Thermo Scientific Dionex IonPac User manual

PRODUCT MANUAL
IONPAC®FAST ANION ANALYTICAL COLUMN
(4 x 250 mm, P/N SP5516)
QUICKSTART STEPS AND LINKS
Click blue text below to get started.
1. See Section 3, “Operation”. Note operation precautions and chemical purity
requirements.
2. See Section 4.1, “Eluent Preparation". Make the required stock and working solutions
for eluents.
3. See “Quality Assurance Report”. Run the Production Test Chromatogram as a system
check.
4. See Section 4.3, "Standard Operating Conditions" for an example application.
5. See “Column Care" for column cleanup and long-term storage recommendations.
©DIONEX Corporation, 1997, 1998, 2002
Document No. 032882
Revision 05
7 November 2002

Document No. 032882-05 IonPac Fast Anion Page 2 of 12
TABLE OF CONTENTS
SECTION 1 - INTRODUCTION ....................................................................................................... 3
SECTION 2 - INSTALLATION ......................................................................................................... 4
2.1 System Requirements ............................................................................................................................................... 4
SECTION 3 - OPERATION ............................................................................................................... 5
3.1 Operation Precautions .............................................................................................................................................. 5
3.2 Chemicals Required .................................................................................................................................................. 5
SECTION 4 - EXAMPLEAPPLICATIONS...................................................................................... 6
4.1 Eluent Preparation .................................................................................................................................................... 6
4.1.1 PreparationOf100xEluentConcentrates-0.5MNa2CO3/0.0075M NaHCO3.......................................................................................................... 6
4.1.2 Dilution of the Eluents Concentrate ............................................................................................................................7
4.2 Regenerant Preparation ........................................................................................................................................... 7
4.3 Standard Operating Conditions ................................................................................................................................8
SECTION 5 - TROUBLESHOOTING GUIDE ................................................................................. 9
5.1 High Backpressure................................................................................................................................................... 9
5.2 High Background, Noise ........................................................................................................................................ 10
5.3 Poor Peak Resolution ............................................................................................................................................. 10
5.3.1 Lossof Column Efficiency ........................................................................................................................................ 10
5.3.2 Short Retention Times............................................................................................................................................... 11
5.3.3 Poor Resolution of Chloride, Nitrite, and/or Bromide................................................................................................ 11
5.3.4 Poor Resolution of Phosphate and Nitrate................................................................................................................ 11
5.3.5 Poor Resolution of Phosphate and Sulfate ............................................................................................................... 11
5.4 Spurious Peaks ........................................................................................................................................................11
5.4.1 ColumnContamination.............................................................................................................................................. 11
5.4.2 Baseline Upsets ........................................................................................................................................................ 12

Document No. 032882-05 IonPac Fast Anion Page 3 of 12
SECTION 1 - INTRODUCTION
TheIonPacFastAnionAnalyticalColumn(P/N039590)isdesignedspecificallyfortherapidanalysisofanionsindefinedmatrices.
Itprovidesthemostrapidanalysisavailable.Sevencommonanionscanbedeterminedinlessthan3minutes.Itisidealforachieving
maximumthroughputofrelativelysimple,well-characterizedsamples.
The4mmx250mmIonPacFastAnionAnalyticalColumnhasanionexchangecapacityofapproximately8-10µeq/column.This
resin is composed of 15 micron 4% XL polystyrene/ divinylbenzene substrate agglomerated with anion exchange latex and has
nominal efficiency of 10,000 plates/meter for sulfate using standard operating conditions.
TheIonPacFastAnionAnalyticalColumncanbeoperatedatflowratesupto3.0mL/min.Optimally,theIonPacFastAnionAnalytical
Column should generate a system backpressure of approximately 950 psi when operated with an eluent flow rate of 2.0 mL/min.
For any problems that have been encountered in shipping or that are not covered by the appropriate Product Manuals, additional
support can be obtained through any of the DIONEX Regional Offices listed in “DIONEX Worldwide Offices.”
Figure 1

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SECTION2 -INSTALLATION
2.1 System Requirements
TheIonPacFastAnionAnalyticalColumnmustberunonaSeries2000ior4000iIonChromatograph(IC)equippedwithanAnion
MicroMembraneSuppressor,AMMSIII,P/N056750) and a Conductivity Detector.
NOTE
Tosaveregenerantpreparation time,consumption,andwaste, itisrecommended thattheAutoRegenAccessory be
purchased.TheAutoRegenAccessorycanonlybeused with theMicroMembraneSuppressor.
Tominimizethepossibilityofcolumnoverloadandtoobtainmaximumcolumnefficiency,sampleloopvolumesshouldbe20µl-
orsmaller.
This manual assumes that you are already familiar with installation and operation of the Ion Chromatograph (IC) and Anion
MicroMembraneSuppressor(AMMSIII).Ifyoudonotunderstandtheoperationofyoursystem,takethetimetofamiliarizeyourself
with the operator’s manuals for these products before beginning an analysis.
CAUTION
Donotrunsuppressorsover40°C.Ifanapplicationrequiresahighertemperature,placethesuppressoroutsideofthe
oven.

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SECTION 3 - OPERATION
3.1 Operation Precautions
A. The eluent pH should be between 2 and 11. The sample pH should be between 2 and 13. Exceeding the limits of these
pHrangeswill cause Irreversibledamagetothe IonPac FastAnionAnalyticalColumn.Do not usehydroxidetoadjust
the pH of the eluent thus effecting the selectivity of the system. Using hydroxide in the eluent may cause irreversible
damage to the IonPac Fast Anion Analytical Column.
B. Substitution of either an Anion Fiber Suppressor or a Packed-bed Fiber Suppressor will compromise the resolution of
solutepeaksontheIonPacFastAnionAnalyticalColumn.ThesystemshouldbefittedwithanAnionMicroMembrane
Suppressor for best results.
C. Make sure there are no extraneous valves or pieces of tubing in the chromatographic system after the injection valve
(i.e.,betweentheinjectionvalveandtheanalyticalcolumn,theanalyticalcolumnandtheSuppressor,andtheSuppressor
andthedetectorcell).Useonly0.012inch(0.3mm)IDtubing(P/N035548)tomakeconnections.Maketubinglengths
as short as Is practical.
D. Use degassed or helium-purged deionized water with a specific resistance of 18.2 megohm-cm to prepare the eluent
concentrate and eluent. If these are not used, excess dissolved carbon dioxide in the water will affect the carbonate/
bicarbonate ratio in the eluent.
E. TherecommendedregenerantfortheAnionMicroMembraneSuppressor(AMMSIII)is20mNSulfuricAcid.Thereare
several important operating precautions that must be observed in order to successfully use the AMMS III. Study the
AMMS III Product Manual carefully before beginning an analysis.
3.2 Chemicals Required
Obtaining precise and accurate results requires eluents that are free of ionic impurities. Chemicals and deionized water used to
prepareeluentsmustbeofthehighestpurityavailable.Lowtraceimpuritiesandlowparticlelevelsineluentsalsohelpprotectyour
expensive ion exchange analytical column and system components. Dionex cannot guarantee proper column performance when
the quality of the chemicals and water used to prepare eluents has been compromised.
ReagentGradeinorganicchemicalsshould always be used to prepare ionic eluents. Whenever possible, inorganic chemicals that
meet or surpass the latest American Chemical Society standard for purity (universally accepted standard for reagents) should be
used. These inorganic chemicals will detail the purity by having an actual lot analysis on each label.
ThedeionizedwaterusedtoprepareeluentsshouldbeTypeIReagentGradeWaterwithaspecificresistanceof18.2megohm-cm.
Thedeionizedwatershouldbefreeofionizedimpurities,organics,microorganismsandparticulatematterlargerthan0.2µm.Bottled
HPLC-Grade Water should not be used since most bottled water contains an unacceptable level of ionic impurities. Finally,
thoroughly degas all deionized water prior to preparing any eluents.

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SECTION4-EXAMPLEAPPLICATIONS
Separation and elution of common anions on the IonPac Fast Anion Analytical Column has been optimized utilizing a specific
carbonate/bicarbonateeluent.Bothmonovalentanddivalentanionsareelutedinlessthanthreeminutesbasedontheconcentration
and proportions of sodium carbonate and sodium bicarbonate. The Suppressor reaction product is carbonic acid (H2CO3) which
results in a low background conductivity.
4.1 Eluent Preparation
The 2.00 mM Na2CO3/0' 15 mM NaHC03eluent is prepared daily by the dilution of a 100X eluent concentrate. This allows the
chromatographertoeasilyandpreciselypreparelargevolumesofeluentwhileatthesametimeusingaminimumamountofstorage
space.
SincetheIonPacFastAnion Column is susceptible to irreversible damagefromeluentswithpHoutsidethe range of 2 and 11, the
100Xeluent concentrate is also recommended forcolumn cleanup (see, “Column Care”).
4.1.1 Preparation Of 100x Eluent Concentrates - 0.5 M Na2CO3/0.0075 M NaHCO3
A 100X concentrate can be made from either reagent grade chemicals or from DIONEX eluent concentrates.
NOTE
Donotusehydroxide toadjustthepH oftheeluentin ordertoadjusttheion exchangeselectivityofthe system.Using
hydroxideintheeluentmaycause irreversibledamagetotheIonPacFast Anion AnalyticalColumn.
USINGREAGENTGRADESALTS
A. Weigh10.6g of anhydrous Na2CO3and 0.63 g ofNaHCO3intoa500ml- volumetric flask.
B. Add 250mLof degassed, deionizedwaterhaving aspecificresistanceof 18.2megohm-cmtothe flaskandthoroughly
dissolve the Na2CO3and the NaHCO3.
C. Dilute to a final volume with degassed, deionized water having a specific resistance of 18.2 megohm-cm.
USINGDIONEXELUENTCONCENTRATES
Itis possible to dilute the DIONEX 0.5 M Na2CO3concentrate (P/N 037162) and the 0.5 M NaHCO3concentrate (P/N
037163)directlytomakethe eluents, but the dilution factorissolargethattheprecise duplication of the diluted eluent
may be difficult to achieve from one dilution to the next. For the sake of precision and ease of preparation, DIONEX
recommends that the 100X eluent concentrates be prepared from the 0.5 M concentrates for use in making the eluents
A. Add200mLof0.5MNa2CO3concentrate(P/N037162)and15mLof0.5MNaHCO3concentrate(P/N037163)ina500
mLvolumetricflask.
B. Add 250mLof degassed, deionizedwaterhaving aspecificresistanceof 18.2megohm-cmtothe flaskandthoroughly
dissolve the Na2CO3 and the NaHCO3.
C. Dilute the final volume of 500 mL degassed, deionized water having a specific resistance of 18.2 megohm-cm.

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4.1.2 Dilution of the Eluents Concentrate
Dilute 10.0 mL of 100X eluent concentrate to one liter in a volumetric flask, using degassed, deionized water having a specific
resistance of 18.2 megohm-cm. The eluent is now ready for use.
4.2 Regenerant Preparation
Theregenerantis20mNsulfuricacid.Dilute40mL(about40gm)ofAnionRegenerantConcentrate(0.5Nsulfuricacid,P/N037164
orP/N039601)to1Lusingdeionizedwater.IfyouarenotusingtheAutoRegenAccessory(P/N039594),prepareseverallitersof
the regenerant.

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4.3 Standard Operating Conditions
Sample Loop Volume: 20 µL
Analytical Column: IonPac Fast Anion Analytical Column
Eluent: 2.00 mM Na2CO3
0. 15 mM NaHCO3
Eluent Flow Rate: 2.0 mL/min
MMS Suppressor: Anion MicroMembrane Suppressor, AMMS III
MMS Regenerant: 20 mNH2SO4
Regenerant Flow Rate: 3-5 mL/min
Full Scale Range: 30 µS
Expected Background Conductivity: 10 to 15 µS
Expected System Operating Backpressure: 800 to 1000 psi
Analyte mg/L
1. Fluoride 1.5
2. Chloride 2.5
3. Nitrite 7.5
4. Bromide 7.5
5. Nitrate 10
6. Phosphate 15
7. Sulfate 10
Figure 1

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SECTION5- TROUBLESHOOTINGGUIDE
ThepurposeoftheTroubleshootingGuideistohelpyousolveoperatingproblemsthatmayarisewhileusingtheIonPacFastAnion
AnalyticalColumn.FormoreinformationonproblemsthatoriginatewiththeIonChromatograph(IC)ortheAnionMicroMembrane
Suppressor(AMMSIII),refertotheTroubleshootingGuideintheappropriateoperator’smanual.Ifyoucannotsolvetheproblem
onyourown, calltheDionexRegional Office(see,“DIONEXWorldwide Offices”) nearestyou.
5.1 High Backpressure
TotalsystempressurewhenusingtheIonPacFastAnionAnalyticalColumnonlyshouldbelessthan1000psi-Ifthebackpressure
ishigherthan1000psi,it isadvisabletofindoutwhatiscausingthehighpressure.Thesystemshouldbeusedwith anin-linefilter
for the eluents. Make sure you have one in place and that it is not contaminated.
A. Makesurethatthepumpissetto2.0mL/minute.Higherflowrateswillcausehigherpressure.Measurepumpflowrate
with a graduated cylinder and a stopwatch if necessary.
B. Find out what part of the system is causing the high backpressure. It could be a tubing that has plugged or whose walls
are collapsed, an injection valve with a plugged port, the analytical column with particulates plugging the inlet bed
support, a plugged in-line filter, the Anion MicroMembrane Suppressor or the detector.
Tofindoutwhichpartiscausingtheproblem,disconnectthepumpeluentlinefromtheinjectionvalveandturnthepumpon.Watch
the pressure. It should not exceed 50 psi. Continue adding the system’s components (injection valve, analytical column, Anion
MicroMembrane Suppressor (AMMS) and detector) one by one, while watching the pressure. The pressure should increase up
toamaximumof1000psiwhentheanalyticalcolumnisconnected.TheAMMSwilladdupto100psi.Noothercomponentsshould
add more than 100 psi of pressure. Refer to the appropriate manual for cleanup or replacement of the problem component.
C. IftheIonPacFastAnionAnalyticalColumnisthecauseofhighbackpressure,itsinletbedsupportmaybecontaminated.
To change the bed support, follow the instructions below using one of the two spare bed supports included in the Ship
Kit.
1. Disconnect the column from the system.
2. Using two open-end wrenches, carefully unscrew the inlet (top) column fitting.
3. Turn the end fitting over and tap it against a benchtop or other hard, flat surface to remove the bed support and
seal assembly. Discard the old assembly.
4. Placeanewbedsupportassembly(P/N042955)andendfitting(P/N52809).Usetheendofthecolumntocarefully
start the bed support assembly into the end fitting.
5. Screw the end fitting back onto the column. Tighten it fingertight, then an additional 1/4 turn (25 in/lb). Tighten
further only if leaks are observed.

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NOTE
Ifanyofthecolumnpackingbecomeslodgedbetweenthe endofthecolumnandthebedsupportwasherassembly, no
amountoftighteningwillsealthecolumn.Makesurethatthewasherandtheendofthecolumnarecleanbeforescrewing
theendfittingback ontothecolumn.
6. Reconnect the column to the system and resume operation.
5.2 High Background, Noise
In a properly working system, the background conductivity level for the standard eluent systems is shown below:
ELUENT EXPECTEDBACKGROUNDCONDUCTIVITY
2.00mM Na2CO310-15µS
0.15mMNaHCO3
Asystemwithahighbackgroundwillprobablyalsohavehighnoise,withtheresultingincreaseindetectionlimits.Ifthebackground
conductivity increases to above 20 psi check the following items.
A. Make sure that the eluent and regenerant are made correctly as described in Section 4?
B. Make sure that the eluents are made from reagent grade chemicals or better.
C. Make sure that the deionized water used to prepare the reagents has a specific resistance of 18.2 megohm-cm.
D. If the above items have been checked and the problem persists, the Anion MicroMembrane Suppressor (AMMS III)
is probably causing the problem.
1. Check the regenerant flow rate at the suppressor’s RegenOut port to make sure it at least 3 mL/min.
2. Checkthe eluent flow rate. It should be 2.0 mL/min-
3. Preparefreshregenerantsolution.BypasstheRegenRecycleCartridge(ifyouareusinganAutoRegenAccessory).
If the background is high, you probably need to clean or replace your AMMS III. For instructions on how to do
this, refer to the AMMS III Product Manual. If bypassing the Anion AutoRegen Regenerant Cartridge returns the
background to normal, the AutoRegen Regenerant Cartridge may be contaminated or may have expired. Refer to
the Product Manual for the AutoRegen Regenerant Cartridge Refills (Document No. 032852) for complete
instructions.
4. If after cleaning the AMMS III, the background conductivity is still too high, the regenerant is probably
contaminated and needs to be replaced. It is also probable that the cartridge has been contaminated and should
berinsedofcontaminatedregenerant.RefertotheTroubleshootingGuideoftheAutoRegenRegenerantCartridge
InstallationInstructionsandTroubleshootingGuide(DocumentNo.032852)fordetailsonremovingcontaminants
from the AutoRegen Cartridge.
5.3 Poor Peak Resolution
5.3.1 Loss of Column Efficiency
A. Checktoseeifheadspacehasdevelopedintheanalyticalcolumn(e.g.,duetoimproperuseofthecolumnsuchasusing
thecolumnwithorganicsolvents,submittingittohighpressuresorhighpH).Removethecolumn’stopendfitting(see
Section 5. 1, Step C). 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.