeeeeeeeseeseeeesenerens 14 2 1 3 Backpressure Instructions ccccsscessesssessecseeeseeeseeseeeseeeseeeseceseceaeceaecaaecaaecaeecaeeeaeeaeecaeeeseseeeeeeeeereearens 14 3s Mis Gea ACO sis csiesdicondecceassecedecaetedectasccakcacntsciect eadeeenssseisadsedasdeceeticie occ seosest doos ss essas esotas saas LO 3 1 Installing the Dionex CRD 200 4 mm and 2 mm versions between the Suppressor and the Detection Cell ccccccccsccsseceseceseceseeeseeeseeeseecseecsaecaeceaeceaecnseeeeseeeeseeeeeneensees 15 3 1 1 Mounting the Dionex CRD 200 to
22. orate Chemistry 8 C Column IonPac AS4A AG4A 4 mm Without Eluent 100 mM boric acid 7 CRD 5 5 mM KOH EG us Flow Rate 1 5 mL min 2 5 Suppressor ASRS ULTRA IL 4 mm Current 300 mA 0 Oven 30 C 012345 67 8 9 1011 Minutes Concentrator IonPac AG4A 81 Volume 40 mL C With 51 CRD Sample Concentration ppb uS 2 Fluoride 10 Carbonate n a 2 54 Chloride 10 O E a a S S S S S S E 01234567 8 9 1011 Minutes nae Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 25 of 29 065068 06 5 Operation A typical anion application at ppb level shown below demonstrates the utility of the Dionex CRD 200 to remove CO and aid in the improved quantitation of sulfate Figure 10 Dionex CRD 200 with AS19 Gradient Chemistry CRD Application with AS19 Gradient Chemistry Conditions 130 Tis a l Column AS19 4 mm hee w o CRD Flow rate 1 0 ml min in Suppressor ASRS Ultra II 4 mm Current 300 mA i 4005 0 200 220 Loop 200 ul 1 00 f Oven 30 C i i J Time Gradient mM fees See 0 10 0 40 Peepers TU DATA Pa a 10 10 0 0 5 0 10 0 15 0 20 0 25 0 30 0 35 0 5 45 30 45 1 80 uS T300 30 1 10 a w CRD 35 10 0 625 d of NU Sample Concentration ppb 0400 g0 00 20 A0 Fluoride 10 1 00 4 Chloride 15 1 5 8 Nitrite 50 2 3 i i Bromide 50 it I 6 A Nitrate 50 0 40 Fe Carbonate n a 0 0 5 0 10 0 15 0 20 0 25 0 30 0 35 0 Sul
23. rong tubing dimensions for a given application may damage the CRD 200 and suppressor modules 1 The Dionex CRD 200 is installed on the top of the Dionex ERS module as shown in Figure 6 2 To begin plumbing of the Dionex CRD 200 refer to the plumbing schematic as shown in Figure 7 a b c d e Turn off the pump and the Dionex ERS suppressor before making any connections Remove the plugs from the Dionex CRD 200 ports Connect an approximately 2 inch length of 0 062 1 16 OD Black or Red tubing from the ELUENT OUT port of the suppressor to the ELUENT IN port of the CRD 200 red label Connect an approximately 6 inch length of 0 062 1 16 OD Black or Red tubing from the conductivity cell inlet port to the ELUENT OUT port of the Dionex CRD 200 yellow label Connect a short piece of 1 8 OD tubing opaque from the backpressure coil at the cell outlet port to the REGEN IN port of the suppressor Connect an approximately 5 inch length of 1 8 OD tubing opaque from the REGEN OUT port of the suppressor to the REGEN IN port of the Dionex CRD 200 orange label Product Manual for Dionex CRD 180 and 200 Page 16 of 29 3 Installation g Divert the REGEN OUT port of the Dionex CRD 200 blue label to the waste or use it as a regenerant stream for other modules such as continuously regenerated trap column Dionex CR TC and the Eluent generator EG degas assembly h Reinstall the suppressor and the
24. rt on the Dionex CRD 200 The DCR bottle should be completely filled to the top with 200mM base In the above setup the cell effluent displaces the DCR bottle hence the contents of the DCR bottle should be replenished when the eluent container is replenished For further information on DCR operation refer to the DCR manual 3 1 5 Installing the Dionex CRD 200 in the Vacuum Mode of Operation Thermo Scientific 065068 06 The Dionex CRD can also be operated in the vacuum mode to support specific applications such as analysis of anions in an ammoniated water sample Operation using the base regenerant is not recommended for these samples since ammonia out gases in a basic environment and can cause anomalous baseline shifts To install the Dionex CRD 200 in the vacuum mode a continuous source of vacuum is needed that would generate approximately 65mm of Hg Install the Dionex CRD 200 as described oo before However in step e the fluid from the cell is diverted to waste a Connect a 6 piece of 0 005 ID PEEK tubing red to the REGEN OUT port on the Dionex CRD This is a bleed line for the vacuum b Connect a 1 8 OD opaque tubing 18 to the REGEN IN port on the CRD and then connect the other end of the tubing to a vacuum source c Apply a vacuum to the regenerant channel to aid removal of volatile components such as CO and NH3 Product Manual for Dionex CRD 180 and 200 Page 19 of 29 3 Installation 3 1 6 Ins
25. s not recommended for use with columns using bead sizes greater than 4 um Product Manual for Dionex CRD 180 and 200 Page 11 of 29 2 Getting Started 2 Getting Started The Dionex CRD 180 and CRD 200 must be handled with care to ensure proper operation Fittings only need to be finger tightened A Do not attempt to disassemble the Dionex CRD 180 or CRD 200 it may result in irreversible damage WARNING 2 1 Dionex CRD 180 and CRD 200 Quick Start 2 1 1 Hydrating the Dionex CRD 200 4 mm and 2 mm versions Step 1 Using a 5 cc disposable plastic syringe P N 016640 and the 10 32 Luer adaptor P N 046888 push approximately 3 mL of degassed DI water through the ELUENT IN port Using a 5 cc disposable plastic syringe P N 016640 and the 1 4 28 Luer adaptor P N 024305 Remove the storage tubing from the Regen OUT port and push 5 mL of degassed DI water through the REGEN OUT port Figure 4 the ELUENT OUT port to the REGEN IN port on the CRD by using suitable tubing and pumping 5 mL of deionized water through the CRD ELUENT IN port In the above step it NOTE is recommended to bypass the guard and analytical columns A Step 1 can be accomplished by installing the Dionex CRD 200 in the system and connecting Step 2 Allow the Dionex CRD 200 to sit for approximately 10 minutes to fully hydrate the Dionex CRD 200 membrane Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 12 of 29 065068 06 2 Getting Starte
26. ssor Always minimize tubing lengths for obtaining efficient peaks For 4 mm or 5 mm A applications standard bore format use 0 010 ID x 0 062 1 16 OD Black tubing For 2 mm applications microbore format or 3 mm applications use 0 005 ID x 0 062 NOTE 1 16 OD Red tubing 1 The Dionex CRD 200 is installed on the top of the Dionex ERS suppressor The Dionex CRD 200 is shipped with self adhesive Velcro tape that is used to attach the device to the Dionex ERS suppressor 2 To install remove the suppressor from the Chromatography Module and remove all connections to the suppressor 3 Remove the backing tape from the self adhesive Velcro on the Dionex CRD 200 Figure 5 and push it firmly into place on the suppressor as shown in Figure 6 The Dionex CRD 200 can be easily removed or reinstalled by simply pulling the device on and off the Dionex ERS suppressor Figure5 Velcro tape on rear of Dionex CRD 200 Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 15 of 29 065068 06 3 Installation Figure 6 Dionex CRD 200 Installed on Suppressor 3 1 2 Plumbing the Dionex CRD 200 between the Suppressor and the Detection Cell A NOTE Thermo Scientific 065068 06 For 4 mm or 5 mm applications standard bore format use 0 010 ID x 0 062 1 16 OD Black tubing For 2 mm or 3 mm applications microbore format use 0 005 ID x 0 062 1 16 OD Red tubing Connecting the w
27. talling and Plumbing the Dionex CRD 200 4 mm between a Dionex AS DV or Dionex AS40 Autosampler and Injection Valve The Dionex CRD 200 may be installed on the top of the Dionex ERS module as in Section 3 1 alternatively the Dionex CRD 200 may be installed elsewhere in the system The included self adhesive Velcro can be used to attach the Dionex CRD 200 to any convenient solid surface 2 Replace the PEEK injection tubing on the bleed valve of the Dionex AS40 auto sampler with a 50 cm 18 in piece of orange 0 51 mm or 0 020 in i d tubing Install the free end into the Eluent In port of the Dionex CRD 200 3 Cut another 20 cm 8 in piece of orange PEEK and install one end in the Eluent Out port of the Dionex CRD 200 and the other end into Port 5 of the injection valve 4 Connect the regenerant waste line of the EGC degas module to the Regen In port of the Dionex CRD 200 5 Connect another length of 1 6 mm or 0 063 in i d Teflon to the Regen Out port of the Dionex CRD 200 and direct the other end to waste A It is important that the flow rate of the sample through the Dionex CRD 200 does not exceed 2 0 mL min On a Dionex AS40 this is achieved by selecting the Concentrate WARNING mode See the Dionex AS40 Operators Manual for more information Application Update 153 Fast Determinations of Phosphate and Citrate In Carbonated Beverages Using On Line Degassing with the Carbonate Removal Device CR
28. the Suppressor cecccecccessesssceseceseceeeceeesecaecaeecaeeeeeeseeeeeeeneeeeens 15 3 1 2 Plumbing the Dionex CRD 200 between the Suppressor and the Detection Cell cece 16 3 1 3 External Water Setup iesin inisini aeeie niese EEEE E EE EEEE o KA EEEE EEEE E 19 3 1 4 Chemical Regenerant Mode isiccc ccccccccccseseessscsdeccseseiceus sted cicestendsteacacdscessetesdecddcosseceessadeddecsageddeseedieestavs 19 3 1 5 Installing the Dionex CRD 200 in the Vacuum Mode of Operation ceeeseseeseceeeeececeeeeeseeaeeneens 19 3 1 6 Installing and Plumbing the Dionex CRD 200 4 mm between a Dionex AS DV or Dionex AS40 Autosampler and Injection Valve uo ceeecceeeeesceeeeeceseeeeeseceeesecacesecsaeeneeaeeaeeaeeaeeeeeneens 20 3 2 Installing the Dionex CRD 180 or CRD 200 Capillary between the suppressor and conductivity Cell eececcccescsssesseeeeeeeseeeseecseecseecaeceaeceseceseenseeeeseeesseeeeeneeeaeensees 20 3 2 1 Mounting the Dionex CRD 180 or CRD 200 Capillary in the IC System ceccesseecseereeeeeeeees 20 3 2 2 Plumbing the Dionex CRD 180 or CRD 200 between the suppressor and the detection cell 21 3 2 3 External W ater SQtup iiss ssecedscacquesscsteces cdsacuszecageesecacpevsaegatieas cscaesdeecavenacgueteag evades ccnteuas cdadeuancdaderseegategnacas 21 3 3 Dionex CRD 180 or CRD 200 Backpressure Measurement cccccscesseeeteceseceseceeeeseeeeeeeesneeaes 22 d APMC ATs warccssrcccncscvsssnessendcens
29. tosdsenaroussascnandcanuteedenaccquacecsduscecendaenanssdeutesesnaedeentaesivesubeencaemie ZO 4 1 Recommended Applications ccccccccscessessseeseesseecssecsseceseceseceseceeeeaeeeseecsaecsuecaeceaeceaeenseenseeaes 23 4 2 Negative Dip at the Carbonate Peak Location ececceseeseeeeceseeseeeecesecaeeeecesecaeeeeeesecnaeeneeeeeeaeeas 24 3 OPGranON T A E T E EEE N ENEE So 5 1 Example Chromatograms secisscssccssscsscvecocastasncadesdvaacevceavacdeeacand cauasenadceksassacchacsddesnvacetuenteanaceseasaies 25 Thermo Scientific Product Manual for Dionex CRD 180 and 200 Page 5 of 29 065068 06 Contents 6 Troubleshooting sisi ccs ccesccensaeuswhdativcckanesuickeneandaeuntcantdaccauccsebuossedanscevensincanciogiasecbapasvesigusensdeace 27 6 1 Leakage Due to High Backpressure cccsccesscesscesseeeceeeceeeeeeneeeseceseeeseecsaecsaecsaecaeceseenaeenaeenaes 27 6 2 Poor CO Removal Efficiency ccccecccesseceseceseceseceseceeeeeeeeeeneceseeeseecssecssecsaecsecesecnaeeneeeseeeeneeeags 27 6 3 INO PEAKS a fates cated fase aS dies et Pests cag Bats tact Posts etude a a teat Santaatodiaesnasdisatauedsacens tate nat oscaen actos 27 6 4 High Noise in the Baseline and on Top of the Peaks cc cccecsseeseesseeneesseensecesecsseeseeenseeeseeeses 28 6 5 Negative Dips Before All the Analyte Peaks ccccccssccssecessceeeceeeeeeeeeeseeeseeeseeesaeeaeesseenaeenaeens 28 6 6 Negative Peak or Dip at the Carbonate Peak Location cccccc
30. umbing instructions Check for leaks and reconnect The Dionex CRD 180 or CRD 200 may have an internal leak due to damage replace the device Product Manual for Dionex CRD 180 and 200 Page 27 of 29 6 Troubleshooting 6 4 High Noise in the Baseline and on Top of the Peaks a Ensure that the recommended RFIC EG system pressure is maintained optimal operating pressure for 2 mm and 4 mm systems is 2300 psi If needed add the backpressure coil for raising the total system pressure by installing 0 003 ID Yellow tubing between the EG degas module and the injection valve b Release any trapped gases in the cell suppressor or the Dionex CRD 180 or CRD 200 by systematically opening the lines from e ELUENT OUT port of the suppressor e The ELUENT IN and ELUENT OUT ports of the Dionex CRD 180 or CRD 200 e The cell outlet port 6 5 Negative Dips Before All the Analyte Peaks a Analytical IC systems only The tubing leading into or exiting the Dionex CRD 200 may not be cut straight Recut the ends of the tubing ensuring the cut is perpendicular to the tubing and the finish is smooth and flat b The suppressor may not be fully regenerated Regenerate the suppressor using sulfuric acid as outlined in the suppressor User s Manual c The Dionex CRD 180 or CRD 200 may have an internal leak due to damage Replace the device if a leak is detected 6 6 Negative Peak or Dip at the Carbonate Peak Location a Refer to Section 4 2
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