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colu
mns IonPac AS15 Anion-Exchange Column
Passion. Power. Productivity.
0 38-0.3
µS
Minutes
28425
Peak Concentration (µg/L) A B1. Fluoride 0.018 0.48 2. Chloride 0.12 2.493. Nitrite 0.042 2.534. Carbonate — —5. Sulfate 0.075 4.726. Bromide — 2.367. Nitrate 0.15 2.588. Phosphate — 2.15
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The IonPac® AS15 is a high-capacity, hydroxide-selective anion-exchange column designed for the determination of trace-level concentrations of inorganic anions and low molecular weight organic acids, including fluoride, glycolate, acetate, formate, chloride, nitrite, carbonate, sulfate, oxalate, bromide, nitrate, and phosphate in high-purity water matrices encountered in the semiconductor and power generation industries. The IonPac AS15 column offers excellent retention of fluoride from the water dip and uses a simple hydroxide eluent easily supplied by the Eluent Generator (EG).
The IonPac AS15 column is available in formats from 0.4 to 4 mm, allowing use of capillary to analytical flow rates, and supporting advanced IC × IC applications.
Superior Chromatographic Performance• Universalcolumnfortrace-level
concentrationsofinorganicanionsandlowmolecularweightorganicacidsinhigh-puritywatermatrices.
• TheIonPacAS15-5µm(3×150mm) columnisrecommendedforfastseparationofcommoninorganicanionsandmonovalentorganicacidsin15minutes.
• IonPacAS15-9µm(0.4×250, 2×250and4×250mm)columnsarerecommendedforhigher capacityapplications(25minuteanalysistime).
• TheAS15Capillarycolumn (0.4×250mm)offersreducedeluent consumption,reducedoperatingcosts,andexcellentreproducibility.
• Columnselectivityoptimizedfora30°Coperatingtemperaturetoensurereproducibleretentiontimes.
• Large-loopinjectionsforppb-levelanalysis.
• Samplepreconcentrationforultra-trace(ppt-level)analysisusingopti-mizedAC15concentratorcolumn.
• Superiorretentionandresolutionofearly-elutinganions,includingfluo-ride,glycolate,acetate,andformate.
• SimplifiedoperationisprovidedbytheEG,whichrequiresonlyadeionizedwatersourcetoproducepotassiumhydroxideeluent.
• Hydroxideeluentsuppressestoaverylowbackgroundfortrace-leveldeterminations.
• Compatiblewithorganicsolventstoenhanceanalytesolubility,tomodifycolumnselectivity,orforeffectivecolumncleanup.
• Directtransferof4mmapplicationstothe0.4mm,3mm,and2mm columnformatsformoreeco-nomicaloperation,reducedeluentconsumption,andincreasedmasssensitivity.
2
High-Efficiency Particle StructureTheIonPacAS15packingisa
uniquestructurecomposedofahighlycrosslinkedcoreandananion-exchangelayergraftedtothesurface,asshowninFigure1.TheAS15columnsubstrateiscomposedofamacroporousresinbead (5µmdiameterforthe3mmcolumnand9µmforthe0.4mm,4mm, and2mmcolumns)consistingof ethylvinylbenzenecrosslinkedwith55%divinylbenzene.
Theanion-exchangelayerisfunctionalizedwithalkanolquaternaryammoniumgroupsandhasacontrolledthickness,whichresultsinexcellentmasstransfercharacteristicsand consequently,highlyefficientpeaks.
Versatile CapabilityTheIonPacAS15columnis
idealfortheisocraticseparationoffluoride,chloride,carbonate,nitrite,sulfate,bromide,nitrate,andphosphateinhighpuritywatermatricesusingasimplehydroxideeluentandsuppressedconductivitydetection.Fluorideiswellresolvedfromthewaterdipwith elutionofhighlyretainedanalytes suchasphosphatein15minusingthe 3×150mmcolumnand<25min usingthe0.4×250mmor4×250mmcolumns,asillustratedinFigure2.
TheIonPacAS15-5µm (3×150mm)columnusesthesamealkanolammoniumfunctionalgroupsastheAS15-9µm(4×250mm)column,butdiffersincolumnformatandresinparticlesize.Asaresult,the3mmcolumnprovidestheadvantagesoffasteranalysistimeforthecommoninorganicanions,reducedeluentconsumption,andimprovedminimumdetectionlimitscomparedtothe4mmcolumn.TheAS15-5µm(3×150mm)columnisrecommendedforthefastseparationofthecommoninorganicanionsandlowmolecularweightorganicacids.
Figure 1. Structure of an IonPac AS15-9µm packing particle.
Figure 2. Comparison of the IonPac AS15-5µm (3 × 150 mm), AS15-9µm (4 × 250 mm), and AS15-9µm (0.4 × 250 mm) columns for separation of inorganic anions.
Anion ExchangePolymer layer
Highly Crosslinked Core
4.5m
13786
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Column: A) IonPac AG15, AS15-5µm (3 × 150 mm) B) IonPac AG15, AS15-9µm (4 × 250 mm) C) IonPac AG15, AS15 (0.4 × 250 mm)Eluent: A) 42 mM Potassium hydroxide B) 40 mM Potassium hydroxide C) 38 mM Potassium Hydroxide Eluent Source: EGC-KOHTemperature: 30 °CFlow Rate: A) 0.5 mL/min B) 1.2 mL/min C) 0.012 mL/minInj. Volume: A) 5 µL B) 10 µL C) 400 nLDetection: Suppressed conductivity, ASRS®-ULTRA, AutoSuppression® recycle mode
Peaks: 1. Fluoride 2 mg/L (ppm) 2. Chloride 5 3. Carbonate – 4. Nitrite 10 5. Sulfate 10 6. Bromide 20 7. Nitrate 20 8. Phosphate 30
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Thehigh-capacity IonPacAS15-9µm0.4×250mm, 4×250mmand2×250mmcolumnsarerecommendedforhighercapacityapplicationsandprovidemaximumresolutionoftracecomponentsinthepresenceofhighconcentrationsof otheranions.
3
AS15 Capillary FormatTheIonPacAS15Capillary
column(0.4×250mm)ispackedwiththesamematerialastheequivalentstandardboreversion(producingthesameperformanceasa4mmcolumn),butrequiresonly1/100ththeeluentflowrate.Thecapillaryformatofferstheadvantageoflesseluentconsumptionprovidingreducedoperatingcosts.Figure3illustratestheseparationoftracelevelinorganicanionsusingtheIonPacAS15capillarycolumnafterconcentrationontheIonSwift®MAC-100Concentratorcolumn.Excellentretentiontimereproducibilitycanbeachievedwith thecapillaryformat.
Large Loop Injections for µg/L (ppb) Level Analysis
TheIonPacAS15columnselectivityandhighcapacityallowthedeterminationoftracelevelsofinorganicanionsandlowmolecularweightorganicacidsinhigh-puritywatermatricesusingalarge-loopinjection.Figure4illustratestheseparationofinorganicanionsandlowmolecularweightorganicacidsinahigh-puritywatersampleusingthistechnique.Separationwasachieved usingapotassiumhydroxidegradientwithsuppressedconductivitydetectionatatemperatureof30°C.Lowµg/L(ppb)levelsoftheseanalytescaneasilybequantifiedusinga1mLinjectiononanIonPacAS15-5µm(3×150mm) column.Theconductivityofthehydroxideeluentcanbesuppressedto averylowbackground,facilitatingtrace-levelanalysis.
Figure 4. Determination of inorganic anions and low molecular weight organic acids in high-purity water using a large-loop injection and a potassium hydroxide gradient on an IonPac AS15-5µm (3 × 150 mm) column.
284250 38Minutes
1.6
µS
-0.3
Column: IonPac AS15-9µm (0.4 × 250 mm)Eluent Source: Capillary EGC-KOH cartridge Eluent: 7 mM KOH (0 to 10 minutes), 7 to 32 mM KOH (10 to 16 minutes), 32 to 50 mM KOH (16 to 30 minutes), 50 to 65 mM (30 to 33 minutes), 7 mM KOH (33 to 38 minutes) Flow Rate: 12 µL/minTemperature: 30 °CDetection: Suppressed conductivity, ACES 300, Anion Capillary Electrolytic Suppressor, AutoSuppression recycle modeConcentrator: IonSwift MAC-100 Concentrator (0.5 mm × 80 mm)Inj. Volume: 180 µL Sample: A: Deionized water B: Deionized water spiked with 0.5 µg/L Fluoride, 2.5 µg/L chloride, nitrite, bromide, nitrate, and phosphate, 5.0 µg/L sulfate
Peak Concentration (µg/L) A B1. Fluoride 0.018 0.48 2. Chloride 0.12 2.493. Nitrite 0.042 2.534. Carbonate — —5. Sulfate 0.075 4.726. Bromide — 2.367. Nitrate 0.15 2.588. Phosphate — 2.15
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B
Figure 3. Separation of inorganic anions at trace concentrations using the IonPac AS15 Capillary column and the IonSwift MAC-100 Concentrator column.
0 2 4 6 8 10 12 14Minutes
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µS
Column: IonPac AG15, AS15-5µm (3 × 150 mm)Eluent : 10 mM Potassium hydroxide for 4 min to 60 mM at 11 min Eluent Source: EG40Temperature: 30 °CFlow Rate: 0.7 mL/minInj. Volume : 1000 µLDetection: Suppressed conductivity, ASRS-ULTRA 2-mm, AutoSuppression recycle mode
Peaks: 1. Fluoride 1 µg/L (ppb) 2. Glycolate 4 3. Acetate 4 4. Formate 2 5. Chloride 2 6. Nitrite 2 7. Carbonate – 8. Sulfate 2 9. Oxalate 2 10. Bromide 4 11. Nitrate 4 12. Phosphate 6
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Figure 6. Determination of trace levels of chloride and sulfate in high purity water using a large loop injection on the IonPac AS15-5µm (3 × 150 mm) column.
AC15 Concentrator Column for Preconcentration for Ultratrace (ng/L) Analysis
Monitoringanioniccontaminantsatlowng/L(ppt)levelsinultrapurewaterisacriticalissueinthesemicon-ductorandpowergenerationindustries.Usingpreconcentrationtechniques,low-pptlevelsofinorganicanionsandlowmolecularweightorganicacidscanbedeterminedeasily.Figure5illustrates thistechniqueusinganIonPacAC15concentratorcolumn,whichisdesignedforreproduciblerecoveriesoftraceanionssuchaschlorideandsulfate fromhigh-puritywater.Usingsamplepreconcentration,low-pptlevelsof inorganicanionsandlowmolecularweightorganicacidscanberoutinelymeasuredinpowerplantandsemicon-ductorpurewater.
Trace Analysis is Easier with the Eluent Generator
CombiningtheIonPacAS15 columnwiththeEGmakestraceanionanalysiseveneasier.TheEGmakes potassiumhydroxideeluentelectrolyti-callyfromwater.Theuseofthisultra-purehydroxideasaneluentresultsinalowbackgroundandstablebaseline.Routineppb-levelanalysisofinorganicanionsandlowmolecularweightorgan-icacidsbydirectinjectionispossiblewiththeIonPacAS15columnusing theEG,asillustratedinFigures4and5.
Trace Analysis of Inorganic Anions and Low Molecular Weight Organic Acids in High Ionic Strength Matrices
Highcapacitycolumnsallowlargeloopinjectionswhilemaintainingthepeakshapesoftracecomponents,eveninthepresenceofhighconcentrationsofotheranions(e.g.carbonate)thatmaybepresentinthehigh-puritywatermatricesencounteredinthesemiconductorandpowergenerationindustries.
Figure 5. Determination of inorganic anions and low molecular weight organic acids from a 20-mL sample volume of high-purity water using the IonPac AS15-9µm (2 × 250 mm) column.
Figure6showstheuseofthe IonPacAS15-5µm(3×150mm) columnfortracechlorideandsulfateinahigh-puritywatermatrixcontaininghighconcentrationsofcarbonate.Usinganisocraticpotassiumhydroxideeluent,carbonateiswellresolvedfromchlorideandsulfateanddoesnotinterferewithquantification.Forhigh-puritywater applicationsthatrequiredetermination ofafewspecificanalytes,afastrunusingtheAS15-5µm(3×150mm)columnisrecommended.
Forapplicationsrequiringhighercapacity,theAS15-9µmcolumnsarerecommended.The0.4mm,4mm, and2mmIonPacAS15-9µmcolumnshaveveryhighcapacities,providing excellentresolutionofinorganicanionsincomplexsamplematrices.Figure7 comparestheseparationofinorganicanionsinawastewatersampleontheIonPacAS15-5µm(3×150mm)andAS15-9µm(4×250mm)columns.
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Sample Volume: 20 mL, preconcentrated Detection: Suppressed conductivity, ASRS-ULTRA 2-mm, AutoSuppression® recycle mode
Peaks: 1. Fluoride 0.1 µg/L (ppb) 2. Acetate 0.1 3. Formate 0.1 4. Chloride 0.1 5. Nitrite 0.1 6. Carbonate – 7. Sulfate 0.1 8. Oxalate 0.1 9. Bromide 0.1 10. Nitrate 0.1 11. Phosphate 0.1
Column: IonPac AG15, AS15-9µm (2 × 250 mm)ConcentratorColumn: IonPac AC15Eluent: Potassium hydroxide, 10 mM from 0 to 4 min, 10 mM to 40 mM from 4 min to 14 min, 40 mM to 60 mM from 14 to 18 minEluent Source: EG40Temperature: 30 °CFlow Rate: 0.5 mL/min
0 5Minutes
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Column: IonPac AG15, AS15-5µm (3 × 150 mm)Eluent: 42 mM Potassium hydroxideEluent Source: EG40Temperature: 30 °CFlow Rate: 0.5 mL/min
Inj. Volume: 1000 µL Detection: Suppressed conductivity, ASRS-ULTRA 2-mm, AutoSuppression recycle mode
Peaks: 1. Chloride 1 µg/L (ppb) 2. Carbonate 1000 3. Sulfate 1
5
Figure 7. Analysis of an industrial wastewater sample on the IonPac AS15-5µm (3 × 150 mm) and AS15-9µm (4 × 250 mm) columns.
Figure 8. Separation of weakly retained organic acids using a potassium hydroxide gradient on the IonPac AS15-5µm (3 × 150 mm) column.
Determination of Inorganic Anions and Low Molecular Weight Organic Acids
Lowmolecularweightorganicacidsandmono-anddivalentinorganicanionscommonlyencounteredinthechemical,semiconductor,andpowergenerationindustriescanbedeterminedinasinglerunusingtheIonPacAS15-5µm (3×150mm)column.Figure8 illustratestheseparationofweaklyretainedanionssuchasacetate,formate,propionate,andbutyrateinasimulatedindustrialchemicalsampleusinga hydroxidegradientatacontrolled temperatureof30°C.
System RecommendationsTheIonPacAS15columnis
recommendedforusewithDionex ICS-2100orICS-5000ICsystemsequippedwithanEG.TheAS15columncanalsobeusedwitholderDionexICsystemsequippedwithanEGoranRFC-30Reagent-Free®Controller.TheEGisusedtoautomaticallyproducepotassiumhydroxidegradientsfromdeionizedwater.
Suppressor RecommendationsForoptimumeaseofuseand
economy,usetheIonPacAS15columnwiththeASRS®300AnionSelf-Regen-eratingSuppressor®orACES™ Anion CapillaryElectrolyticSuppressor300.OperatetheAS15atanelevated temperature(30°C)toensure reproducibleretentiontimes.
Anion Trap ColumnsWhenusingtheEGforeluent
delivery,aCR-ATCcolumnshouldbeinstalledbetweentheEGcartridgeandtheEGdegasmodule.Alternately,4mm,3mm,and2mmsystemscanusetheATC-HCcolumn,installedbetweenthepumpoutletandinletoftheEluGencartridgeintheEGmodule.Whenperformingsodiumhydroxide-gradientapplicationsontheIonPacAS15 columnusinghand-preparedbottledeluents,theATC-3shouldbeinstalledbetweenthegradientpumpandtheinjectionvalvetoremoveanionic contaminantsfromtheeluent.
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Column: A) IonPac AG15, AS15-5µm (3 × 150 mm) B) IonPac AG15, AS15-9µm (4 × 250 mm)Eluent: A) 10 mM Potassium hydroxide for 4 min to 60 mM at 9 min B) 8 mM Potassium hydroxide for 6 min to 55 mM at 18 minEluent Source: EG40Temperature: 30 °CFlow Rate: A) 0.7 mL/min B) 1.6 mL/minSample Prep.: Industrial wastewater, 1:10 dilutionInj. Volume: A) 5 µL B) 10 µLDetection: Suppressed conductivity, ASRS-ULTRA, AutoSuppression recycle mode
Peaks: 1. Chloride 2. Carbonate 3. Sulfate 4. Bromide 5. Chlorate
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Peaks: 1. Fluoride 1 mg/L (ppm) 2. Glycolate 5 3. Acetate 5 4. Formate 5 5. Propionate 5 6. Chloride 2 7. Nitrite 2 8. Butyrate 5 9. Carbonate 30 10. Sulfite 2 11. Sulfate 2 12. Oxalate 3 13. Bromide 5 14. Nitrate 5 15. Phosphate 10 16. Chlorate 10 17. Thiosulfate 10
Column: IonPac AG15, AS15-5µm (3 × 150 mm)Eluent: 10 mM Potassium hydroxide for 4 min to 60 mM at 9 minEluent Source: EG40Temperature: 30 °CFlow Rate: 0.7 mL/minInj. Volume: 5 µL Detection: Suppressed conductivity, ASRS-ULTRA 2-mm, AutoSuppression recycle mode
16393
Concentrator ColumnsForconcentratorwork,whena
singlepistonpumpsuchastheAXPpump(pulsedamperrequired)isusedforsampledelivery,usetheIonPacAG15Guardcolumn,ultratraceanionconcentratorcolumns(UTAC-LP1,UTAC-ULP1,UTAC-XLP1,UTAC-LP2, UTAC-ULP2,orUTAC-XLP2),or thetraceanionconcentratorcolumns
(TAC-ULP1orTAC-2).UsetheUTAC-LP1,UTAC-LP2orthe TAC-LP1whenthesampleisdeliveredwithasyringeorwithalow-pressureautosamplersuchastheAS-DV.
Forconcentratorworkwith a0.4mmcapillarycolumn,usetheIonPacAG15CapillaryGuard columnortheIonSwiftMAC-100 Concentratorcolumn.
6
SPECIFICATIONS
Dimensions: IonPacAS15CapillaryColumn: 0.4×250mm
IonPacAG15CapillaryGuardColumn: 0.4×50mm
IonPacAS15AnalyticalColumn: 2×250,3×150,and4×250mm
IonPacAG15GuardColumn: 2×50,3×30,and4×50mm
IonPacAC15ConcentratorColumn: 2×50and4×50mm
Maximum Operating Pressure: 4000psi(StandardorMicrobore) 5000psi(Capillary)
Mobile Phase Compatibility: pH0–14;0–100%HPLCsolvents
Substrate Characteristics: BeadDiameter: 5µm(3×150mm)
9µm(0.4×250,2×250and 4 × 250 mm)
13µm(AC15)
PoreSize: 100Å(AS15,AG15) Microporous,<10Å(AC15) Crosslinking(%DVB):55%
Latex Characteristics (AC15): LatexCrosslinking:6% LatexDiameter:85nm
Ion-Exchange Group: Surface-functionalizedwithalkanol quaternaryammoniumion(AS15, AG15)Latex-functionalizedwith alkanolquaternaryammoniumion (AC15)
Functional Group Characteristics: Medium–highhydrophobicity(AS15,AG15) Verylowhydrophobicity(AC15)
Capacity: 2.25µeq(0.4×250mmcapillarycolumn) 0.45µeq(0.4×50mmcapillaryguardcolumn) 56.25µeq(2×250mmanalyticalcolumn) 11.25µeq(2×50mmguardcolumn) 2.2µeq(2×50mmconcentratorcolumn) 70µeq(3×150mmanalyticalcolumn) 14µeq(3×30mmguardcolumn) 225µeq(4×250mmanalyticalcolumn) 45µeq(4×50mmguardcolumn) 9µeq(4×50mmconcentratorcolumn)
AC15 Void Volume: 9µL(2×50mm) 210µL(4×50mm)
Column Construction:PEEK®with10–32threadedferrule-styleend fittings.Allcomponentsarenonmetallic.
ORDERING INFORMATION
IntheU.S.,call(800)346-6390orcontacttheDionexRegionalOfficenearestyou. OutsidetheU.S.,orderthroughyourlocalDionexofficeordistributor.Referthefollowingpartnumbers:
AS15 Analytical and Guard Columns Part Number
IonPacAS15-9µmCapillaryColumn(0.4×250mm)..............................................................................................................................075662
IonPacAG15-9µmGuardColumn(0.4×50mm)....................................................................................................................................075663
IonPacAS15-9µmAnalyticalColumn(4×250mm)...............................................................................................................................053940
IonPacAG15-9µmGuardColumn(4×50mm).......................................................................................................................................053942
IonPacAS15-5µmAnalyticalColumn(3×150mm)...............................................................................................................................057594
IonPacAG15-5µmGuardColumn(3×30mm).......................................................................................................................................057597
IonPacAS15-9µmAnalyticalColumn(2×250mm)...............................................................................................................................053941
IonPacAG15-9µmGuardColumn(2×50mm).......................................................................................................................................053943
Trap Columns
CR-ATCContinuouslyRegeneratedAnionTrapColumn(forusewithsystemsequippedwithaneluentgeneratororRFC-30Reagent-Free
Controller)..................................................................................................................................................................................................060477
CR-ATCContinuouslyRegeneratedAnionTrapColumn(Capillary)(forusewithCapillaryAnionColumns).....................................072078
ATC-3AnionTrapColumn(9×24mm)(forusewith4mmcolumns)...................................................................................................059660
ATC-3AnionTrapColumn(4×35mm)(forusewith2mmcolumns)...................................................................................................059661
ATC-HCAnionTrapColumn(forusewiththeEG).................................................................................................................................059604
Trace Anion Concentrator Columns
IonPacAC15ConcentratorColumn(2×50mm;forusewith2-mmand3-mmcolumns)......................................................................055695
IonPacAC15ConcentratorColumn(4×50mm).....................................................................................................................................055694
IonSwiftMAC-100MonolithAnionConcentratorColumn(0.5×80mm)..............................................................................................074702
TAC-LP1TraceAnionConcentrator(4×35mm)....................................................................................................................................046026
TAC-ULP1TraceAnionConcentrator(5×23mm).................................................................................................................................061400
UTAC-LP1UltraTraceAnionConcentratorLowPressure(4×35mm)................................................................................................063079
UTAC-ULP1UltraTraceAnionConcentratorUltraLowPressure(5×23mm).....................................................................................063475
UTAC-XLP1UltraTraceAnionConcentratorExtremelyLowPressure(6×16mm).............................................................................063459
UTAC-LP2UltraTraceAnionConcentratorLowPressure(4×35mm).................................................................................................072779
UTAC-ULP2UltraTraceAnionConcentratorUltraLowPressure(5×23mm).....................................................................................072780
UTAC-XLP2UltraTraceAnionConcentratorExtremelyLowPressure(6×16mm).............................................................................072781
ACES, ASRS, AutoSuppression, IonPac, IonSwift, and Reagent-Free are registered trademarks of Dionex Corporation. PEEK is a trademark of Victrex PLC.
North America
U.S./Canada (847) 295-7500 South America
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