Thermo Scientific IONPAC AG2 GUARD COLUMN User manual

PRODUCT MANUAL
IONPAC®AG2 GUARD COLUMN
(4 x 50 mm, P/N SP4834)
IONPAC®AG3 GUARD COLUMN
(4 x 50 mm, P/N 043182)
IONPAC®AG4 GUARD COLUMN
(4 x 50 mm, P/N 035310)
IONPAC®AG5 GUARD COLUMN
(4 x 50 mm, P/N 035396)
IONPAC®CG2 GUARD COLUMN
(4 x 50 mm, P/N 035370)
IONPAC®AS2 ANALYTICAL COLUMN
(4 x 250 mm, P/N SP4831)
IONPAC®AS3 ANALYTICAL COLUMN
(4 x 250 mm, P/N 043181)
IONPAC®AS4 ANALYTICAL COLUMN
(4 x 250 mm, P/N 035311)
IONPAC®AS5 ANALYTICAL COLUMN
(4 x 250 mm, P/N 035395)
IONPAC®CS2 ANALYTICAL COLUMN
(4 x 250 mm, P/N 035371)
QUICKSTART STEPS AND LINKS
Click blue text below to get started.
1. See Section 2, “Operation”. Note operation precautions and chemical purity
requirements.
2. See “Quality Assurance Reports”. Run the Production Test Chromatogram as
a system check.
3. See “Column Care” for column cleanup and long-term storage
recommendations. ©DIONEX Corporation, 1997, 1998, 2002
Document No. 032226
Revision 14
12 November 2002

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 2 of 14
TABLE OF CONTENTS
SECTION 1 - INTRODUCTION ..................................................................................................... 3
1.1 Overview ................................................................................................................................................................... 3
1.2 Chemicals ................................................................................................................................................................. 3
1.3 Column Storage ........................................................................................................................................................ 3
1.4 Recommended Operating Pressures....................................................................................................................... 3
1.5 Applications .............................................................................................................................................................. 3
SECTION 2 - OPERATION ............................................................................................................. 4
2.1 General Operation Precautions .............................................................................................................................. 4
2.2 Chemicals Required ................................................................................................................................................. 4
2.2.1 Inorganic Chemicals .................................................................................................................................................. 4
2.2.2 Solvents .................................................................................................................................................................... 4
2.2.3 DeionizedWater ........................................................................................................................................................ 4
SECTION 3 - STANDARD CONDITIONS .................................................................................... 5
3.1 Standard Reagents ................................................................................................................................................... 5
3.2 Standard Flow Rates and Back Pressures .............................................................................................................. 6
SECTION 4 - INITIALSTART-UP PROCEDURES ...................................................................... 7
SECTION 5 - TROUBLESHOOTING GUIDE ............................................................................... 8
5.1 High Back Pressure ................................................................................................................................................ 8
5.1.1 Finding the Source of High System Pressure............................................................................................................ 8
5.1.2 Replacing Column Bed SupportAssemblies ............................................................................................................. 9
5.1.3 Bed Support Descriptions ....................................................................................................................................... 10
5.2 High Background or Noise .................................................................................................................................... 12
5.2.1 Preparation of Eluents ............................................................................................................................................. 12
5.2.2 A ContaminatedAnion Trap Column ...................................................................................................................... 12
5.2.3 AContaminated Guard orAnalytical Column ......................................................................................................... 12
5.2.4 Contaminated Hardware .......................................................................................................................................... 12
5.2.5 A Contaminated Self-Regenerating Suppressor (SRS™) or the MicroMembrane™ Suppressor (MMS) ............... 13
5.3 Poor Peak Resolution ............................................................................................................................................ 13
5.3.1 Lossof Column Efficiency ...................................................................................................................................... 13
5.3.2 Poor Resolution Due to Shortened Retention Times .............................................................................................. 13
5.3.3 Loss of Front End Resolution ................................................................................................................................. 14
5.4 Spurious Peaks ...................................................................................................................................................... 14

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 3 of 14
SECTION 1 - INTRODUCTION
1.1 Overview
Thismanualdescribeshowtopreparethiscolumnforoperation.Theinitialstart-upprocedureusuallyconsistsofinstallingacolumn
in the Chromatography Module, flushing it with deionized water to remove the storage solution, and equilibrating it with eluent.
1.2 Chemicals
Thechemicalsusedtomakeeluents,standards,regenerantsandpost-columnreagentsmustbeofveryhighpurityinordertoobtain
reliable, consistent and accurate analytical results. Before starting an analysis, consult Section 2.2, “Chemicals Required,” for
chemicalpurityrequirements.
1.3 Column Storage
If a column will not be used within one week after testing, prepare it for long-term storage. Flush the column first with deionized
water and then with the storage solution specified in Section 3, “Standard Conditions,” of this manual. Cap both ends securely,
using the plugs supplied with the column.
1.4 Recommended Operating Pressures
Operatingacolumnaboveitsrecommendedpressurelimitcancauseirreversiblelossofcolumnperformance.SeeTable2,“Standard
Flow Rates and Back Pressures,” for standard and maximum back pressures.
1.5 Applications
For help in selecting the correct column for your application, contact the nearest DIONEX Office (see, “DIONEX Worldwide
Offices”).
Alwaysrememberthatassistanceisavailableforanyproblemthatmaybeencounteredduringtheshipmentoroperation
of DIONEX instrumentation and columns through the DIONEX North America Technical Call Center at 1-800-
DIONEX-0(1-800-346-6390)orthroughanyoftheDIONEXOfficeslisted in, “DIONEXWorldwideOffices.”

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 4 of 14
SECTION 2 - OPERATION
2.1 General Operation Precautions
2.2 Chemicals Required
Obtaining reliable, consistent and accurate results requires eluents that are free of ionic and spectrophotometric impurities.
Chemicals,solventsand deionized water usedtoprepareeluentsmust be of thehighestpurityavailable.Low trace impurities and
lowparticlelevels in eluents alsohelptoprotect your ion exchangecolumnsandsystem components. DIONEX cannotguarantee
propercolumn performancewhenthe qualityofthechemicals,solventsandwaterused toprepareeluents hasbeencompromised.
2.2.1 Inorganic Chemicals
ReagentGrade inorganic chemicals should always be used toprepare ionic eluents. Whenever possible, inorganic chemicals that
meetorsurpassthelatestAmericanChemicalSocietystandardforpurityshouldbeused.Theseinorganicchemicalswilldetailthe
purity by having an actual lot analysis on each label.
2.2.2 Solvents
CAUTION
Eluents used on columns containing low cross-linked resins must contain less than 5% organic solvents.
Ifsmallamountsofsolventsareaddedtoioniceluentstomodifytheionexchangeprocessorimprovesamplesolubility,thesolvents
usedmustbefreeofionicimpurities.However,sincemostmanufacturersofsolventsdonottestforionicimpurities,itisimportant
that the highest grade of solvents available be used. Currently, several manufacturers are making ultrahigh purity solvents that
are compatible for HPLC and spectrophotometric applications. These ultrahigh purity solvents will usually ensure that your
chromatographyisnotaffectedbyionicimpuritiesinthesolvent.CurrentlyatDIONEX,wehaveobtainedconsistentresultsusing
High Purity Solvents manufactured by Burdick and Jackson and Optima®Solvents by Fisher Scientific.
2.2.3 Deionized Water
Thedeionizedwater usedtoprepareeluents shouldbeDegassed Type I Reagent Grade Water with aspecificresistanceof 18.2
megohm-cm.Thedeionizedwatershouldbefreeofionizedimpurities,organics,microorganismsandparticulatematterlargerthan
0.2µm.BottledHPLC-GradeWater(withtheexceptionofBurdick&Jackson)shouldnotbeusedsincemostbottledwatercontains
an unacceptable level of ionic impurities. Finally, thoroughly degas all deionized water prior to preparing any eluents.
CAUTION
< 5% Organic Solvent in the Eluent
Filter and Degas Eluents
Filter Samples

IonPac AS2, AS3, AS4, AS5, CS2 Manual Document No. 032226-14 Page 5 of 14
SECTION 3 - STANDARD CONDITIONS
3.1 Standard Reagents
Table 1
Storage Solutions, Eluents and Regenerants
Column Storage Standard Standard
Solution Eluent Regenerant
ANIONANALYTICALANDGUARDCOLUMNS
IonPac®AS2/AG2 100 mM NaOH 3 mM Na2CO3/2 mM NaOH 10X Eluent Concentration
IonPacAS3/AG3 100 mM NaOH 2.2 mM Na2CO3/2.8 mM NaHCO310X Eluent Concentration
IonPacAS4/AG4 100 mM NaOH 2.25 mM Na2CO3/2.8 mM NaHCO310X Eluent Concentration
IonPacAS5/AG5 100 mM NaOH 2.8 mM Na2CO3/2.2 mM NaHCO310X Eluent Concentration
CATIONANALYTICALANDGUARDCOLUMNS
IonPac CS2/CG2 100 mM NaOH 10 mM Oxalic/7.5 mM Citric Acids 10X Eluent Concentration
(pH 4.35)

IonPac AS2, AS3, AS4, AS5, CS2 Manual Document No. 032226-14 Page 6 of 14
3.2 Standard Flow Rates and Back Pressures
Table 2
Standard Flow Rates and Back Pressures
Column Standard Expected Maximum
FlowRate Back Pressure Back Pressure
AnionAnalyticalandGuardColumns
IonPac AS2/AG2 3.0mL/min 600 psi/200 psi 1,500 psi
IonPac AS3/AG3 3.0mL/min 600 psi/200 psi 1,500 psi
IonPac AS4/AG4 2.0mL/min 1,000 psi/300 psi 2,000 psi
IonPac AS5/AG5 2.0mL/min 1,000 psi/300 psi 2,000 psi
Cation Analytical and Guard Columns
IonPacCS2/CG2 2.3mL/min 650 psi/150 psi 1,500 psi

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 7 of 14
SECTION4 -INITIAL START-UPPROCEDURES
Fortheinitialstart-upofbothanionandcationanalyticalcolumns,preparetheeluentlistedonthetestchromatogram,setthepump
to the proper flow rate and perform the following initial start-up procedures. In the case of a guard or suppressor column, use the
test conditions on the production test chromatogram for the analytical column required for the application.
A. Connect the column directly to the pump with a short piece of tubing.
B. Direct the effluent of the column to a separate waste container.
C. Pump10mL(30mLforpacked-bedsuppressors)ofdeionizedwaterthroughthecolumnatthestandardflowratelisted
in Table 2, “Standard Flow Rates and Back Pressures.”
D. Assemble the system (trap, concentrator, guard, analytical and suppressor columns depending on the application).
E. Pump10mLofthestandardproductiontesteluentthatislistedontheAnalyticalColumnTestChromatogram,through
the System to equilibrate the columns.
F. PerformtheProductionTestChromatogramtotestthecolumnandsystemperformance.Notethatguardandanalytical
columns are fully equilibrated when successive runs have the same solute retention times.
NOTE
IonPac FastAnionAnalytical Column
You must use a 20 µLinjection loop with the IonPac FastAnion
to prevent excessive system band broadening and column overloading.
Maintain the eluent at between pH 2 and 11. Do not use hydroxide eluents.

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 8 of 14
SECTION5-TROUBLESHOOTING GUIDE
ThepurposeoftheTroubleshooting Guide is to help you solve operatingproblemsthatmayarisewhileusingDIONEXcolumns.
Formoreinformation on problemsthatoriginatewiththe Ion Chromatograph(IC)orthesuppressor, refer totheTroubleshooting
Guide in the appropriate operator’s manual. If you cannot solve the problem on your own, call the nearest DIONEX Office (see,
“DIONEXWorldwideOffices”).
5.1 High Back Pressure
5.1.1 Finding the Source of High System Pressure
Totalsystempressure when using specific DIONEX columns is flow rate dependent.Referto Table 2, “Standard Flow Rates and
Back Pressures,” for specific flow rates and back pressures for the column system that your are operating. If the system pressure
ismorethan20%higherthanthetotalbackpressureestimatedfromthebackpressureslistedinTable2,“StandardFlowRatesand
BackPressures,”itisadvisabletofindoutwhatiscausingthehighsystempressure.ThesystemshouldbeusedwithaHigh-Pressure
In-LineFilter(P/N035331)fortheeluentswhichispositionedbetweenthepumppressuretransducerandtheinjectionvalve.Make
sure you have one in place and that it is not contaminated.
A. Make sure thatthe pump is set to the correct eluentflow rate. Higherthanrecommendedeluentflowrateswillcause
higher pressure. Measure the pump flow rate if necessary with a stop watch and graduated cylinder.
B. Find out what part of the system is causing the high pressure. Itcouldbeapieceoftubingthathaspluggedorwhose
wallsarecollapsed,aninjectionvalvewithapluggedport,acolumnwithparticulatespluggingthebedsupport,aplugged
High-Pressure In-Line Filter, the suppressor or the detector cell.
To find out which part of the chromatographic system is causing the problem, disconnect the pump eluent line from the injection
valveandturnthepumpon. Watch the pressure; it should not exceed 50psi.Continueaddingthesystem’scomponents(injection
valve, column(s), suppressor and detector) one by one, while watching the system pressure. The pressure should increase up to
amaximumwhenthecolumn(s)areconnected.ThismaximumsystempressurecanbeestimatedfromthedatainTable2,“Standard
Flow Rates and Back Pressures.” No other components should add more than 100 psi of pressure. If high system back pressure
isfoundtobeduetoaspecificsystemcomponent,refertotheappropriatemanualforcleanuporreplacementofproblemcomponent.

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 9 of 14
5.1.2 Replacing Column Bed Support Assemblies
If the column inlet bed support is determined to be the cause of the high back pressure, it should be replaced. To change the inlet
bed support assembly, refer to the following instructions, using one of the two spare inlet bed support assemblies included in the
ShipKit.
A. Disconnect the column fromthe system.
B. Carefully unscrew the inlet (top) column fitting,using twoopenendwrenches.
C. Remove the bed support. Turn the end fitting over and tap it against a benchtop or other hard, flat surface to remove
the bed support and seal assembly. If the bed support must be pried out of the end fitting, use a sharp pointed object
suchasapairoftweezers,butbecarefulthatyouDO NOTSCRATCHTHEWALLSOF THE ENDFITTING.Discard
the old bed support assembly.
D. Place a new bed support assembly into the end fitting. Makesure thattheendof the columntubeisclean and freeof
anyparticulatemattersothatitwillproperlysealagainstthebedsupportassembly.Usetheendofthecolumntocarefully
start the bed support assembly into the end fitting. Part numbers for bed supports and other DIONEX components can
befoundin,“DIONEXProductSelectionGuide.”
CAUTION
Ifthecolumntubeendisnotcleanwheninsertedintotheendfitting,particulatemattermayobstructapropersealbetween
theendofthecolumntubeandthebedsupportassembly.Ifthisisthecase,additionaltighteningmaynotsealthecolumn
but instead damage the column tube or the end fitting.
E. Screw the endfitting back onto the column. Tightenitfingertight,thenanadditional1/4turn(25inxlb).Ifthecolumn
continuestoleak, contactyournearestDIONEX Office(see,“DIONEXWorldwide Offices”).
F. Reconnect thecolumn tothesystem andresume operation.
NOTE
Replace the outlet bed support ONLY if high pressure persists after replacement of the inlet fitting.

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 10 of 14
5.1.3 Bed Support Descriptions
The following bed support assemblies are supplied with the different DIONEX Column Lines:
ColumnLine Assembly Component
Description P/N Descriptions
4-mmHPIC(Tefzel®) 035843 Bed Support
030838 O-Ring
FLOW
O-RING
BED SUPPORT

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 11 of 14
ColumnLine Assembly Component
Description P/N Descriptions
4-mmIonPac
(1/4-28LiquidLineFitting) 042310 Bed Support Assembly
041375 Bed Support
039835 Seal Washer
4-mmIonPac
(10-32LiquidLineFitting) 042955 Bed Support Assembly
041375 Bed Support
042956 Seal Washer
BED SUPPORT
CHROMATOGRAPHY
IonPac
AS4
P/N35311 S/N 9835
FLOW

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 12 of 14
5.2 High Background or Noise
In a properly working system, the background conductivity level for the standard eluent system is shown in Table 1, “Storage
Solutions, Eluents and Regenerants.” If the background conductivity is higher than listed in Table 1, “Storage Solutions, Eluents
and Regenerants,” check for eluent and system contamination as follows.
5.2.1 Preparation of Eluents
A. Make sure thatthe eluentsand the regenerantare made correctly.
B. Makesure thatthe eluents aremade fromchemicalswith therecommended purity.
C. Make sure that the deionized water used to prepare the reagents has a specific resistance of 18.2 megohm-cm .
5.2.2 A Contaminated Anion Trap Column
Ifyouaredoinggradientanalysis,anAnionTrapColumn(ATC)shouldbeinstalledbetweenthepressuretransduceronthegradient
pump the injection valve. If it has not been installed, install one and watch the background conductivity. If the background
conductivity decreases, the ATC is trapping contaminants from the eluent. The eluents probably have too many impurities (see
Section5.2.1,“PreparationofEluents”).
Ifthe ATCisalready installed,removeit. Ifthebackgroundconductivitydecreases,theATCisthesourceof thehighbackground
conductivity.
A. Disconnectthe ATCfrom theinjectionvalve anddirect the outletto waste.
B. Flushthe ATCwith200 mLof70 mMNa2B4O7toremove anytrappedimpurities.
C. Equilibrate the ATC with the strongest eluent used during the gradient run at the flow rate specified in Table 2,
“StandardFlow Ratesand BackPressures.”
D. Ifthe problempersists, replacethe ATC.
5.2.3 A Contaminated Guard or Analytical Column
Remove the guard and analytical columns from the system. Is the background conductivity still high? If the column is the cause
of the high background conductivity, clean the column as instructed in Section 6.3, “Column Cleanup.”
5.2.4 Contaminated Hardware
To eliminate the hardware as the source of the high background conductivity, bypass the suppressor and pump deionized water
with a specific resistance of 18.2 megohm-cm through the system. The background conductivity should be less than 2 µS. If it is
not, check the detector/conductivity cell calibration by injecting deionized water directly into it. See the appropriate manual for
details.

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 13 of 14
5.2.5 A Contaminated Self-Regenerating Suppressor (SRS™) or the MicroMembrane™Suppressor (MMS)
If the above items have been checked and the problem persists, the SRS or the MMS is probably causing the problem.
A. ChecktheregenerantflowrateattheREGENOUTportoftheSRSortheMMS.Fortheexampleisocraticapplications,
this flow rate should be 3 - 5 mL/min in the Chemical Suppression Mode of operation.
B. Check the eluent flow rate. Theeluentflowrateformost4-mmapplicationsshouldbe2.0mL/min.RefertotheAnion
Self-Regenerating Suppressor Product Manual (Document No. 031367), the Cation Self-Regenerating Suppressor
Product Manual (Document No. 031370), the Anion MicroMembrane Suppressor Product Manual (Document No.
031728) or the Cation MicroMembrane Suppressor Product Manual (Document No. 031728) to ensure that the eluent
is within suppressible limits.
C. Ifyou areusing an AutoRegen®Accessorywith theSRS(in theChemical Suppression Mode)or theMMS,prepare
fresh regenerant solution. Test both the suppressor and the AutoRegen Regenerant Cartridge for contamination.
1. IfthebackgroundconductivityishighafterpreparingfreshregenerantandbypassingtheAutoRegenRegenerant
Cartridge,youprobably needtoclean orreplaceyour SRSor MMS.
2. Ifthebackground conductivityislowwhenfreshlypreparedregenerantisrunthroughtheSRSorMMSwithout
anAutoRegen Accessory in-line,test theAutoRegen RegenerantCartridge toseeif itis expended.Connectthe
freshly prepared regenerant to the AutoRegen Regenerant Cartridge. Pump approximately 200 mL of regenerant
through the AutoRegen Regenerant Cartridge to waste before recycling the regenerant back to the regenerant
reservoir.IfthebackgroundconductivityishighafterplacingtheAutoRegenAccessoryin-line,youprobablyneed
to replace the AutoRegen Regenerant Cartridge. Refer to the “AutoRegen Regenerant Cartridge Refill Product
Manual”(Document No.032852)forassistance.
5.3 Poor Peak Resolution
Poor peak resolution can be due any or all of the following factors.
5.3.1 Loss of Column Efficiency
A. Checkto seeif headspacehas developedin the guardor analyticalcolumn. Thismaybeduetotheimproperuseofthe
column such as submitting it to high pressures. Remove the column’s top end fitting (see Section 5.1.2, “Replacing
Column Bed Support Assemblies”). If the resin does not fill the column body all the way to the top, the resin bed has
collapsed, creating a headspace. The column must be replaced.
B. Extra-columneffects can result in sampleband dispersion,making the peaks' elution lessefficient. Makesureyou
are using tubing with an ID of no greater than 0.012" to make all eluent liquid line connections between the injection
valve and the detector cell inlet, and that the tubing lengths are as short as possible. Check for leaks.
5.3.2 Poor Resolution Due to Shortened Retention Times
Even with adequate system and column efficiency, resolution of peaks will be compromised if analytes elute too fast.
A. Check the flow rate. Seeiftheeluentflowrateisfasterthantheflowratespecifiedbytheanalyticalprotocol.Measure
the eluent flow rate after the column using a stopwatch and graduated cylinder.
B. Checkto seeifthe eluent compositionsandconcentrations arecorrect.Aneluentthatistoostrongwillcausethepeaks
to elute faster. Prepare fresh eluent. If you are using a gradient pump to proportion the eluent, components from two
or three different eluent reservoirs, the resulting eluent composition may not be accurate enough for the application.
Use one reservoir containing the correct eluent composition to see if this is the problem. This may be a problem when

IonPac AS3, AS4, AS5, CS2 Document No. 032226-14 Page 14 of 14
one of the proportioned eluents is less than 5%.
C. Columncontamination canleadto alossof columncapacity.Thisisbecausealloftheionexchangesiteswillnolonger
beavailableforthesampleions.Polyvalentanionsmightbeconcentratingonthecolumn.RefertoSection6.3,“Column
Cleanup,” for recommended column cleanup procedures.
Possiblesourcesofcolumncontaminationareimpuritiesinchemicalsandinthedeionizedwaterbeingused.Beespecially
careful to make sure that the recommended chemicals are used. The deionized water should have a specific resistance
ofatleast18.2 megohm-cm.
D. Dilutingthe eluentwillimprovepeak resolution, butwillalsoincrease theanalytes’retentiontimes.Ifa10%dilution
of the eluent is not sufficient to obtain the desired peak resolution, or if the resulting increase in retention times is
unacceptable, clean the column (see Section 6.3, “Column Cleanup”).
Aftercleaning the column, reinstall it in the system and let it equilibrate with eluent for about 30 minutes. Thecolumn
is 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. If you need
assistance in solving resolution problems, contact the nearest DIONEX Office (see, “DIONEX Worldwide Offices”).
5.3.3 Loss of Front End Resolution
Ifpoorresolutionsandefficienciesareobservedfortheveryearlyelutingpeaksnearthesystemvoidvolumecomparedtothelater
eluting peaks, check the following:
A. Impropereluent concentrationmaybethe problem.Remaketheeluentasrequiredforyourapplication.Ensurethatthe
water and chemicals used are of the required purity.
B. Columnoverloading maybe theproblem.Reducetheamountofsampleionsbeinginjectedontotheanalyticalcolumn
by either diluting the sample or injecting a smaller volume onto the column.
C. Sluggish operation of the injection valve may be the problem. Checktheairpressureandmakesurethereareno gas
leaks or partially plugged port faces. Refer to the valve manual for instructions.
D. Improperlysweptoutvolumesanywhereinthesystempriortotheguard andanalyticalcolumnsmaybetheproblem.
Swapcomponents,oneatatime,inthesystempriortotheanalyticalcolumnandtestforfront-endresolutionafterevery
system change.
5.4 Spurious Peaks
A. Thecolumns maybecontaminated. Ifthesamplescontainanappreciablelevelofpolyvalentionsandthecolumnisused
withaweakeluentsystem,polyvalentanionsmaycontaminatetheanalyticalcolumn.Theretentiontimesfortheanalytes
willthendecreaseandspurious,inefficient(broad)peakscanshowupatunexpectedtimes.Cleanthecolumnasindicated
inSection6.3,“ColumnCleanup”.
Ifyouneedassistanceindeterminingthebestwaytocleanstronglyretainedsolutesinyour specific sample matrix off
ofDIONEXcolumns,contactthenearestDIONEXOffice(see,“DIONEXWorldwideOffices”).
B. The injection valve may need maintenance. Whenaninjectionvalveisactuated,thepossibilityofcreatingabaseline
disturbanceexists.Thisbaselineupsetcanshowupasapeakofvaryingsizeandshape.Itwillhappenwhentheinjection
valve needs to be cleaned or retorqued (see Valve Manual). 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 as long as they do not interfere with the quantification of the peaks of interest.
Ifcleaningandretorquingthevalvedoesnothelp,replacethevalve.ConsultthenearestDIONEXOffice(see,“DIONEX
Worldwide Offices”) for help in services or replacing a suspect valve.

IonPac®AS2
Analytical (4 x 150 mm)
Product No. SP4831
Serial No. : 0019 Pressure (PSI) : 290 Date : 11/19/99 9:46:28 AM
02.00 4.00 6.00 8.00 10.00 12.00 14.00
Minutes
-2.0
0
2.0
4.0
6.0
8.0
10.0
µS
0019
1
2
34
Eluent: 3 mM Na2CO3/2 mM NaOH
Flow Rate: 3.0 mL/min
Detection: Suppressed Conductivity at 30 µSFS
ASRS®-ULTRA
AutoSuppression®Recycle Mode
Injection Volume: 100 µL
Storage Solution: 100 mM NaOH
Peak Information : Found Components
Peak
No.
1
2
3
4
Retention
Time
0.53
2.85
7.81
10.38
Name
Fluoride
Chloride
Phosphate
Sulfate
(mg/L)
2.0
3.0
15.0
15.0
Efficiency
1729
1088
760
789
Asymmetry
(10%)
3.0
1.1
1.0
1.0
Resolution
11.73
6.73
1.97
n/a
File Name : I:\LBURHANUDIN\QA REPORT BOOK _PDF_DXD_FILES\SP4831_AS2 _C001.DXD

IonPac®AS3
Analytical (4 x 250 mm)
Product No. 43181
Serial No. : 3649 Pressure (PSI) : 480 Date : 5/18/00 10:04:50 AM
Eluent: 2.8 mM NaHCO3/ 2.2 mM Na2CO3
Flow Rate: 3.0 mL/min
Detection: Suppressed Conductivity at 30 µSFS
ASRS®-ULTRA
AutoSuppression®Recycle Mode
Injection Volume: 50 µL
Storage Solution: 0.1 M NaOH
02.00 4.00 6.00 8.00 10.00 12.00
Minutes
-2.0
0
2.0
4.0
6.0
8.0
10.0
12.0
14.0
µS
3649
1
2
345
Peak Information : Found Components
Peak
No.
1
2
3
4
5
Retention
Time
0.76
1.79
4.08
6.07
8.52
Name
Fluoride
Chloride
Phosphate
Nitrate
Sulfate
(mg/L)
2.0
3.0
15.0
10.0
15.0
Efficiency
4500
3009
1961
1635
2076
Asymmetry
(10%)
1.6
1.1
1.0
2.1
1.0
Resolution
11.72
9.21
4.13
3.64
n/a
File Name : C:\PEAKNET\DATA\EXAMPLES\43181 AS3_004.DXD

IonPac®AS4
Analytical (4 x 250 mm)
Product No. 35311
Serial No. : 16 Pressure (PSI) : 710 Date : 9/7/00 8:15:02 AM
Eluent: 2.8 mM NaHCO3/ 2.2 mM Na2CO3
Flow Rate: 2.0 mL/min
Detection: Suppressed Conductivity at 30 µSFS
ASRS®-ULTRA
AutoSuppression®Recycle Mode
Injection Volume: 50 µL
Storage Solution: 0.1 M NaOH
01.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
Minutes
-2.0
0
2.0
4.0
6.0
8.0
10.0
12.0
14.0
16.0
µS
16
1
2
3
4
5
Peak Information : Found Components
Peak
No.
1
2
3
4
5
Retention
Time
0.79
1.56
2.59
4.87
6.86
Name
Fluoride
Chloride
Phosphate
Nitrate
Sulfate
(mg/L)
5.0
20.0
10.0
15.0
25.0
Efficiency
2550
2625
2437
1285
2149
Asymmetry
(10%)
2.6
1.1
0.9
2.9
1.2
Resolution
8.42
6.21
6.09
3.51
n/a
File Name : C:\PEAKNET\DATA\EXAMPLES\35311 AS4_A006.DXD

IonPac®AS5
Analytical (4 x 250 mm)
Product No. 35395
Serial No. : 8874 Pressure (PSI) : 871 Date : 1/9/01 5:27:47 PM
01.0 2.0 3.0 4.0 5.0 6.0 7.0
Minutes
0
2.0
4.0
6.0
8.0
10.0
12.0
14.0
µS
8874
1
2
3
4
Eluent: 2.2 mM Na2CO3/ 2.8 mM NaHCO3
Flow Rate: 2.0 mL/min
Detection: Suppressed Conductivity
ASRS®-ULTRA
AutoSuppression®Recycle Mode
Injection Volume: 50 µL
Storage Solution: 0.1 M NaOH
Peak Information : Found Components
Peak
No.
1
2
3
4
Retention
Time
0.77
1.09
1.96
5.27
Name
Fluoride
Chloride
Nitrate
Sulfate
(mg/L)
2.0
3.0
10.0
15.0
Efficiency
2071
1817
3065
4122
Asymmetry
(10%)
3.0
1.5
1.8
1.5
Resolution
3.70
7.19
14.13
n/a
File Name : C:\PEAKNET\DATA\EXAMPLES\35395 AS5 4MM_011.DXD

IonPac®CS2
Analytical (4 x 250 mm)
Product No. 35371
Serial No. : 4604 Pressure (PSI) : 570 Date : 4/27/00 11:32:21 AM
01.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00
Minutes
0
-2
5.00x10
-1
1.00x10
-1
1.50x10
-1
2.00x10
-1
2.50x10
-1
3.00x10
-1
3.50x10
-1
4.00x10
-1
4.50x10
AU
4604
1
23
Eluent: 10 mM Oxalic acid/7.5 mM Citric
acid, pH 4.35 w/LiOH
Eluent Flow Rate: 1.0 mL/min
Post-Column Reagent: 3x10-4M 4-(2-
pyridlazo)resorcinol in 3.0 MNH4OH/1.0 M
CH3COOH
PCR Flow Rate: 0.5 mL/min
Detection: Absorbance at 520 nm, 0.5 AUFS
Injection Volume: 50 µL
Storage Solution: 0.1 M NaOH
Peak Information : Found Components
Peak
No.
1
2
3
Retention
Time
1.25
4.08
5.71
Name
Copper
Zinc
Cobalt
(mg/L)
1.0
2.0
2.0
Efficiency
2158
3922
1801
Asymmetry
(10%)
2.5
1.2
1.2
Resolution
15.41
4.09
n/a
File Name : C:\PEAKNET\DATA\EXAMPLES\35371 CS2 4MM_B010.DXD

IonPac AS3, AS4, AS5, CS2 Column Care Document No. 03226C14 Page 1 of 4
COLUMN CARE
RECOMMENDED OPERATION PRESSURES
Operating a column above its recommended pressure limit can cause irreversible loss of column performance. The maximum
recommended operating pressure for the columns covered by this manual are listed in Table 2, "Standard Flow Rates and Back
Pressures."
COLUMN STORAGE
For short-term storage, the strongest eluent in use can be used as the storage solution. For long-term storage, use the storage
solutionlistedinTable1,"StorageSolutions,EluentsandRegenerants."Flushthecolumnfor10minuteswiththestoragesolution.
Cap both ends securely, using the plugs supplied with the column.
COLUMN CLEANUP
The following column cleanup protocols have been divided into three general isocratic protocols to remove acid-soluble, base-
solubleororganic contaminants. They can be combined into one gradient protocol ifdesiredbut the following precautions should
be observed.
Always ensure that the cleanup protocol used does not switch between eluents which may create high pressure eluent interface
bands in the column. High pressure bands can disrupt the uniformity of the packing of the column bed and irreversibly damage
the performance of the column. High pressure bands in the column can be created by pumping successive eluents through the
column that are not miscible or that have eluent components that will precipitate out in the other eluent. The precipitation of the
salts in solvents during column rinses can result in very high pressure bands. High viscosity mixing bands can be created between
two eluents having solvents with a very high energy of mixing.
CAUTION
Eluents used on columns containing low cross-linked resins must contain less than 5% organic solvents.