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IonPac CS14 Manual

Doc. No. 034848-10

Page 38 of 54

5.18 Methanesulfonic acid / 18-Crown-6 Gradient Elution of Alkanolamines with Group I & II
Cations

The IonPac CS14 can be used to monitor the amine content in the quality control of chemical additives, process solutions,
plating baths, and scrubber solutions. To optimize resolution, the 18-Crown-6 ether complexing agent can be added to the
eluent as illustrated in this example. This chemical forms a strong complex with monovalent cations such as potassium,
ammonium and ethanolamine. These complexes are very highly retained, increasing the retention times of these cations. Due
to the differences in the degree of complexation and the selectivity of the resin for the complexes, the elution order of the ions,
ethanolamine and ammonium, and ethanolamine and triethanolamine, are reversed. This technique can be useful for the
determination of alkanolamines in the presence of high ammonium or potassium concentrations since these two analytes elute
late.

The determination of monoethanolamine, triethanolamine and other alkanolamines in the presence of ammonia, Group I & II
cations can be accomplished by gradient elution using 5 mM methanesulfonic acid (MSA) as the initial eluent and then
stepping to 21 mM methanesulfonic acid (MSA) after 12 minutes.

This eluent can be suppressed using the AutoSuppression Recycle Mode. To convert the column back to eluents without 18-
Crown-6 ether, wash the column with an acetonitrile/DI water gradient from 5% to 40% acetonitrile, hold for 20 minutes, and
then equilibrate to the new operating conditions. Carefully flush all lines and fittings used with the 18-Crown-6 eluent.

Sample Loop Volume:

6.25 µL (2-mm), 25 µL (4-mm)

Analytical Column:

IonPac CS14 Analytical Column

Eluent:

See Chromatogram

Eluent Flow Rate:

0.25 mL/min (2-mm), 1.0 mL/min (4-mm)

SRS Suppressor:

Cation Self-Regenerating Suppressor, CSRS ULTRA (2-mm or 4-mm)
Recycle Mode

or MMS Suppressor:

Cation MicroMembrane Suppressor, CMMS III (2-mm or 4-mm)

MMS Regenerant:

100 mN TBAOH

(tetrabutylammonium hydroxide)

Expected Background Conductivity:

< 1 µS

Storage Solution:

Eluent

Eluent 1:

Type I DI Water

Eluent Flow Rate:

1.0 mL/min

Eluent 2:

10 mM MSA

(4-mm System)

Eluent 3:

100 mM MSA

Eluent 4:

10 mM 18-Crown-6

TIME (min)

%E1

%E2

%E3

%E4

Comments

Equilibration

0.0

45

30

0

25

Equilibrate to 3.0 mM MSA / 2.5 mM 18-Crown-6

10.0

45

30

0

25

Analysis

0.0

45

30

0

25

Inject, 3.0 mM MSA / 2.5 mM 18-Crown-6

0.1

45

30

0

25

Inject Valve to Load Position

10.0

45

30

0

25

3.0 mM MSA / 2.5 mM 18-Crown-6

15.0

35

0

40

25

40 mM MSA / 2.5 mM 18-Crown-6

35.0

35

0

40

25

40 mM MSA / 2.5 mM 18-Crown-6

35.1

45

30

0

25

3.0 mM MSA / 2.5 mM 18-Crown-6

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Содержание Dionex IonPac CS14 Guard

Страница 1: ...Thermo Scientific Dionex IonPac CS14 Columns Product Manual P N 034848 10 July 2012 Part of Thermo Fisher Scientific ...

Страница 2: ...1 of 54 PRODUCT MANUAL for the IONPAC CG14 GUARD COLUMN 2 x 50 mm P N 044122 4 x 50 mm P N 044124 IONPAC CS14 ANALYTICAL COLUMN 2 x 250 mm P N 044121 4 x 250 mm P N 044123 2012 Thermo Fisher Scientific Document No 034848 Revision 10 July 2012 ...

Страница 3: ... Loop 2 15 μL 11 3 3 2 The 4 mm System Injection Loop 10 50 μL 11 3 4 Sample Concentration 11 3 5 IonPacCG14GuardColumns 11 3 6 Eluent Storage 11 3 7 Cation Self Regenerating Suppressor Requirements 11 3 8 CationAtlas Electrolytic Suppressor Requirements 12 3 9 Cation MicroMembrane Suppressor Requirements 12 3 10 UsingAutoRegen 12 3 11 Detector Requirements 12 SECTION 4 OPERATION 13 4 1 General Op...

Страница 4: ...aminesWith Resolution EnhancementThrough Gradient Elution 24 5 9 Isocratic Elution of Mono Di andTrimethylamines and Resolution Enhancement throughAddition of Solvent to Eluent 25 5 10 Elution of Mono Di andTriethylaminesWith Resolution EnhancementThrough theAddition of Solvent to the Eluent 26 5 11 GradientElutionofCyclohexylamine 28 5 12 ElutionofAliphaticMonoamines 29 5 13 Gradient Elution ofAl...

Страница 5: ... Poor Peak Resolution 47 6 6 1 Loss of Peak Efficiency throughout the Chromatogram 47 6 6 2 Loss of Resolution Throughout the Chromatogram Due to Shortened Retention Times 47 6 6 3 Loss of Early Eluting Peak Resolution 48 6 7 Spurious Peaks 48 APPENDIXA QUALITYASSURANCE REPORT 49 APPENDIX B COLUMN CARE 52 Recommended Operating Pressures 52 ColumnStart Up 52 Column Storage 52 ColumnConditioning 52 ...

Страница 6: ...lution with the strong cation exchangers The hydrophilic characteristic of the surface permit alkyl and alkanolamines to be eluted with good peak symmetry and efficiency However short chain alkanolamines such as monoethanolamines may exhibit improved separations on the IonPac CS12 The IonPac CS14 Column is compatible with eluents having pH from 0 to 14 and is solvent compatible The column can be u...

Страница 7: ...raph IC If you do not understand the operation of the system take the time to familiarize yourself with the various system components before beginning an analysis You may need to make a liquid line fitting The IonPac CS14 Analytical Column and the IonPac CG14 Guard Column have 10 32 PEEK end fittings for use with ferrule bolt liquid line fittings If you have an Ion Chromatograph with Tefzel liquid...

Страница 8: ...n Loop 2 15 µL Use the Rheodyne Microinjection Valve Model No 9126 DIONEX P N 044697 for full loop injections 15 µL 10 50 µL System Void Volume Eliminate switching valves couplers and the GM 3 Gradient Mixer Use only the Microbore GM 4 2 mm Mixer P N 049135 Minimize dead volumes Switching valves couplers can be used Use the GM 2 GM 3 or recommended gradient mixers Pumps Use the GS50 GP50 GP40 IP20...

Страница 9: ...3 VDM 2 Cell 6 mm 10 µL P N 043113 CD20 CD25 CD25A ED40 ED50 or ED50A Conductivity Cell with DS3 P N 044130 or with shield P N 044132 CDM 2 CDM 3 Cell P N 042770 Either the TS 1 with the TS 2 can be used with the CDM 2 or the CDM 3 Do not use the TS 2 or the TS 1 with the ED40 ED50 ED50A or the CD20 CD25 CD25A Ensure 30 40 psi back pressure after the cell see Table 3 Color Dionex P N ID inches ID ...

Страница 10: ...ubing see Dionex Product Selection Guide may be used but peak efficiency will be compromised which may also result in decreased peak resolution Minimize the lengths of all connecting tubing and remove all unnecessary switching valves and couplers If you need assistance in properly configuring your system contact the Dionex Office nearest you see Dionex Worldwide Offices 3 2 Installing the Cation T...

Страница 11: ...riodic maintenance and lost data A Disconnect the CTC It should be installed between the injection valve B Direct the outlet of the CTC to a separate waste container C Flush the CTC Use 30 mL of a 10X eluent concentrate of the strongest eluent required by the application at a flow rate of 2 0 mL min D Flush the CTC prior to start up Prior to the use of the chromatographic system on the next day fl...

Страница 12: ...umn must be used for trace cation concentrator work on 2 mm systems See Section 4 5 Sample Concentration for details on sample concentration 3 5 IonPac CG14 Guard Columns An IonPac CG14 Guard Column is normally used with the IonPac CS14 Analytical Column Retention times will increase by approximately 20 when a guard column is placed in line prior to the analytical column A guard is placed prior to...

Страница 13: ...ty a pressurized vessel rather than the AutoRegen must be used When using an AutoRegen System the regenerant passes over the hydroxide form anion exchange resin in the AutoRegen Cation Regenerant Cartridge where specific anionic contaminants such as chloride ions are continuously removed from the regenerant TBAOH to restore the salt form of the regenerant to the base form If solvents are used in t...

Страница 14: ...s eluents that are free of ionic impurities Chemicals solvents and deionized water used to prepare eluents must be of the highest purity available Low trace impurities and low particle levels in eluents also help to protect your ion exchange columns and system components Dionex cannot guarantee proper column performance when the quality of the chemicals solvents and water used to prepare eluents h...

Страница 15: ...n using a solvent in an ionic eluent column generated back pressures will depend on the solvent used concentration of the solvent the ionic strength of the eluent and the flow rate used The column back pressure will vary as the composition of water acetonitrile mixture varies The practical back pressure limit for the IonPac CS14 columns is 4 000 psi 27 57 MPa The IonPac CS14 is compatible with the...

Страница 16: ...e capacity of the AutoRegen Cation Regenerant Cartridge If acetonitrile is used with suppressed conductivity a pressurized vessel rather than the AutoRegen must be used 4 5 Sample Concentration The IonPac CG14 Guard Column or the Low Pressure Trace Cation Concentrator TCC LP1 should be used for trace cation concentrator Trace cation concentrators are used primarily in high purity water analysis Th...

Страница 17: ...nic concentration you may be able to increase the sensitivity of your system by using sample concentration techniques see Section 4 5 Sample Concentration 5 1 Preparation of Eluent Stock Solution Concentrates CAUTION WARNING Methanesulfonic acid MSA trifluoroacetic acid andpyrophosphoric acid are corrosives and strong irritants Avoidbreathingthevapors Always prepare these reagents in a fume hood W...

Страница 18: ...etic acid TFA or 18 Crown 6 Ether Using the table below pipet X 0 mL of the 1 0 N MSA or TFA eluent concentrate see Section 5 1 Preparation of Eluent Stock Solution Concentrates into a 1 L volumetric flask Dilute to 1 L using deionized water with a specific resistance of 18 2 megohm cm Degas the eluent Table 6 mM Eluents from 1 0 M Stock Solutions m M mL of 1 0 M MSA or TFA MSA or TFA 4 4 0 8 8 0 ...

Страница 19: ...specification standards all columns undergo the following production control test Sample Loop Volume 6 25 µL 2 mm 25 µL 4 mm Analytical Column IonPac CS14 Analytical Column Eluent 10 mM MSA Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm ...

Страница 20: ... Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regenerant 100 mN TBAOH tetrabutylammonium hydroxide or AES Suppressor Cation Atlas Electrolytic Suppressor CAES up to 25 µeq min Expected Background Conductivity 3 µS Storage Solution Eluent Figure 3 IsocraticElutionofAmmonium GroupI IICa...

Страница 21: ...lumn is not harmed in any way Sample Loop Volume 6 25 µL 2 mm 25 µL 4 mm Analytical Column IonPac CS14 Analytical Column Eluent 10 mM MSA Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regenerant 100 mN TBAOH tetrabutylammonium hydro...

Страница 22: ...phoric acid by washing the column with 100 mM methanesulfonic acid for 30 minutes Sample Loop Volume 6 25 µL 2 mm 25 µL 4 mm Analytical Column IonPac CS14 Analytical Column Eluent See Chromatogram Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm Recycle Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm o...

Страница 23: ... concentration is used to optimize the positioning of morpholine between potassium and magnesium and improve the morpholine peak shape The third example illustrates the determination of trace levels of lithium sodium ammonium potassium magnesium and calcium in a high purity power plant water treated with morpholine 1 0 mL of sample was concentrated on a CG14 guard column and then analyzed The samp...

Страница 24: ...ULTRA AutoSuppression External Water Mode Analyte mg L 1 Li 1 0 2 Na 4 0 3 NH4 5 0 4 K 10 0 5 Morpholine 50 0 6 Mg2 5 0 7 Ca2 10 0 1 mg L 1 ppm Analyte mg L 1 Li 0 5 2 Na 2 0 3 NH4 2 5 4 K 5 0 5 Morpholine 25 0 6 Mg2 2 5 7 Ca2 5 0 1 mg L 1 ppm System 2 mm Flow Rate 0 25 mL min Injection 1 0 mL concentrated on an IonPac CG14 Analyte μg L 1 Li 0 5 2 Na 2 0 3 NH4 150 0 4 K 2 0 5 Morpholine 2 000 0 6 ...

Страница 25: ...essor CSRS ULTRA 2 mm or 4 mm External Water Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regenerant 100 mN TBAOH tetrabutylammonium hydroxide Expected Background Conductivity 1 µS Storage Solution Eluent Eluent 1 Type I DI Water Eluent Flow Rate 1 0 mL min Eluent 2 100 mM MSA 4 mm System Eluent 3 10 Acetonitrile TIME min E1 E2 E3 Comments Equilibration 0 0 70 5...

Страница 26: ...nalytical Column Eluent See Chromatogram Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm Recycle Mode or External Water Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regenerant 100 mN TBAOH tetrabutylammonium hydroxide Expected Background Conductivity 1 µS Storage Solution Eluent Figure ...

Страница 27: ...onPac CS14 Analytical Column Eluent See Chromatogram Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm Recycle Mode or External Water Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regenerant 100 mN TBAOH tetrabutylammonium hydroxide Expected Background Conductivity 1 µS Storage Solution El...

Страница 28: ... 2 5 4 Ethylamine 10 0 5 K 5 0 6 Diethylamine 10 0 7 Mg2 2 5 8 Ca2 5 0 9 Triethylamine 50 0 1 mg L 1 ppm Gradient Eluent As listed above CSRS ULTRA AutoSuppression External Water mode Isocratic Eluent 10 mM MSA CSRS ULTRA AutoSuppression Recycle Mode 0 10 20 30 μS 0 Minutes 1 2 34 5 6 5 7 8 9 0 10 20 30 μS 0 Minutes 1 2 3 4 5 6 5 7 8 9 ...

Страница 29: ...pressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm External Water Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regenerant 100 mN TBAOH tetrabutylammonium hydroxide Expected Background Conductivity 1 µS Storage Solution Eluent Eluent 1 Type I DI Water Eluent Flow Rate 1 0 mL min Eluent 2 100 mM MSA 4 mm System Eluent 3 50 Acetonitrile TIME min E1...

Страница 30: ...me 6 25 µL 2 mm 25 µL 4 mm Analytical Column IonPac CS14 Analytical Column Eluent See Chromatogram Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm Recycle Mode or External Water Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regenerant 100 mN TBAOH tetrabutylammonium hydroxide Expected Ba...

Страница 31: ... 1 mg L 1 ppm Figure 10 Analysis of Aliphatic Monoamines Analyte mg L 1 Li 0 5 2 Na 2 0 3 NH4 2 5 4 K 5 0 5 Mg2 2 5 6 Ca2 5 0 7 n Propylamine 7 5 8 tert Butylamine 12 5 9 sec Butylamine 12 5 10 iso Butylamine 12 5 11 n Butylamine 37 5 1 mg L 1 ppm GradientEluent Aslistedabove CSRSULTRA AutoSuppressionExternalWaterMode Isocratic Eluent 20 mM MSA 1 0 ACN CSRSULTRA AutoSuppressionExternalWaterMode Is...

Страница 32: ... 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm External Water Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regenerant 100 mN TBAOH tetrabutylammonium hydroxide Expected Background Conductivity 1 µS Storage Solution Eluent Eluent 1 Type I DI Water Eluent Flow Rate 1 0 mL min Eluent 2 100 mM MSA 4 mm System Eluent 3 10 Ac...

Страница 33: ...pholine 25 0 11 sec Butylamine 10 0 12 iso Butylamine 10 0 13 Mg2 2 5 14 Ca2 5 0 15 2 Methylpiperidine 20 0 16 Di n propylamine 20 0 17 3 Methylpiperidine 20 0 18 Cyclohexylamine 20 0 19 N Methylcyclohexylamine 20 0 20 Tripropylamine 20 0 1 mg L 1 ppm Figure 12 GradientElutionofAlkylamines Ammonia GroupI IICations 0 10 20 μS 0 Minutes 1 2 3 10 5 4 5 6 7 5 15 25 9 8 10 11 12 13 14 15 30 16 17 18 19...

Страница 34: ...on External Water Mode to suppress the eluent Sample Loop Volume See Chromatogram Analytical Column IonPac CS14 Analytical Column Eluent See Chromatogram Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm Recycle Mode or External Water Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regeneran...

Страница 35: ... eluents without 18 Crown 6 ether the column is washed with an acetonitrile deionized water gradient from 5 to 40 acetonitrile held for 20 minutes and then reversed back to the new operating conditions Sample Loop Volume 4 5 µL 2 mm 18 µL 4 mm Analytical Column IonPac CS14 Analytical Column Eluent 10 mM Trifluoroacetic acid 8 mM 18 Crown 6 1 2 Acetonitrile Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL ...

Страница 36: ...ac CS14 Analytical Column Eluent See Chromatogram Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm External Water Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regenerant 100 mN TBAOH tetrabutylammonium hydroxide Expected Background Conductivity 1 µS Storage Solution Eluent Isocratic Elue...

Страница 37: ...ia alkali and alkaline earth metals can be accomplished by gradient elution using 5 mM methanesulfonic acid MSA as the initial eluent and then stepping to 21 mM methanesulfonic acid MSA after 12 minutes The CSRS ULTRA can be used in the AutoSuppression Recycle Mode Sample Loop Volume 6 25 µL 2 mm 25 µL 4 mm Analytical Column IonPac CS14 Analytical Column Eluent See Chromatogram Eluent Flow Rate 0 ...

Страница 38: ...hylaminoethanol 5 0 7 K 5 0 8 Dimethylaminoethanol 10 0 9 N Ethyldiethanolamine 30 0 10 Di iso Propanolamine 20 0 11 Diethylaminoethanol 20 0 12 Mg2 1 0 13 Ca2 2 0 1 mg L 1 ppm Figure 16 Methanesulfonic Acid Gradient Elution of Alkanolamines with Ammonium Group I II Cations 1 2 3 4 5 7 8 9 6 0 10 20 30 μS 0 Minutes 1 3 2 4 40 10 11 12 13 ...

Страница 39: ...luent and then stepping to 21 mM methanesulfonic acid MSA after 12 minutes This eluent can be suppressed using the AutoSuppression Recycle Mode To convert the column back to eluents without 18 Crown 6 ether wash the column with an acetonitrile DI water gradient from 5 to 40 acetonitrile hold for 20 minutes and then equilibrate to the new operating conditions Carefully flush all lines and fittings ...

Страница 40: ... 1 Dimethylamino 2 propanol 10 0 7 Diethylaminoethanol 10 0 8 N n propyl diethanolamine 30 0 9 Mg2 0 5 10 Ca2 1 0 11 Ethanolamine 5 0 12 NH4 2 5 13 K 5 0 1 mg L 1 ppm Identified as a sample impurity Figure 17 MethanesulfonicAcid 18 Crown 6GradientElutionof Alkanolamines GroupI IICations 1 2 3 4 5 7 8 9 6 10 11 12 13 0 10 20 30 μS 0 Minutes 2 6 4 40 ...

Страница 41: ...ent will decrease baseline conductivity Sample Loop Volume 6 25 µL 2 mm 25 µL 4 mm Analytical Column IonPac CS14 Analytical Column Eluent See Gradient Program listed below Eluent Flow Rate 0 25 mL min 2 mm 1 0 mL min 4 mm SRS Suppressor Cation Self Regenerating Suppressor CSRS ULTRA 2 mm or 4 mm External Water Mode or MMS Suppressor Cation MicroMembrane Suppressor CMMS III 2 mm or 4 mm MMS Regener...

Страница 42: ...ofTemperatureontheGradientElutionof DiamineswithAmmonia GroupI IICations The CSRS ULTRA should be placed outside of the oven for oven temperatures 40 C Minimize tubing lengths between the column the CSRS ULTRA and the cell Use the AutoSuppression External Water Mode to ensure proper cooling of the CSRS ULTRA Temperature 60 C Temperature 23 C RoomTemperature 0 5 10 15 µS 0 Minutes 1 2 3 4 5 3 6 7 8...

Страница 43: ...ES Not Suppressing Check Current Component Manual CMMS Not Suppressing Check Regenerant Component Manual Check AutoRegen Cartridge Component Manual Contamination Bad Eluents Remake Eluents 6 2 6 4 Contaminated Column Clean Column 6 3 Column Care Contaminated CSRS CAES or CMMS Clean Suppressor 6 5 Component Manual Hardware Operation Proportioning Valve Service Valve Component Manual Poor Peak Resol...

Страница 44: ...psed walls an injection valve with a clogged port a column with particulates clogging the bed support a clogged High Pressure In Line Filter the 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 add...

Страница 45: ...ed support assembly into 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 4 mm Columns 2 mm Columns Part P N P N Analytical Column 044123 044121 Guard Column 044124 044122 Bed Support Assembly ...

Страница 46: ... 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 in the system are a potential source for metal contamination of the column The new Dionex ThermoFlare or PEEK ferrule fittings are preferred Inspect the eluen...

Страница 47: ... flow rate after the column using a stopwatch and graduated cylinder Refer to the Cation Self Regenerating Suppressor ULTRA Product Manual Document No 031370 or to the Cation MicroMembrane Suppressor III Product Manual Document No 031728 for assistance in determining if the eluent is within suppressible limits F If you are using an AutoRegen Accessory with the CSRS in the Chemical Suppression Mode...

Страница 48: ...ssemblies If the resin does not fill the column body all the way to the top it means that the resin bed has collapsed creating a headspace The column must be replaced B Extra column effects can result in sample band dispersion making the peaks elution less efficient Make sure you are using PEEK tubing with an i d of no greater than 0 010 for 4 mm systems or no greater than 0 005 for 2 mm systems t...

Страница 49: ...proximately 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 pressure an...

Страница 50: ...S14 Manual Doc No 034848 10 Page 49 of 54 APPENDIX A QUALITY ASSURANCE REPORT Quality Assurance Report IonPac CS14 Analytical Column 2 x 250 mm Quality Assurance Report IonPac CS14 Analytical Column 4 x 250 mm ...

Страница 51: ...25 mL min Detection Suppressed Conductivity CSRS ULTRA 2 mm AutoSuppression Recycle Mode Injection Volume 2 5 µL Storage Solution Eluent Peak Information Found Components Peak No 1 2 3 4 5 6 Retention Time 3 29 3 63 4 26 5 35 8 34 9 73 Name Lithium Sodium Ammonium Potassium Magnesium Calcium mg L 0 5 2 0 2 5 5 0 2 5 5 0 Efficiency 3942 4320 2785 4100 4010 3973 Asymmetry 10 1 4 1 3 2 1 1 8 1 3 1 3 ...

Страница 52: ...ressed Conductivity CSRS ULTRA AutoSuppression Recycle Mode Plot Scale Autoscale Injection Volume 25 µL Storage Solution Eluent Peak Information Found Components Peak No 1 2 3 4 5 6 Retention Time 3 10 3 44 4 08 5 16 8 41 9 85 Name Lithium Sodium Ammonium Potassium Magnesium Calcium mg L 0 5 2 0 2 5 5 0 2 5 5 0 Efficiency 4986 5418 4099 5104 4452 4388 Asymmetry 10 1 1 1 2 1 4 1 6 1 2 1 3 Resolutio...

Страница 53: ... column 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 ensu...

Страница 54: ...separately C Set the pump flow rate to 1 0 mL min for a CS12 4 mm Analytical or Guard Column or set the pump flow rate to 0 25 mL min for a CS12 2 mm Analytical or 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 ...

Страница 55: ...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 before resuming normal operation for at least 30 minutes F Reconnect the IonPac CS14 Analytical Column outlet to the suppressor and the inlet to either the IonPac CG14 2 mm or 4 mm Guard Column or the gradient pump G Equilibrate the system w...

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