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Product Manual for IonPac CS16

Page 50 of 65

SECTION 6 – TROUBLESHOOTING GUIDE

The purpose of the Troubleshooting Guide is to help you solve operating problems that may arise while using IonPac CS16
columns. For more information on problems that originate with the Ion Chromatograph (IC) or suppressor, refer to the
Troubleshooting Guide in the appropriate operator’s manual. If you cannot solve the problem on your own, contact the
Dionex North America Technical Call Center at 1-800-DIONEX-0 (1-800-346-6390) or the nearest Dionex Office (see,
“Dionex Worldwide Offices”).

Table 8

CS16/CG16 Troubleshooting Summary

Observation Cause

Action

Reference

Section

High Back Pressure

Unknown component

Isolate blockage

6.1.1

Plugged column bed supports

Replace bed supports

6.1.2

Plugged system hardware

Unplug, Replace

Component manual

High Background
Conductivity and/or High
Noise

Improper Suppressor
Operation

CSRS, CCES or CAES Not Suppressing

Check current

6.5 A, Component manual

Check REGEN OUT flow

6.5 A, Component manual

Check for leaks

6.5 A, Component manual

CMMS not suppressing

Check regenerant

6.5 C, Component manual

Check AutoRegen cartridge

6.5 C, Component manual

Air bubble trapped in CSRS or CAES

Remove bubble by loosening
fittings

6.4

Contamination

Bad eluents

Remake eluents

6.2, 6.4

Contaminated column

Clean column

6.3.1, 7.4

Contaminated suppressor

Clean suppressor

6.3.1 A, 6.5, Component manual

Hardware Operation

Proportioning valve

Service valve

Component manual

Poor Peak Resolution

Poor Efficiency

Large system void volumes

Replumb system

6.6.3 B, Component manual

Sluggish injection valve

Service valve

6.6.3 A, Component manual

Contaminated or deformed bed support

Replace bed support

6.1.2

Column headspace

Replace column

6.6.1 A

Column overloading

Reduce sample size

5.18

Low sample pH

Reduce sample size, Dilute
Sample, Use OnGuard II A

5.17

Fronting Peaks

Low sample pH

Reduce sample size, Dilute
Sample, Use OnGuard II A

5.17

Column overload

Reduce sample size

5.18

Contaminated or deformed bed support

Replace bed support

6.1.2

Column headspace

Replace column

6.6.1 A

Tailing Peaks

Contaminated suppressor

Clean suppressor

6.3.1 A, 6.5, Component Manual

Column overloading

Reduce sample size

5.18

Short Retention

Flow rate too fast

Recalibrate pump

6.6.2 A

Times

First peaks elute too fast

Equilibrate to first eluent

6.6.3 A

Bad eluents

Remake eluents

6.6.2 B

Column contamination

Clean column

6.62 C

Spurious Peaks

Column contamination

Pretreat samples

6.3.1, 6.7 A, 6.7 B

Sluggish injection valve

Service valve

6.7 C, Component Manual

Poor Qualifications of
Divalents

Sample loop contamination

Flush, replace

6.3.2

Document No. 031747-05

December 2010

Содержание IonPac CG16

Страница 1: ... 05 For new orders of the following parts discussed in this manual please use the updated part numbers listed below Part Old Part Number in this manual Updated Part Number to use for new orders PROD COL IP CS16 5X250MM 057573 079805 PROD COL IP CG16 3X50MM 059595 079931 ...

Страница 2: ...IonPac CS16 IonPac CG16 for ...

Страница 3: ... x 50 mm P N 057574 3 x 50 mm P N 059595 0 5 x 50 mm P N 075402 IONPAC CS16 ANALYTICAL COLUMN 5 x 250 mm P N 057573 3 x 250 mm P N 059596 0 5 x 250 mm P N 075401 2010 Dionex Corporation Document No 031747 Revision 05 December 2010 Document No 031747 05 2010 Dionex Corporation December 2010 ...

Страница 4: ...Suppressor and Cation Capillary Electrolytic Suppressor Requirements 14 3 9 Cation Atlas Electrolytic Suppressor Requirements 14 3 10 Cation MicroMembrane Suppressor Requirements 14 3 11 Using Displacement Chemical Regeneration DCR with the Chemical Suppression Mode 14 3 12 Using AutoRegen with the Chemical Suppression Mode 15 3 13 Detector Requirements 15 SECTION 4 OPERATION 16 4 1 General Operat...

Страница 5: ...ganese at 60 C 40 5 16 Sample pH at 40 C 41 5 17 Linear Working Range at 40 C 42 5 18 Step Change Elution of Ethanolamine and the Common Cations on the IonPac CS16 3 mm 43 5 19 Diverse Concentration Ratios of Ammonium to Ethanolamine on the IonPac CS16 3 mm at 40 C 44 5 20 Gradient Elution of Ethanolamine Hydrazine and the Common Cations 45 5 21 Gradient Elution of Common Cations and Amines at 60 ...

Страница 6: ... Particle Diameter µm Substratea X linking Capacity Column meq column Functional Group Hydrophobicity CS16 5 x 250 mm 5 5 55 8 4 Carboxylic acid Medium CG16 5 x 50 mm 5 5 55 1 7 Carboxylic acid Medium CS16 3 x 250 mm 5 5 55 3 0 Carboxylic acid Medium CG16 3 x 50 mm 5 5 55 0 6 Carboxylic acid Medium CS16 0 5 x 250 mm 5 5 55 0 084 Carboxylic acid Medium CG16 0 5 x 50 mm 5 5 55 0 017 Carboxylic acid ...

Страница 7: ...ttings for use with ferrule bolt liquid line fittings If you have an Ion Chromatograph with Tefzel liquid lines having 1 4 28 ThermoFlare fittings it will be necessary to obtain one or more Tefzel liquid lines with a PEEK bolt and ferrule fitting on one end and a 1 4 28 ThermoFlare fitting on the other end See Dionex Liquid Line Fittings for detailed instructions on purchasing or making these line...

Страница 8: ... EG40 P N 053920 or EG50 P N 053922 for gradient applications is highly recommended for minimum baseline change when performing eluent step changes or gradients Use the GP40 GP50 IP20 IP25 in Standard Bore Configuration The GPM 3 Gradient Mixer should be used for gradient analysis on systems other than the GP50 and IP25 The GP40 has an active mixer NOTE Use of an EG40 P N 053920 or EG50 P N 053922...

Страница 9: ...ack Pressure Psi ft at 1 mL 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 0 033 0 026 2 437 0 609 0 081 Black 042690 0 010 0 025 0 015 6 960 1 740 0 232 Red 044221 0 005 0 013 0 004 111 360 27 840 3 712 Yellow 049715 0 003 0 008 0 001 859 259 214 815 28 642 Document No 031747 05 2010 Dionex Corporation December 2010 ...

Страница 10: ...signed to be run on any Dionex Ion Chromatograph equipped with suppressed conductivity detection Gradient or isocratic methods should be performed on a system having a gradient pump configured for standard bore operation For alternate detection than conductivity refer to Section 2 3 1 4 Installation of the Capillary Column 1 Before installing the new separator column tear off the column label and ...

Страница 11: ...15 mm 4 53 in 072189 Guard column inlet to injection valve Precision cut 0 062 mm 0 0025 in ID PEEK tubing blue 75 mm 2 93 in 074603 35 mm guard column outlet to 150 mm separator column inlet Precision cut 0 062 mm 0 0025 in ID PEEK tubing blue labeled VALVE PORT 3 210 mm 8 27 in 072187 Separator column inlet to injection valve if a guard column is not present 0 25 mm 0 010 in ID PEEK tubing black...

Страница 12: ...rd Column Separator Column 210 mm 4 5 in Precision Cut Tubing P N 072187 use with any length seperator column 1 2 1 2 Figure 4 Tubing Connections for Separator Column Only 5 Lift up the lid of the column cartridge to open it 6 Remove the fitting plug from the outlet fitting on the separator column Orient the fitting with a flat side up see Figure 5 and push the fitting into the opening at the fron...

Страница 13: ...mn cartridge 9 Route the guard column inlet tubing if used or the separator column inlet tubing through the clip on the top edge of the column cartridge lid 10 Close the lid you should hear a click and route the tubing into the slot on the front of the column cartridge see Figure 6 If the columns are installed correctly the cartridge lid snaps closed easily If the lid does not close easily do not ...

Страница 14: ...ysis To install the CTC complete the following steps A Remove the Gradient Mixer It is installed between the gradient pump pressure transducer and the injection valve B Connect the gradient pump directly to the CTC Connect a waste line to the CTC outlet and direct the line to a waste container C Flush the CTC For the CTC 1 use 200 mL of a 10x eluent concentrate of the strongest eluent required by ...

Страница 15: ...ueous sample matrix This can be accomplished by concentrating large volumes of the sample onto a concentrator column and then using this column in place of the sample loop The sample should be pumped into the concentrator column in the OPPOSITE direction of the eluent flow otherwise the chromatography will be compromised This process concentrates all cationic analyte species onto the trace cation ...

Страница 16: ... use TBAOH as regenerant and with no current applied to the CSRS 300 suppressor When the oven is operated at 40 C the suppressor should be placed outside the oven If you are installing an IonPac CS16 5 mm Analytical Column use a CSRS 300 4 mm P N 053948 If you are installing an IonPac CS16 3 mm Analytical Column use a CSRS 300 2 mm P N 053949 If you are installing an IonPac CS16 0 5 mm Capillary C...

Страница 17: ...nt This results in slowly increasing background conductivity The rate at which the background conductivity increases versus the required analysis sensitivity will determine how often the regenerant must be changed It is not necessary to change the AutoRegen Regenerant Cartridge until it is completely expended Use Dionex Cation Regenerant Solution TBAOH 0 1 M tetrabutylammonium hydroxide P N 039602...

Страница 18: ...Background Conductivity 3 µS Storage Solution Eluent 4 2 Operating Precautions IonPac CS16 Operation Precautions Operate below 4 000 psi 27 57 MPa Filter and Degas Eluents Filter Samples Do not use this column with alcohols CAUTION 4 3 Chemical Purity Requirements Reliable consistent and accurate results require eluents free of ionic impurities Chemicals solvents and deionized water used to prepar...

Страница 19: ... breathing the vapors Always use these reagents in a fume hood Wear gloves and goggles 4 4 1 1 0 N Methanesulfonic Acid MSA Stock Solution A 1 0 N methanesulfonic acid stock solution can be prepared as follows A Weigh out 96 10 g of methanesulfonic acid MSA 99 P N 033478 B Carefully add this amount to a 1 liter volumetric flask containing about 500 mL of deionized water C Dilute to the mark and mi...

Страница 20: ...ultrahigh purity solvents that are compatible for HPLC and spectrophotometric applications These ultrahigh purity solvents will usually ensure that your chromatography is not affected by ionic impurities in the solvent Currently at Dionex we have obtained consistent results using High Purity Solvents manufactured by Burdick and Jackson and Optima Solvents by Fisher Scientific When using a solvent ...

Страница 21: ...6 Page 19 of 65 Table 7 HPLC Solvents for Use with IonPac CS16 Columns Solvent Maximum Operating Concentration Acetonitrile 100 Methanol 0 2 Propanol 0 Tetrahydrofuran 20 Document No 031747 05 2010 Dionex Corporation December 2010 ...

Страница 22: ...nt containing only 5 of the current solvent type Exchange this eluent for an eluent with 5 of the new solvent type and then equilibrate the column and allow the system to stabilize approximately 10 minutes Next run a 15 minute gradient from 5 of the new solvent type to the highest percentage that will be used during the new analysis protocol Properly equilibrate the column when changing to a solve...

Страница 23: ... made from high purity reagents and deionized water All water used in the preparation of eluents should be degassed deionized water For chemical purity requirements see Section 4 3 Chemical Purity Requirements After running synthetic standards to calibrate your system you may find that real sample matrices foul your columns For this reason it is always advisable to use a guard column to protect th...

Страница 24: ...in Temperature 40 C Suppressor Cation Self Regenerating Suppressor 300 4 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent 0 5 1 0 1 5 2 0 2 5 0 0 2 0 4 0 6 0 8 1 0 1 2 1 4 1 6 1 8 5 4 6 1 3 2 0 µS 1 6 10 0 15 Minutes 5 ...

Страница 25: ...Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent 0 5 10 15 20 25 Minutes 0 16 1 99 µS 1 2 3 4 5 6 Analyte mg L 1 Lithium 0 05 2 Sodium 0 20 3 Ammonium 0 25 4 Potassium 0 50 5 Magnesium 0 25 6 Calcium 0 50 where 1 mg L 1 ppm Figure 8 IonPac CS16 3 mm Production ...

Страница 26: ...Eluent Flow Rate 1 0 mL min Temperature 40 C Suppressor Cation Self Regenerating Suppressor 300 4 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent 0 5 1 0 1 5 2 0 2 5 1 0 1 2 1 4 1 6 1 8 2 0 5 4 6 1 3 2 1 0 µS 2 0 10 0 ...

Страница 27: ...Suppressor CSRS 300 2 mm or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 0 5 µS Storage Solution Eluent 0 5 10 15 20 25 30 35 Minutes 0 10 1 90 µS 3 1 2 4 5 6 Analyte mg L 1 Lithium 0 05 2 Sodium 0 20 3 Ammonium 0 25 4 Potassium 0 50 5 Magnesium 0 25 6 Calcium 0 50 where 1 mg L 1 p...

Страница 28: ...5 µL Loop Eluent 48 mM Methanesulfonic acid MSA Eluent Flow Rate 1 0 mL min Temperature 40 C SRS Suppressor Cation Self Regenerating Suppressor 300 4 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent Analyte mg L 1 Lithi...

Страница 29: ...iving to room temperature fluctuations as shown in the following section Column IonPac CS16 5 mm Analytical Column no guard Sample Volume 25 µL Loop Eluent See Chromatogram Eluent Flow Rate 1 0 mL min Temperature Room Temperature approximately 22 C Suppressor Cation Self Regenerating Suppressor 300 4 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm...

Страница 30: ...Self Regenerating Suppressor 300 2 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent Eluent 38 mM Methanesulfonic acid MSA 22 C 0 5 10 15 20 0 26 2 96 6 18 9 40 1 2 3 4 5 6 Analyte mg L 1 Lithium 0 5 2 Sodium 2 0 3 Ammon...

Страница 31: ...r magnesium a divalent Column IonPac CS16 3 mm Analytical Column no guard Sample Volume 25 µL Loop Eluent 36 mM Methanesulfonic acid MSA Eluent Source EG40 Eluent Flow Rate 0 5 mL min Temperature 60 C SRS Suppressor Cation Self Regenerating Suppressor 300 2 mm in AutoSuppression Recycle Mode suppressor placed outside the oven or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Rege...

Страница 32: ...Flow Rate 1 0 mL min Temperature 40 C SRS Suppressor Cation Self Regenerating Suppressor 300 4 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent 0 5 1 0 1 5 2 0 2 5 0 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 7 5 4 6 1 3 2 0 µS 8 ...

Страница 33: ...mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent Figure 15a 0 2 4 6 8 1 0 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0 3 0 0 3 2 1 2 0 20 µS 0 32 8 0 Minutes 2 4 6 10 A Analytes mg L ppm 1 Sodium 100 00 2 Ammonium 0 01 0 2 4 6 8 1 0 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0 3 0 0 3 2 1 2 0 20 µS 0 32 8 0 Minutes 2 4 6 10 B Analytes mg L...

Страница 34: ...ressor Cation Self Regenerating Suppressor 300 2 mm in AutoSuppression Recycle Mode with CTC 1 between CELL OUT and REGEN IN ports or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent 0 2 4 6 8 10 0 360 0 420 0 480 0 540 2 A Analytes mg L ppm 1 Sodium 100 00...

Страница 35: ...o guard Sample Volume 25 µL Loop Trap Column CTC 1 is placed between the CELL OUT and the REGEN IN ports Eluent 30 mM Methanesulfonic acid MSA Eluent Flow Rate 1 0 mL min Temperature 40 C SRS Suppressor Cation Self Regenerating Suppressor 300 4 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Rege...

Страница 36: ...ng Suppressor 300 4 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent 48 mM Methanesulfonic acid MSA 0 5 1 0 1 5 2 0 2 5 0 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 1 0 5 4 6 3 1 2 0 1 µS 1 0 10 0 15 Minutes 5 20 25 Analyte mg L...

Страница 37: ...olumn no guard Sample Volume 25 µL Loop Sample Dilution 0 5 100 Eluent 30 mM Methanesulfonic acid MSA Eluent Flow Rate 1 0 mL min Temperature 40 C SRS Suppressor Cation Self Regenerating Suppressor 300 4 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conducti...

Страница 38: ...uppressor Cation Self Regenerating Suppressor 300 4 mm in AutoSuppression Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 4 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent 28 mM Methanesulfonic acid MSA 0 5 1 0 1 5 2 0 2 5 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 1 0 1 1 9 8 7 6 0 2 µS 1 0 10 0 15 ...

Страница 39: ...d outside of the column oven Column IonPac CS16 3 mm Analytical Column no guard Sample Volume 25 µL Loop Eluent 20 mM Methanesulfonic acid MSA Eluent Flow Rate 0 5 mL min Temperature 60 C SRS Suppressor Cation Self Regenerating Suppressor 300 2 mm in AutoSuppression Recycle Mode Suppressor placed outside oven or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Regenerant TBAOH MMS ...

Страница 40: ...s used in the eluent recycle mode Note that the suppressor is placed outside the chromatography oven when temperatures exceed 40 C as they do here Column IonPac CS16 3 mm Analytical Column no guard Eluent 6 mM MSA gradient from 0 to 13 min to 8 mM MSA gradient from 13 to 25 min to 55 mM MSA Eluent Source EG40 Flow Rate 0 5 mL min Inj Volume 25 µL Detection Suppressed conductivity CSRS 300 2 mm out...

Страница 41: ...t 6 mM MSA gradient from 0 to 13 minutes to 8 mM MSA gradient from 13 to 25 minutes to 55 mM MSA Eluent Flow Rate 0 5 mL min Temperature 60 C SRS Suppressor Cation Self Regenerating Suppressor 300 2 mm in AutoSuppression Recycle Mode Suppressor placed outside oven or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Ex...

Страница 42: ...le Volume 25 µL Loop Eluent 26 mM Methanesulfonic acid MSA Eluent Source EG40 Eluent Flow Rate 0 36 mL min Temperature 60 C SRS Suppressor Cation Self Regenerating Suppressor 300 2 mm in AutoSuppression Recycle Mode placed outside oven or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivit...

Страница 43: ...f lower pH can be pre treated before injection with an OnGuard II A cartridge in the bicarbonate form Anions in the sample will be exchanged for the bicarbonate in the OnGuard resin The bicarbonate ions neutralize the hydronium ion in the sample Column IonPac CS16 5 mm Analytical Column no guard Analyte mg L 1 Lithium 0 1 2 Sodium 0 4 3 Ammonium 0 5 4 Potassium 1 0 5 Magnesium 0 5 6 Calcium 1 0 Sa...

Страница 44: ...ing the highest calibration point The large resolution among all peaks permits quantitation even when efficiency symmetry are poor due to overloading Quantification using peak areas is possible from low ppb to 500 ppm concentration Column IonPac CG16 5 mm Guard Column CS16 5 mm Analytical Column Sample Volume 25 µL Loop Eluent 30 mM Methanesulfonic acid MSA Eluent Flow Rate 1 0 mL min Temperature ...

Страница 45: ... 5 mM Methanesulfonic acid MSA step to 56 mM MSA at 17 min Eluent Flow Rate 0 36 mL min Temperature 40 C SRS Suppressor Cation Self Regenerating Suppressor 300 2 mm in AutoSuppression Recycle Mode CTC 1 P N 040192 between CELL OUT and REGEN IN ports or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Backgrou...

Страница 46: ...enerating Suppressor 300 2 mm in AutoSuppression Recycle Mode CTC 1 P N 040192 between CELL OUT and REGEN IN ports or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent 0 5 10 15 20 0 300 0 500 0 700 µS 1 2 A Analyte µg L 1 Ammonium 40 2 Ethanolamine 5000 1 M...

Страница 47: ...rature 40 C SRS Suppressor Cation Self Regenerating Suppressor 300 2 mm in AutoSuppression Recycle Mode CTC 1 P N 043132 between CELL OUT and REGEN IN ports or MMS Suppressor Cation MicroMembrane Suppressor CMMS 300 2 mm MMS Regenerant TBAOH MMS Mode Displacement Chemical Regeneration DCR Expected Background Conductivity 2 µS Storage Solution Eluent 0 5 10 15 20 25 30 35 40 0 0 88 1 75 2 63 3 50 µ...

Страница 48: ...um 500 000 3 Ammonium 25 4 Ethanolamine 50 5 Hydrazine 200 6 Potassium 50 7 Magnesium 25 8 Calcium 50 Minutes With this same gradient condition 20 000 1 concentration ratio of Na to NH4 ammonium can be determined Figure 29 Continued Gradient Elution of Ethanolamine Hydrazine and the Common Cations Document No 031747 05 2010 Dionex Corporation December 2010 ...

Страница 49: ...t contained no organic solvent so the suppressor was used in the eluent recycle mode The suppressor was placed outside the chromatographic oven as the temperature exceeded 40 C Column IonPac CS16 3 mm Analytical Column no guard Eluent 6 mM MSA gradient from 0 to 13 min to 8 mM MSA gradient from 13 to 25 min to 55 mM MSA gradient from 25 to 30 min to 60 mM MSA Eluent Source EG40 Flow Rate 0 5 mL mi...

Страница 50: ...n the eluent recycle mode as there is no organic solvent used however the suppressor must be placed outside the chromatographic oven when temperatures exceed 40 C as they do here Column IonPac CS16 3 mm Analytical Column no guard Eluent 6 mM MSA gradient from 0 to 10 min to 9 mM MSA gradient from 10 to 30 min to 70 mM MSA Eluent Source EG40 Flow Rate 0 5 mL min Inj Volume 25 µL Detection Suppresse...

Страница 51: ... Flow Rate 10 µL min Peak 1 Lithium 2 Sodium 3 Ammonium 4 Potassium 5 Magnesium 6 Calcium Temperature 40 C Suppressor CCES 300 Cation Capillary Electrolytic Suppressor Detection Suppressed conductivity Injection Volume 0 4 µL 0 4 8 12 16 20 24 0 2 2 5 µS 1 2 3 4 5 6 Minutes Figure 32 Separation of Six Cations on a Capillary CS16 column Document No 031747 05 2010 Dionex Corporation December 2010 ...

Страница 52: ...ination Bad eluents Remake eluents 6 2 6 4 Contaminated column Clean column 6 3 1 7 4 Contaminated suppressor Clean suppressor 6 3 1 A 6 5 Component manual Hardware Operation Proportioning valve Service valve Component manual Poor Peak Resolution Poor Efficiency Large system void volumes Replumb system 6 6 3 B Component manual Sluggish injection valve Service valve 6 6 3 A Component manual Contami...

Страница 53: ... particulates clogging the bed support a clogged High Pressure In Line Filter suppressor or the detector cell To determine which part of the chromatographic system is causing the problem disconnect the pump eluent line from the injection valve and turn the pump on Watch the pressure it should not exceed 50 psi 0 34 MPa Continue adding system components injection valve column s suppressor and detec...

Страница 54: ...nto the end fitting Make sure that the end of the column tube is clean and free of any particulate matter so that it will properly seal against the bed support assembly Use the end of the column to carefully start the bed support assembly into the end fitting IonPac CS16 IonPac CS16 IonPac CS16 5 mm Columns 3 mm Columns 0 5 mm Columns Part P N P N P N Analytical or Capillary Column 057573 059596 0...

Страница 55: ...zed water of the proper purity 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 C The system should be as metal free as possible Gripper tubing fittings used in older systems are a potential source for metal contamination of the column The new Dionex ThermoFlare or PEEK ferrule fittings are preferred ...

Страница 56: ...s contaminated and acting as a concentrator 6 Replace the sample loop with new tubing and repeat this test 7 If there is still a quantification problem check other components of the system tubing injection valve detector cell or call your Dionex representative If you have a divalent quantification problem in your system but you neither have the time nor replacement parts you can still get accurate...

Страница 57: ...luent typically 1 mL min for 5 mm operation or 0 36 mL min for 3 mm operation or 0 10 mL min for 0 5 mm operation If it is used in the AutoSuppression External Water Mode it should be at least 5 mL min for non solvent containing eluents When solvents are used in the eluent the regenerant flow rate should be approximately 10 mL min E Check the eluent flow rate See if the eluent flow rate is equival...

Страница 58: ...esult in sample band dispersion causing loss of peak efficiencies Make sure you are using PEEK tubing with an i d of no greater than 0 010 for 5 mm systems or 0 005 for 3 mm systems to make all eluent liquid line connections between the injection valve and the detector cell inlet Cut the tubing lengths as short as possible Check for leaks B Check to see if headspace has developed in the guard or a...

Страница 59: ...uire approximately 10 minutes to equilibrate to the initial eluent The minimum equilibration time can be determined by making successive runs with increasing equilibration times The column is equilibrated to the initial eluent when additional equilibration time does not increase the runtime of the first eluting peaks B Sluggish operation of the injection valve may be the problem Check the air pres...

Страница 60: ...ary tube fitting make sure that the ferrule and fitting bolt are at least 2 mm 0 1 in from the end of the tubing before you insert the tubing into the port Do not place the ferrule and fitting bolt flush with the end of the tubing Figure 33 illustrates the correct and incorrect placement of the ferrule and fitting bolt on the tubing Correct Incorrect 2 mm Figure 34 Correct and Incorrect Ferrule an...

Страница 61: ...ANCE REPORT Quality Assurance Report IonPac CS16 Analytical Column 3 x 250 mm Quality Assurance Report IonPac CS16 Analytical Column 5 x 250 mm Quality Assurance Report IonPac CS16 Capillary Column 0 5 x 250 mm Document No 031747 05 2010 Dionex Corporation December 2010 ...

Страница 62: ...Product Manual for IonPac CS16 Page 60 of 65 Document No 031747 05 2010 Dionex Corporation December 2010 ...

Страница 63: ...Product Manual for IonPac CS16 Page 61 of 65 Document No 031747 05 2010 Dionex Corporation December 2010 ...

Страница 64: ...Product Manual for IonPac CS16 Page 62 of 65 Document No 031747 05 2010 Dionex Corporation December 2010 ...

Страница 65: ... effluent to a waste container B Rinse the column for 90 minutes with 0 5 mN sulfuric acid and 10 acetonitrile C Rinse the column for 30 minutes with eluent D Reconnect the column to the suppressor Column Cleanup The following column cleanup protocols have been divided into two general isocratic protocols A Acid soluble contaminants B Hydrophobic cations and organic contaminants Always ensure that...

Страница 66: ...Analytical or Guard Column Set the pump flow rate to 0 010 mL min for a CS16 Capillary or Capillary Guard Column D Rinse the column for 15 minutes with 10 mM HCl before pumping the chosen cleanup solution over the column E Pump the cleanup solution 1 M HCl or 500 mM oxalic acid through the column for 60 minutes F Rinse the column for 15 minutes with 10 mM HCl before pumping eluent over the column ...

Страница 67: ...E2 0 0 100 0 20 0 0 100 25 0 0 100 45 0 100 0 55 0 100 0 D Rinse the column for 15 minutes with 10 mM HCl before pumping eluent over the column E Equilibrate the column s with eluent for at least 30 minutes before resuming normal operation F Reconnect the IonPac CS16 Connect the Analytical Capillary Column outlet to the Suppressor and the inlet to either the IonPac CG16 Guard Column or the Pump Mo...

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