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Troubleshooting

Thermo Scientific

Product Manual for IonPac AS31 Columns

Page 38 of 45

155007-01

For Research Use Only. Not for use in diagnostic procedures.

Column contamination can lead to a loss of column capacity. This is because all of the ion

exchange sites will no longer be available for the sample ions. For example, polyvalent ions or

metals from the sample may concentrate on the column. Refer to

Section

6.5

“Column Cleanup

Procedure” for recommended column cleanup procedures.

Possible sources of column contamination are impurities in chemicals and in the deionized
water used for eluents or components of the sample matrix. Be especially careful to make
sure that the recommended chemicals are used. The deionized water should have a specific
resistance of 18.2 megohm-cm.

After cleaning the column, reinstall it in the system and let it equilibrate with eluent for about

30 minutes. The column is sufficiently equilibrated when consecutive injections of the

standard give reproducible retention times. The original column capacity should be restored

by this treatment, since the contaminants should be eluted from the column.

5.4.4

Loss of Front-End Resolution

If poor resolution or efficiency is observed for the peaks eluting near the system void volume

compared to the later eluting peaks, check the following:
A.

Eluent concentration: Incorrect eluent concentration may be the problem. Remake the eluent

as required for your application. Ensure that the water and chemicals used are of the required

purity. The eluent concentration maybe incorrect if the flow delivered to the eluent generator

cartridge is incorrect. Check pump flow rate.

Sample concentration and injection volume: Column overloading may be the problem.

Reduce the amount of sample ions being injected onto the analytical column by either diluting

the sample or injecting a smaller volume onto the column.

System plumbing: Improperly swept out volumes anywhere in the system prior to the guard

and analytical columns may be the problem. Reconnect components one at a time in the

system prior to the columns, and test for front-end resolution after every system change.

5.5

Spurious Peaks

In a system where peaks are observed where none are expected, both the column and the system

should be checked.
A.

The columns may be contaminated. If the samples contain an appreciable level of polyvalent

ions and the column is used with a weak eluent system, the retention times for the analytes

will then decrease and spurious, inefficient (broad) peaks can show up at unexpected times.

Clean the column as indicated in

Section

“Column Cleanup”.

The injection valve may need maintenance. When an injection valve is actuated, the

possibility of creating a baseline disturbance exists. This baseline upset can show up as a

peak of varying size and shape. This will occur when the injection valve needs to be cleaned

or serviced. Check to see that there are no restrictions in the tubing connected to the valve.

Also check the valve port faces for blockage and replace them if necessary. Refer to the valve

manual for troubleshooting and service procedures. Small baseline disturbances at the

beginning or at the end of the chromatogram can be overlooked so long as they do not

interfere with the quantification of the peaks of interest.

NOTE

Содержание Dionex IonPac AG31

Страница 1: ...For Research Use Only Not for use in diagnostic procedures 6 Dionex IonPac AS31 Columns 155007 Revision 01 December 2018 User Manual ...

Страница 2: ... Columns Page 2 of 45 155007 01 For Research Use Only Not for use in diagnostic procedures Product Manual for Dionex IonPac AS31 Analytical Column Analytical Column 2 250 mm Item 303147 Dionex IonPac AG31 Guard Column Guard Column 2 50 mm Item 303148 ...

Страница 3: ...ion 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 u...

Страница 4: ...y 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 injury Also used to identify a situation or practice that may seriously damage the instrument but will not cause injury Indicates information of general interest IMPORTANT Highlights information neces...

Страница 5: ...emical Requirements and Solvent Compatibility 15 3 5 Eluent Preparation 16 3 5 1 Manually Prepared Eluents 16 3 5 2 Making Eluents that Contain Solvents 16 3 6 Regenerant Preparation for the Thermo Scientific Dionex Chemically Regenerated Suppressor Dionex CRS 500 17 3 7 Recommendations for Method Development 17 4 Example Applications 18 4 1 Recommendations for Optimum System Performance 18 4 2 Is...

Страница 6: ...ples 32 5 2 High Background 32 5 2 1 Preparation of Eluents 32 5 2 2 A Contaminated Trap Column 32 5 2 3 Contaminated Dionex CR ATC 500 Column 32 5 2 4 A Contaminated Guard or Analytical Column 33 5 2 5 Contaminated Hardware 33 5 2 6 A Contaminated Suppressor 33 5 2 7 Contaminated Regenerant Water 33 5 3 Inconsistent Retention Times 33 5 3 1 Drifting to Shorter Retention Time 34 5 3 2 Drifting to ...

Страница 7: ...Operation Pressures 39 6 2 Column Start Up 39 6 3 Column Storage 39 6 4 Chemical Purity Requirements 39 6 4 1 Inorganic Chemicals 40 6 4 2 Deionized Water 40 6 4 3 Solvents 40 6 5 Column Cleanup 41 6 5 1 Choosing the Appropriate Cleanup Solution 42 6 5 2 Column Cleanup Procedure 43 7 Quality Assurance Report 44 8 Additional Information 45 8 1 General Information on PEEK Tubing 45 ...

Страница 8: ...ermination or other environmental ions in relatively high matrix samples The high capacity and compatibility of this column with mass spectroscopy makes it useful with Reagent Free Ion Chromatography RFICTM systems for several environmental ions The Dionex IonPac AS31 is compatible with pH 0 14 eluents and samples The Dionex IonPac AS31 can be used with any suppressible ionic eluent that does not ...

Страница 9: ...ac AS31 2 mm Analytical column 3000 20 68 0 30 0 40 Dionex IonPac AG31 2 mm Guard column 200 1 38 0 30 0 40 Dionex IonPac AG31 and AS31 2 mm columns 3200 22 06 0 30 0 40 Note 1MPa 145 04 psi b Total backpressure at standard flow rates c In all cases flow rate should not result in pressures over 5 000 psi For assistance visit Unity Lab Services online at www unitylabservices com From the U S call t...

Страница 10: ...rmo Scientific Dionex High Pressure Ion Chromatography Systems A minimum of a Dionex High Pressure Ion Chromatography HPIC System is recommended when running Dionex IonPac AS31 columns due to the higher backpressures generated at typical operational flow rates Systems should have the capability to operate up to at least 5000 psi Standard IC systems with an upper limit of 3000 psi are insufficient ...

Страница 11: ...esolution Minimize the lengths of all connecting tubing and remove all unnecessary switching valves and couplers 2 3 Column Start Up The column is shipped using sodium bicarbonate as the storage solution Prepare the eluent shown on the Quality Assurance Report To remove the storage solution flush the column to waste with the 80 mM KOH eluent for at least 45 minutes and then 15 minutes with QAR elu...

Страница 12: ...y 1 5 under isocratic test conditions Replacing the guard column at the first sign of peak efficiency loss or decreased retention time will prolong the life of the analytical column 2 6 Trap Columns For gradient operation a trap column is installed between the gradient pump and the injection valve and takes the place of the gradient mixer if present The trap column is filled with high capacity ion...

Страница 13: ...ation work with Dionex IonPac columns A pump is used to load the sample onto the concentrator column in the OPPOSITE direction of the eluent flow Once concentration is complete the eluent flow is then directed through the concentrator to the analytical column When using concentration techniques care should be taken not to overload the concentrator column by concentrating an excessive amount of sam...

Страница 14: ...H Eluent Source Dionex EGC 500 KOH cartridge with Dionex CR ATC 500 Dionex ICS 5000 or Dionex CR ATC 600 Dionex ICS 6000 Eluent Flow Rate 0 30 mL min Temperature 15 ºC Suppressor Dionex ADRS 600 Anion Dynamically Regenerated Suppressor AutoSuppression External Water Mode Expected Background Conductivity 1 µS Long term Storage Solution 1 week 100 mM sodium bicarbonate Short term Storage Solution 1 ...

Страница 15: ...si 34 47MPa 3 3 Quality Assurance Reports Each column is qualified to ensure it meets specifications Example copies of these Quality Assurance Reports QARs can be found in Section 7 The QAR supplied with the column should be used as a guide to ensure system performance 3 4 Chemical Requirements and Solvent Compatibility Chemical purity can influence separation performance Only chemicals of the hig...

Страница 16: ... an eluent of 40 acetonitrile prepare the eluent by adding 400 mL of acetonitrile to an eluent reservoir Then add 600 mL of deionized water or eluent concentrate to the acetonitrile in the reservoir Using this procedure to mix solvents with water will ensure that a consistent true volume volume eluent is obtained Premixing water with solvent will minimize the possibility of outgassing When purging...

Страница 17: ...uilibration time from one run to the next Potassium hydroxide is converted to water in the suppressor making it the preferred source of eluent As long as the capacity of the suppressor is not exceeded the eluent hydroxide concentration has little effect on background conductivity For example a gradient run could begin at 17 mM KOH and end at 85 mM KOH with a resulting total baseline change of 1 to...

Страница 18: ... conductivity during the run as well as a fast equilibration time from one run to the next The best choice for an eluent is potassium hydroxide as it is converted to water in the suppressor As long as the capacity of the suppressor is not exceeded the eluent hydroxide concentration has little effect on background conductivity For example a gradient run can begin at 17 mM KOH and end at 85 mM KOH w...

Страница 19: ...ducible resolution and retention Note that the Dionex IonPac AG31 guard column is packed with a microporous resin of proportionally lower capacity and contributes approximately 1 5 increase in retention time when placed in line prior to the analytical column under isocratic test conditions Figure 1 Dionex IonPac AS31 With and Without Dionex IonPac AG31 Guard Column Column See Chromatogram Eluent 2...

Страница 20: ...tive to monovalent anions fluoride chloride bromide and nitrate when temperature is changed from 15ºC to 30ºC Figure 2 Effect of Temperature on Dionex IonPac AS31 Selectivity Column Dionex IonPac AG31 AS31 2mm Eluent 24 mM KOH Eluent Source Dionex EGC 500 KOH cartridge Flow Rate 0 30 mL min Inj Volume 2 5 µL Temperature See Chromatogram Detection SuppressedConductivity Dionex ADRS 600 2 mm AutoSup...

Страница 21: ... resolution Figure 3 Separation of Various Inorganic and Organic Anions Using the Dionex IonPac AS31 Column Column Dionex IonPac AG31 AS31 2mm Eluent 15 mM KOH from 0 to 6 minutes 15 70 mM KOH from 6 to 26 minutes Eluent Source Dionex EGC 500 KOH cartridge Flow Rate 0 30 mL min Inj Volume 2 5 µL Temperature 15 C Detection SuppressedConductivity Dionex ADRS 600 2 mm AutoSuppression recycle mode Pea...

Страница 22: ...7 Laboratory Synthetic Sample Matrix The following chromatograms demonstrate the Dionex IonPac AS31 column s selectivity and capacity using IC method and EPA Method 557 LSSM matrix Figure 4 Analysis of Dalapon Bromate and Haloacetic Acids in LSSM EPA Method 557 Matrix Using the Dionex IonPac AG31 and AS31 Columns Full Scale Expanded Scale 0 5 10 15 20 25 30 35 250 0 2 500 1 2 3 4 5 6 7 8 9 10 11 1...

Страница 23: ...mn The following chromatograms show the analyses of municipal drinking water with and without a spike of 9HAAs Figure 5 Analysis of Municipal Drinking Water Spiked with Nine Haloacetic Acids Using the Dionex IonPac AG31 AS31 Columns Municipal Drinking Water Municipal Drinking Water Spiked with 0 5 ppm of 9 HAAs 0 5 10 15 20 25 30 35 40 0 5 5 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 Minutes µ...

Страница 24: ...ved highly accurate mass values allowing resolution of molecular ions differing in m z by 0 032 Bromate and DCAA With minor In Source fragmentation we observed diagnostic fragments for all components The following table can provide initial guidance on setting up time windows for matrix diversion based on the retention times of chloride carbonate sulfate and nitrate The recommendations below can be...

Страница 25: ... 2 00 KV Funnel RF 40 0 Timed Events Time KOH Divert Valve 0 5 Begin 17 0 Eluent to Waste 0 0 17 0 4 0 17 0 Eluent to MS 7 0 17 0 8 6 Eluent to Waste 11 1 Eluent to MS 18 0 85 0 18 73 Eluent to Waste 21 73 Eluent to MS 40 0 85 0 Eluent to Waste 40 1 17 0 47 0 End Full Scan 50 300 m z 60000 Res Max IT 330 ms during non SIM segments SIM Segments Time Range min Analyte SIM m z ID of m z i Isotope Dia...

Страница 26: ...4 6 59E4 4 Dalapon 140 951 140 952 2 71E4 5 DCAA 126 935 126 936 8 58E4 6 BCAA 172 882 172 884 6 99E4 7 DBAA 216 832 216 834 6 66E4 8 TCAA 118 904 118 905 4 91E4 9 BDCAA 162 854 162 855 3 11E4 10 DBCAA 206 803 206 805 2 37E4 11 TBAA 250 752 250 755 9 03E3 1 2 3 4 5 6 7 8 9 10 11 5 10 15 20 25 30 35 40 Minutes 0 100 Relative Abundance Peak Mass Range m z Intensity 1 MCAA 92 975 92 976 9 59E4 2 MBAA...

Страница 27: ...cording to the eluent generator installation guide for low flow rate operation The column and suppressor are plumbed in the normal configuration Referring to the Figure 9 above the column outlet is connected to the suppressor For MS detection the suppressor is operated in the external water mode and regen water is provided via the auxiliary pump at 0 3 mL min The matrix diversion valve switches th...

Страница 28: ...s spectrometer source may occasionally require physical cleaning followed by several hours of vacuum pumping to regain pristine performance Note that the IC eluent line should not be connected to the MS inlet until the background conductivity is below 3 µS If an ICS 5000 or ICS 6000 is used any of the 6 or 10 port valves in the automation manager AM module can be used for matrix diversion Makeup D...

Страница 29: ...s and Filter Samples 5 1 2 5 1 3 5 1 4 Other System Components Unplug Replace Filter Eluents and Samples Component Manual High Background Conductivity Contaminated Eluents Remake Eluents 5 2 1 Contaminated Trap Column Clean or Replace Trap Column 5 2 2 5 2 3 Contaminated Guard or Analytical Column Clean or Replace Guard and Analytical Column 5 2 4 Contaminated Suppressor Clean or Replace Suppresso...

Страница 30: ...alytical Column when using the test chromatogram conditions should be less than 3800 psi If the system pressure at the standard flow rate is higher than the maximum operational pressure for the system it is advisable to determine the cause of the high system pressure A Make sure that the pump is set to the correct eluent flow rate Higher than recommended eluent flow rates will cause higher pressur...

Страница 31: ...r seal between the end of the column tube and the bed support assembly If this is the case additional tightening may not seal the column but instead damage the column tube or the end fitting Replacement of the 2 mm outlet bed support is not recommended A Disconnect the column from the system B Carefully unscrew the inlet top column fitting Use two open end wrenches C Remove the bed support Turn th...

Страница 32: ...ion Columns Eluent Expected Background Conductivity 17 mM KOH 0 5 0 8 µS 85 mM KOH 0 8 1 5 µS 60 mM KOH 15 Methanol 1 3 µS 5 2 1 Preparation of Eluents A Make sure that the eluents prepared manually and the regenerant are made correctly B Make sure that the eluents are made from chemicals with the recommended purity C Make sure that the deionized water used to prepare the reagents has a specific r...

Страница 33: ...or conductivity cell calibration by injecting deionized water directly into it See the appropriate manual for details 5 2 6 A Contaminated Suppressor If the above items have been checked and the problem persists the Dionex Dynamically Regenerated Suppressor or the Dionex Chemically Regenerated Suppressor is probably causing the problem For details on Dionex Dynamically Regenerated Suppressor opera...

Страница 34: ...luents are prepared manually poorly mixed eluent can cause longer retention time Remake eluent C A pump losing prime will cause retention time drift Prime the pump Refer to the Operator s Manual for correct pump operation D A leaking pump will cause longer retention times Check the pump flow Refer to the Operator s Manual for correct pump operation E Changes in temperature will also cause peaks to...

Страница 35: ...to be tailored for a particular application where selectivity resolution and total run time are optimized Be aware that poor peak resolution can be due to any or all of the following factors 5 4 1 Loss of Column Efficiency When chromatographic efficiency is lost peak resolution may decrease to an unacceptable level as the peaks broaden A Check to see if headspace has developed in the guard or anal...

Страница 36: ...ct and incorrect placement of the ferrule and fitting bolt on the tubing Figure 11 Tailing Peaks Caused by Incorrectly Installed Tubing Fittings Figure 12 Correct and Incorrect Ferrule and Fitting Bolt Placement for Tubing Connections D Check for leaks This can be done by visual inspection at elevated flow rates Use of a paper towel or KimWipe touched to connection will show noticeable wetness eve...

Страница 37: ...vated flow rate or eluent concentration A During gradient analysis the column must be equilibrated with the starting eluent prior to analysis The time required is dependent on the difference in concentration between the start and the end of the gradient If the ion concentration on the column is higher than the starting eluent concentration then peaks may elute early or with inconsistent retention ...

Страница 38: ... incorrect if the flow delivered to the eluent generator cartridge is incorrect Check pump flow rate B Sample concentration and injection volume Column overloading may be the problem Reduce the amount of sample ions being injected onto the analytical column by either diluting the sample or injecting a smaller volume onto the column C System plumbing Improperly swept out volumes anywhere in the sys...

Страница 39: ...ndard give reproducible retention times IMPORTANT When making any tubing connections first turn off the pump This will avoid any slippage of the ferrule under high pressure conditions 6 3 Column Storage For short term storage 1 week use eluent for long term storage 1 week store in eluent in a refrigerator or use 100 mM sodium bicarbonate for the column storage solution when stored at room temperat...

Страница 40: ...vents can be added to the ionic eluents used with Dionex IonPac columns to modify the ion exchange process or improve sample solubility The solvents used must be free of ionic impurities However since most manufacturers of solvents do not test for ionic impurities it is important that the highest grade of solvents available be used Currently several manufacturers are making ultrahigh purity solven...

Страница 41: ...n bed and irreversibly damage the performance of the column High viscosity mixing zones can be created between two eluents having solvents with a very high energy of mixing High pressure zones in the column can be created by pumping successive eluents through the column that are not miscible that have eluent components in one eluent that will precipitate out in the other eluent or by using an acid...

Страница 42: ...ove a variety of metals If after acid treatment the chromatography still suggests metal contamination treatment with chelating acids such as 0 2 M oxalic acid is recommended Ionic and Hydrophobic Contamination Concentrated acid solutions such as 1 to 3 M HCl can be used with compatible organic solvents to remove contamination that is ionic and hydrophobic The acid suppresses ionization and ion exc...

Страница 43: ...ch column separately C For aqueous cleaning solutions set the pump flow rate to 0 25 mL min for a Dionex IonPac 2 mm Analytical or Guard Column D For cleaning solutions containing organic solvents set the pump flow rate 0 12 mL min for a Dionex IonPac 2 mm Analytical or Guard Column E Rinse the column for 10 minutes with deionized water before pumping the chosen cleanup solution over the column or...

Страница 44: ...7 Quality Assurance Report Thermo Scientific Product Manual for IonPac AS31 Columns Page 44 of 45 155007 01 For Research Use Only Not for use in diagnostic procedures 7 Quality Assurance Report ...

Страница 45: ...e should be taken to ensure the correct i d is being used to avoid problems caused by sample dispersion Table 8 Tubing Back Pressures Color Part Number I D inch I D cm Volume mL ft Back Pressure psi ft at 1 mL min Back Pressure psi ft at 0 25 mL min Back Pressure psi cm at 1mL min Green 044777 0 030 0 076 0 137 0 086 0 021 0 003 Orange 042855 0 020 0 051 0 061 0 435 0 109 0 015 Blue 049714 0 013 0...

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