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6

 – Dionex Suppressor Cleanup 

 

 

 

 

Thermo Scientific 

Product Manual for the ERS 500 Suppressor 

Page 70 of 84 

031956-11 

For Research Use Only. Not for Use in Diagnostic Procedures.

 

6.

 

Dionex ERS 500, Dionex ERS 500e and 

Dionex AERS 500 Carbonate Suppressor 
Cleanup 

This  section describes  routine  cleanup procedures  for  the  Dionex  Electrolytically  Regenerated 
Suppressors (Dionex ERS 500, Dionex ERS 500e or Dionex AERS 500 Carbonate) in the case 
of contamination. Consult the Troubleshooting Guide (see 

Section 5, “Troubleshooting Guide”

) 

to first determine that the system is operating properly. If the suppressor is determined to be the 
source  of  higher  than  normal  back  pressure,  higher  than  anticipated  conductivity,  decreased 
suppression  capacity  or  decreased  sensitivity,  cleaning  the  membrane  may  restore  the 
performance of the system. Use the following procedures to clean the membrane. 

 

6.1

 

Metal Contaminants or Precipitates 

 

The suppressor voltage is a good indicator of the resistance across the suppressor. Higher 
resistance may indicate contamination of the suppressor. For more information regarding 
monitoring  the  voltage,  see  Document  No.  031841-02  “Removal  of  Iron  Contamination 
from Electrolytic Suppressors.” 

 

A.

 

Turn off the Dionex ERS or Dionex SRS Control unit and system pump. 

B.

 

Disconnect  the  analytical  (and  guard)  column(s)  from  the  injection  valve  and  the 
suppressor. Refer to the specific analytical column Product Manual for column cleanup 
procedures. 

C.

 

If you are running in the AutoSuppression External Water Mode, turn off the external 
water and disconnect the external water line from the suppressor REGEN IN port.  

D.

 

Disconnect  the  liquid  line  from  the  suppressor  ELUENT  OUT  port  to  the  cell  at  the 
cell fitting and reconnect it to the REGEN IN port. 

E.

 

If  iron  is  present  then  connect  a  temporary  line  from  the  priming  block  or  the  low-
pressure tee on the isocratic or gradient pump to a container with a solution of 0.2 M 
oxalic  acid.  For  4  mm  systems  pump  this  solution  through  the  suppressor  at  1  –  2 
mL/min for 30 minutes. For 2 mm systems pump this solution through the suppressor 
at 0.25–0.50 mL/min for 30 minutes. Proceed to step G. 

F.

 

If iron is not present then proceed to step G. 

 
 

 

NOTE

!

Содержание 082540

Страница 1: ...For Research Use Only Not for Use in Diagnostic Procedures Dionex ERS 500 Suppressor 031956 Revision 11 January 2017 User Manual...

Страница 2: ...y Regenerated Suppressor 500 Dionex CERS 500 4 mm Item 082542 Dionex CERS 500 2 mm Item 082543 Dionex Anion Electrolytically Regenerated Suppressor 500e Dionex AERS 500e 4 mm Item 302661 Dionex AERS 5...

Страница 3: ...ceived 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...

Страница 4: ...ry Indicates a potentially hazardous situation which if not avoided could result in damage to equipment Indicates a potentially hazardous situation which if not avoided may result in minor or moderate...

Страница 5: ...oils for the Dionex ERS 500 Dionex ERS 500e and Dionex AERS 500 Carbonate 24 2 4 1 Assembly 24 2 5 Gas Separator Waste Tube for the Dionex ERS 500 25 2 5 1 Assembly 25 2 6 Electrolytically Regenerated...

Страница 6: ...han 7 days 43 4 Example Neutralizer Mode Applications 44 4 1 System Blank 44 4 1 1 Anion System Blank 44 4 1 2 Cation System Blank 44 4 2 Dionex CERS 500e Conditioning 45 4 3 System Calibration 45 4 3...

Страница 7: ...Suppressor Cleanup 70 6 1 Metal Contaminants or Precipitates 70 6 2 Organic Contaminants 71 Appendix A Current Settings 72 A 1 Optimum Current Settings for Common Eluents Dionex AERS 500 4 and 2 mm a...

Страница 8: ...or has become an integral part of the ion chromatography instrument The suppressors from Thermo Fisher Scientific are designed for continuous operation and do not require any switching or offline rege...

Страница 9: ...Regenerated Suppressor Dionex AERS 500 and the Cation Electrolytically Regenerated Suppressor Dionex CERS 500 to support anion and cation analysis applications The Dionex ERS 500 system consists of a...

Страница 10: ...eric O ring installed in the regenerant channel The eluent in and out ports are independent ports that define the fluidic pathway similar to a column The regenerant flow is arranged to be counter curr...

Страница 11: ...operation the electrolytically generated hydronium ions in the Dionex AERS 500 are driven towards the cathode along with eluent cations by the applied voltage The membrane allows hydronium ions to pa...

Страница 12: ...ly a more conductive acid form Figure 2 AutoSuppression with the Dionex AERS 500 The Dionex Electrolytically Regenerated Suppressor for External Water Mode Dionex ERS 500e is optimized for use in the...

Страница 13: ...ow performance The Dionex AERS 500 Carbonate uses the same ion exchange membranes screens and resin materials as the standard Dionex AERS 500 suppressor The Dionex AERS 500 Carbonate is configured wit...

Страница 14: ...terials such as screens membranes and resins allow hydroxide ions to move from the cathode chamber into the eluent chamber to neutralize the acid eluent MSA ions or eluent or sample counter ions in th...

Страница 15: ...ex ERS 500 Dionex ERS 500e and Dionex AERS 500 Carbonate AutoSuppression Recycle Mode AutoSuppression External Water Mode MPIC Suppression Mode Neutralization Mode The Dionex ERS 500 is not compatible...

Страница 16: ...Yes assuming Ion Pairing Reagent Complex Samples or Samples containing Solvents No Yes 3 Yes Yes assuming Ion Pairing Reagent 1 The Dionex ERS 500 is not recommended for External Water Mode the Dione...

Страница 17: ...s mode Thermo Scientific Dionex recommends the use of a Chemically Regenerated Suppressor Dionex CRS 500 or equivalent for chemical suppression applications Please refer to the Dionex CRS Manual Docum...

Страница 18: ...enerant chambers The regenerant water can be delivered from a pressurized bottle or pump If using a pressurized bottle it is recommend to use the Dionex ERS 500e IMPORTANT The Dionex AERS 500 Carbonat...

Страница 19: ...ations are typically converted to a strongly ionized form The sample cations are now in a weakly dissociated matrix such as water and are ready for analysis 1 2 6 2 Trace Ion Analysis After Neutraliza...

Страница 20: ...a direct replacement for the Dionex SRN series of neutralizers such as the Dionex SRN 300 Dionex SRN II and Dionex SRN products The Dionex ERS 500 Dionex ERS 500e and Dionex AERS 500 Carbonate are des...

Страница 21: ...ppressor performance it is important to operate the suppressor at the recommended current settings as recommended by Chromeleon or as calculated from Section 2 6 1 It is highly recommended to set the...

Страница 22: ...Suppression Mode or MPIC Mode The Dionex ERS 500 Dionex ERS 500e and Dionex AERS 500 Carbonate must be operated with the Gas Separator Waste Tube Item 045460 The use of 28 or 10 32 ferrule bolt style...

Страница 23: ...resolution If an ERS Mode is not available select the equivalent SRS Mode on the power supply to support the Dionex ERS 500 suppressor The Dionex ERS 500 and Dionex ERS 500e are fully compatible with...

Страница 24: ...em 045878 for 2 mm systems the backpressure coils are available in the microbore tubing kit Item 052324 Alternatively lengths and diameters of tubing necessary for proper back pressure are given in Ta...

Страница 25: ...arator Tube above the top of the Waste container C Place the Gas Separator Waste Tube with the 1 8 o d tubing attached into the waste container Ensure the bottom of the Gas Separator Waste Tube is res...

Страница 26: ...Dionex RFC 10 Dionex RFC 30 or Dionex SCC 10 Controller is recommended for older systems that only set the current in discrete values of 50 100 300 or 500 mA A lower flow rate requires a lower curren...

Страница 27: ...rom the equations below Dionex AERS 500 4 mm or Dionex AERS 500 Carbonate 4 mm Sum of eluent concentration mN 2 Carbonate mM Bicarbonate mM hydroxide mM 2 Tetraborate mM custom eluent cation mN where...

Страница 28: ...applications These ultra high purity solvents will usually ensure that your chromatography is not affected by ionic impurities in the solvent Dionex has obtained consistent results using High Purity...

Страница 29: ...umulate The Gas Separator Waste Tube must be open to the atmosphere and not in a confined space to operate properly 3 2 1 Hydration Hydrating the suppressor ensures that the ion exchange membranes are...

Страница 30: ...k pressure coils and with the pump on measure the system pressure P2 4 mm Chromatography 2 mm Chromatography_______________ 1 0 mL min 2 black backpressure coils 0 25 mL min 2 red backpressure coils I...

Страница 31: ...kly ionized form After passing through the conductivity cell this effluent can be redirected to the regenerant inlet on the suppressor thus supplying it with a source of water containing a small amoun...

Страница 32: ...ure coils are provided in the Gas Separator Waste Tube Components Assembly Item 045825 for 4 mm systems The backpressure coils for 2 mm systems are provided in the microbore tubing kit Item 052324 see...

Страница 33: ...and LC25 ovens 1 For all ANION and CATION applications up to 40 C install the suppressor in the oven using the suppressor holder 2 For operation above 40 C and up to 60 C it is recommended that the s...

Страница 34: ...is supplied to the regenerant chambers to generate hydronium or hydroxide ions for neutralization AutoSuppression External Water Mode is used when organic solvents or metallic contaminants are presen...

Страница 35: ...opriate i d tubing depending on your application requirements Refer to Section 2 4 and see Table 3 for the correct back pressure tubing requirements Install and adjust the flow rate of water from the...

Страница 36: ...ate is dependent on two factors the pressure applied to the water reservoir and the current setting It is best to measure it with the current on since the application of current can affect the final f...

Страница 37: ...l suppression mode applications The Dionex ERS 500e and Dionex AERS 500 Carbonate can be used in the Chemical Suppression Mode however the total suppression capacity is reduced compared to a Chemicall...

Страница 38: ...tem 039164 To operate a system in the MPIC Suppression Mode configure the system and use the appropriate sulfuric acid concentration as described in Section 3 6 3 3 6 3 MPIC Suppression Mode Operation...

Страница 39: ...ng on the specific MPIC application The MPIC Suppression Mode is a combination of the AutoSuppression External Water Mode augmented with a chemical regenerant if necessary such as boric acid H3BO3 Whe...

Страница 40: ...CERS 500 at current settings over 300 mA can reduce the life of the suppressor and produce unnecessary baseline noise 2 Measured with power ON using a graduated cylinder For the lower eluent concentra...

Страница 41: ...ure inlet of the plastic reservoir B Make the following liquid line connections 1 Use a coupler Item 039056 to connect one end of the 30 tubing assembly Item 035727 that comes in the AutoNeutralizatio...

Страница 42: ...Operation For detailed operation of Dionex IC systems consult the accompanying Product Manuals The Dionex ERS 500 suppressor is not recommended for use with the Neutralization Mode of Operation The D...

Страница 43: ...ompletely hydrated to maintain liquid seal and chromatographic performance Plug all of the ports after hydration 3 8 1 Short Term Storage 3 to 7 days A Using a plastic syringe push 5 mL of deionized w...

Страница 44: ...inants in deionized water can be removed by installing Dionex IonPac ATC HC column between the sample carrier pump and the Sample Valve The major source of sulfate contamination is usually from the Di...

Страница 45: ...oad 24 sulfuric acid C Switch the sample valve to Inject position and flush the sample loop with deionized water D After the sulfuric acid passes through the neutralizer and IC injection valve approxi...

Страница 46: ...00 234 238 22 n 8 Separation Conditions are shown in Section 4 7 Dionex IonPac AS12A Isocratic Analysis of 25 Sodium Hydroxide 4 5 Recovery Data for Trace Cations in 24 Sulfuric Acid Cation 24 H2SO4 S...

Страница 47: ...ibration 0 90 10 0 0 5 mM NaOH for 7 min 7 0 90 10 0 Analysis 0 0 90 10 0 0 5 mM NaOH Inject 0 2 90 10 0 Inject Valve to Load Position 2 5 90 10 0 0 5 5 0 mM NaOH in 3 5 min 6 0 0 100 0 5 0 38 25 mM N...

Страница 48: ...AG11 Guard Column Analytical Column Dionex IonPac AS11 Analytical Column Eluents E1 Type I Deionized Water E2 5 0 mM NaOH E3 100 mM NaOH Eluent Flow Rate 2 0 mL min 4 mm Electrolytic Suppressor Dionex...

Страница 49: ...1 000 1 009 9 Monochloroacetate 1 000 ND 1 000 0 811 10 Bromate 1 000 ND 1 000 1 036 11 Chloride 0 400 8 750 9 150 9 095 12 Trifluoroacetate 1 000 ND 1 000 1 055 13 Bromide 0 600 ND 0 600 0 640 14 Ni...

Страница 50: ...ion Concentrator i e Dionex UTAC XLP2 Item 072781 Column Dionex IonPac AG12A Dionex IonPac AS12A Eluent 2 7 mM Na2CO3 0 3 mM NaHCO3 Eluent Flow Rate 1 5 mL min Electrolytic Suppressor Dionex Anion Ele...

Страница 51: ...ted 25 NaOH Standard Spiked Value Spiked Conc Conc Conc Conc Conc mg L mg L mg L mg L mg L 1 Chloride 0 200 0 100 0 155 0 003 0 255 0 258 0 004 2 Bromide 0 200 0 100 ND 0 100 0 099 0 008 3 Chlorate 0...

Страница 52: ...n Low Pressure Trace Anion Concentrator i e Dionex UTAC XLP2 Item 072781 Column Dionex IonPac AG12A Dionex IonPac AS12A Eluent 2 7 mM Na2CO3 0 3 mM NaHCO3 Eluent Flow Rate 1 5 mL min Electrolytic Supp...

Страница 53: ...olumn Low Pressure Trace Anion Concentrator i e Dionex UTAC XLP2 Item 072781 Column Dionex IonPac AG12A Dionex IonPac AS12A Eluent 2 7 mM Na2CO3 0 3 mM NaHCO3 Eluent Flow Rate 1 5 mL min Electrolytic...

Страница 54: ...ow Pressure Trace Anion Concentrator i e Dionex UTAC XLP2 Item 072781 Column Dionex IonPac AG12A Dionex IonPac AS12A Eluent 2 7 mM Na2CO3 0 3 mM NaHCO3 Eluent Flow Rate 1 5 mL min Electrolytic Suppres...

Страница 55: ...A Analytical Column Eluent 20 mM Methanesulfonic acid Eluent Flow Rate 1 0 mL min Electrolytic Suppressor Dionex Cation Electrolytically Regenerated Suppressor Dionex CERS 500 Recycled Eluent Mode or...

Страница 56: ...hemical Suppressor Dionex Cation Chemically Regenerated Suppressor Dionex CCRS 500 Chemical Regenerant 100 mN TBAOH Expected Background Conductivity 20 mM MSA 1 S Expected System Operating Back Pressu...

Страница 57: ...Analytical Column Eluent 20 mM Methanesulfonic acid MSA Eluent Flow Rate 1 0 mL min Electrolytic Suppressor Dionex Cation Electrolytically Regenerated Suppressor Dionex CERS 500 Recycled Eluent Mode o...

Страница 58: ...ytical Column Eluent 20 mM Methanesulfonic acid MSA Eluent Flow Rate 1 0 mL min Electrolytic Suppressor Dionex Cation Electrolytically Regenerated Suppressor Dionex CERS 500 Recycled Eluent Mode or Ch...

Страница 59: ...Analytical Column Eluent 20 mM Methanesulfonic acid MSA Eluent Flow Rate 1 0 mL min Electrolytic Suppressor Dionex Cation Electrolytically Regenerated Suppressor Dionex CERS 500 Recycled Eluent Mode...

Страница 60: ...dicates that there is high resistance or an open circuit in the suppressor device typically in the regenerant channel or there is an issue with connectivity of the suppressor to a power supply High re...

Страница 61: ...onex ERS 500 Dionex ERS 500e or Dionex AERS 500 Carbonate at the analytical column end of the line Direct this line to a separate waste beaker B Disconnect the eluent line from the ELUENT OUT port of...

Страница 62: ...mm 100 mA Dionex AERS 500 Carbonate 4 mm 125 mA Dionex AERS 500 Carbonate 2 mm 30 mA 5 2 3 Full or Extended Regeneration Depending on the extent of capacity loss of the suppressor the regeneration pr...

Страница 63: ...Purple trace show recovery during Suppressor Electrolytic Regeneration process The sulfuric acid in the above steps could be replaced with a non oxidizing strong acid such as Methanesulfonic acid MSA...

Страница 64: ...egenerated Suppressor Cleanup C Remake the eluent to be sure that the concentration is correct Be sure that chemicals of the required purity were used to make the eluent see Section 3 1 Chemical Purit...

Страница 65: ...For Research Use Only Not for Use in Diagnostic Procedures Figure 19 Effect of Air Bubbles on Baseline Dionex AERS 500 4 mm Recycle Eluent Mode In the above figure a bubble is released from ELUENT IN...

Страница 66: ...k Pressure Increases Over Time If the increased back pressure does not affect system performance no maintenance is necessary A Check the inlet frits on the guard and analytical column and replace them...

Страница 67: ...0 minutes with the membranes fully hydrated See the Caution Note in Section 3 2 Start Up If the suppressor continues to leak when operated within the proper back pressure range it must be replaced 5 9...

Страница 68: ...ever operated without regenerant flow When operating properly bubbles interspersed with liquid exiting the regenerant chamber indicates good flow Replace the suppressor if operation without flow is kn...

Страница 69: ...the Dionex AERS 500e this problem is caused when the ion exchange sites in the suppressor are converted from the hydronium form to the salt form They must be converted back to the hydronium form for...

Страница 70: ...or Higher resistance may indicate contamination of the suppressor For more information regarding monitoring the voltage see Document No 031841 02 Removal of Iron Contamination from Electrolytic Suppre...

Страница 71: ...ing in the AutoSuppression External Water Mode turn off the external water and disconnect the external water line from the suppressor REGEN IN port D Disconnect the liquid line from the suppressor ELU...

Страница 72: ...of the eluent In the AutoSuppression Recycle Mode the eluent leaving the conductivity cell is recycled through the regenerant chambers as the water supply This eliminates the need for an external rege...

Страница 73: ...5 2 0 48 190 AS11 HC 30 mM OH 0 38 1 5 29 112 60 mM OH 0 38 1 5 57 223 AS15 38 mM OH 0 3 1 2 29 113 40 mM OH 0 5 1 50 AS16 35 mM OH 0 25 1 0 22 87 55 mM OH 0 38 1 5 52 204 AS17 C 15 mM OH 0 25 1 0 10...

Страница 74: ...3 5 mM CO3 2 1 0 mM HCO3 0 3 1 2 50 50 AS14A 8 0 mM CO3 2 1 0 mM HCO3 0 5 1 1 0 50 50 AS22 4 5 mM CO3 2 1 4 mM HCO3 0 3 1 2 50 50 AS23 4 5 mM CO3 2 0 8 mM HCO3 0 25 1 0 50 50 AS10 80 mM OH 0 25 1 0 5...

Страница 75: ...centrations and flow rates of commonly used mobile phases used in anion separations and the optimum recommended current level to suppress the eluent The operation of the Dionex AERS 500 Carbonate requ...

Страница 76: ...he regenerant and has the ability to provide continuous suppression Table 18 20 list the eluent concentrations and flow rates of commonly used mobile phases used in cation separations and the optimum...

Страница 77: ...9 AcN 2 0 3 1 2 18 71 14 mM H2SO4 0 3 1 2 25 99 CS16 30 mM MSA 0 36 1 1 0 3 32 89 48 mM MSA 0 36 1 1 0 3 51 142 CS17 6 mM MSA 0 25 1 0 5 18 40 mM MSA 0 25 1 0 30 118 CS18 5 mM MSA 0 25 4 CS19 8 mM MSA...

Страница 78: ...M H2SO4 9 AcN 2 0 3 1 2 50 100 14 mM H2SO4 0 3 1 2 50 100 CS16 30 mM MSA 0 36 1 1 0 3 50 100 48 mM MSA 0 36 1 1 0 3 100 300 CS17 6 mM MSA 0 25 1 0 50 50 40 mM MSA 0 25 1 0 50 300 CS18 5 mM MSA 0 25 50...

Страница 79: ...A 2 Current Settings for Older Detectors On CD20 and ED40 detectors in Dionex DX 500 instruments the correct current is set by navigating to the SRS field in the Main menu and using the Select keys t...

Страница 80: ...he arrow keys to select Local and press Enter C In the Main or Detail screens navigate using the arrow keys to the field labeled SRS Set the current output level Increase or decrease the levels by usi...

Страница 81: ...Dionex RFC 30 power supply for the Dionex DX 300 instrument B 1 3 ERS Control for the Dionex DX 100 Model DX 1 03 The Dionex ERS 500 Dionex ERS 500e and Dionex ERS 500 Carbonate are not compatible wi...

Страница 82: ...The Dionex ERS 500 and Dionex ERS 500e are fully backwards compatible with all SRS power adapters and settings For optimal performance a Dionex SCC 10 suppressor current controller should be used in...

Страница 83: ...panel on the Dionex SRC 1 is located on the front of that module s cabinet LED indicators inform the operator of the system s operational status The Dionex SRC 1 has its own AC Power On Off switch to...

Страница 84: ...must be flowing to prevent an alarm state When the ERS Control unit is in shutdown mode after detecting a malfunction in the system an alarm message SRS Alarm will flash on the screen To determine the...

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