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www.phenomenex.com

Phenomenex products are available worldwide. For the distributor in your country, contactPhenomenex USA, International Department by telephone, ax or email: [email protected].

AustraliaPO Box 4084Lane Cove, NSW 2066Australia

[email protected]

ail:

el.:

ax:

ail:

AustriaZeppelinstr. 563741 AschaffenburgGermany

[email protected]

Canada411 Madrid Ave.Torrance, CA90501-1430USA

(800) 543-3681(310) [email protected]

DenmarkGydevang 39-413450AllerdDenmark

4824 80484810 [email protected]

FranceParc des Grillons, Bat.360 route de Sartrouville78232 Le Pecq CedexFrance

01 30 09 21 1001 30 09 21 [email protected]

GermanyZeppelinstr. 563741 AschaffenburgGermany

[email protected]

IrelandQueens Avenue,Hurdseld Ind. Est.,Maccleseld, CheshireSK10 2BN, UK

01 247 5405+44 [email protected]

ItalyVia Emilia, 51/C40011 Anzola dellEmilia (BO)Italy


New ZealandP O Box 31-601Milford 0741North Shore CityNew Zealand

[email protected]

Puerto Rico273 Sierra Morena,Suite #104San Juan,Puerto Rico 00926

(800) 541-HPLC(310) [email protected]

United KingdomQueens Avenue,Hurdseld Ind. Est.,Maccleseld, CheshireSK10 2BN, UK

[email protected]

USA411 Madrid Ave.Torrance, CA90501-1430USA

(310) 212-0555(310) [email protected]

TROUBLESHOOTING TOOLS

PRE-INSTALLATION CHECK LIST

CRITICAL COLUMN INSTALLATION STEPS

Replace oxygen, moisture and hydrocarbon trapsas necessary.

Check gas cylinder pressures to ensure that an adequatesupply o carrier, make-up and uel gases are available.Carrier gases should be o the highest purity.Note: It is critical that oxygen and water be removedrom the carrier gas by the appropriate use o ltersand adsorbents.

Ensure that the injection port is clean and reeo sample residues, septum, or capillary debris.

Check and replace as necessary critical injectorcomponents such as seals, liners, and septa.

Check and replace detector seals as necessary. Careully inspect your column or damage or breakage.

Flow meter Leak detector New syringe Column perormance test sample

Methane or other non-retained compound Reerence column New septa, errules and injector liners Instrument manuals

INJECTOR INSTALLATION:

Recommendation:

GC columns do not have a specic directional fow whenreceived rom the manuacturer. Upon initial use o yournew Zebron column, Phenomenex recommends the practiceo dedicating one specic end o the column or injectorinstallation only. This is particularly important when dealingwith active/caustic or contaminating compounds. I these

compounds are routinely injected onto the column,degradation o the phase will occur - leading to higherbleed. A typical rst step to remedying (removing) thisbleed would be to trim 10 cm rom the ront (injector)end o the column and keep trimming this inlet end o thecolumn as necessary. Trying to remedy any bleed issuesby trimming the column may not work i both ends havebeen interchangeably installed into the inlet.

1. Place a capillary nut and errule on the injector end othe GC column, allowing a section o column to protrude.Trim one to two centimeters rom the protruding end toremove errule contamination that may have entered thecolumn. Inspect the cut with a magnier to ensure that asmooth, clean, square-cut edge has been made - recuti necessary.

2. Careully hang the column in the GC oven, beingcautious not to scratch or damage the polyimidecoating on the capillary tubing. Rotate the column toavoid sharp bends o the capillary column and anycontact o the column with oven suraces.

3. Insert the column into the injector exactly the correctdistance specied in the instrument manual. Tighten the

errule nut nger-tight then 1/2 turn with a wrench. I thecolumn can still be moved, tighten another 1/4 turn untilthe column is secure.

4. Adjust the carrier gas to obtain the fow rate listed on thetest chromatogram.

DETECTOR INSTALLATION:

Note: For users with sensitive detectors such as MS andECD, column conditioning steps should be perormed beoreinstalling the column to prevent contamination and requentmaintenance o the detector.

1. Place the column nut and errule past the end o thecolumn and cut a centimeter or two o the end o thecolumn. Be sure that the errule is the right size and

pointing in the correct direction. Inspect the cut witha magnier and ensure that the cut is square and smooth.Recut i needed.

2. Insert the outlet end o the column into the detectorexactly the distance prescribed in the instrumentmanual. Distances will vary between detectors. Tightenthe errule nut nger-tight then 1/2 turn with a wrench.

I the column can still be moved, tighten another1/4 turn until the column is secure.

3. Inspect the column connections or leaks using anelectronic leak detector. Leaks at the inlet end mayintroduce oxygen to the column that will result inincreased column bleed and damage to the columnphase.

COLUMN CONDITIONING:

1. Allow sucient time or the carrier gas to fow throughthe column to purge any oxygen that may be in thesystem.

2. Raise the temperature o the column to the maximumisothermal operating temperature that is listed on theindividual Zebron GC Column Test Report. Maintainthis temperature until a constant baseline is achieved.

Conditioning times will depend on the phase identity andthickness, with thicker lms taking longer to stabilize.I necessary in order to minimize the downtime o theinstrument, columns can be conditioned overnightat the maximum isothermal temperature.

INSTALLATION TESTING:

1. Inject a detectable unretained sample, such as methaneor an FID, to determine dead volume time and lineargas velocity at the desired column temperature. Adjustgas pressure or optimal fow depending on carrier gasselection.

2. The non-retained peak must have ideal peak shape orinstallation is aulty and needs to be redone.

Proper & Improperly Cut Capillary

Correct Incorrect

* See individual phases or detailed specifcations and limitations.

Length (L) ID (r) Phase Thickness (df)

RESOLUTION

(R)R ~

L

To double resolution,quadruple the length

R ~rResolution decreases with

increased diameter

R ~1

d f

Resolution decreases with increased thickness

SAMPLE CAPACITY(SC) SC ~ L

Longer columns haveslightly better capacity

SC ~ r 2Capacity is exponentialas diameter increases

SC ~ df

Sample capacity increases with thicker ilms

RETENTION TIME

(tr)

t r ~ LLonger columns require

longer analysis times

t r ~ rSmaller diameter columnsallow aster analysis times

t r ~ df

Thicker ilms require longer analysis times

Use a thermoconductivity detector to check or leaks.It is highly sensitive to H

2, He, and N

2and will not contaminate

the instrument or column. Liquid leak indicators are notrecommended or capillary columns. There is the risko drawing the liquid into the column or ttings andcontaminating the system.

NOTE:

I Vespel errules are being used, leakage can occur aterthe initial heating phase due to errule deormation. Be surethat the tting is re-tightened ater this initial heating phase,then careully check all corrections or leaks.

CHECKING FOR LEAKS

Non-Polar

Polar

Methane with FID/TCD:

Calculate linear velocity by injecting25-100 L o 1 % methane in N2 gas blend.Measure the retention time o themethane peak and calculate the ollowing:

Linear Velocity (u) = L/t o

Detector Type Marker Compound

ECD Methylene chloride2,3 , DichlorodifuoromethaneFID Methane, Butane1

NPD Acetonitrile2,4

PID ELCD Vinyl chlorideTCD, MS Methane, Butane1, air1. From a disposable lighter2. Place 1-2 drops in an autosampler vial and tightly cap.Shake and inject 1-2 L rom

the headspace o the vial.Do not inject any liquid.3. Use a column temperature above 55 C.4. Use a column temperature above 95 C.

NON-RETAINED PEAK TIMES AND MARKERS

h (u) Curves or Dierent GasesLength (m) H2 (sec) He (sec) N2 (sec)

15 38 75 150

30 75 150 300

60 150 300 600

RECOMMENDED NON-RETAINED RETENTION

TIMES

Tailing peak indicates Symmetrical peak indicatesimproper installation proper installation

I the peak is broad and/or tailing, check the ollowing:

Improper column positioning/insertion into inletor detector

Gross contamination o the splitter sleeve Chipped or cracked splitter sleeve Improper sweeping o sample at column end

by makeup gas Damaged or crushed column end

UNRETAINED VOLUME PEAK SHAPE TESTING

Applications Composition PolarityTemperature

Range*MS

Certitied

ZB-1 Essential oils, gases (renery), hydrocarbons, MTBE,natural gas odorants, oxygenates and GROs,semi-volatiles, simulated distillation, solvent impurities,sulur compounds (light)

100 % Dimethylpolysiloxane Nonpolar -60 to 360/370 C

ZB-1ms Amines, acids, diesel uel, drugs o abuse, favors &ragrances, pesticides, polychlorinated biphenyls (EPA 1668)


ZB-1HT

InernoHigh boiling petroleum products, simulated distillationmethods, long-chained hydrocarbons, high molecular weightwaxes, polymers/plastics, diesel uel, motor oils


ZB-5 Alkaloids, dioxins, drugs, essential oils/favors, FAMEs,

halo-hydrocarbons, PCBs/aroclors, pesticides/herbicides,phenols, residual solvents, semi-volatiles, solvent impurities

5 %-Phenyl

95 %-Dimethylpolysiloxane

Nonpolar -60 to 360/370 C

ZB-5ms Acids, alkaloids, amines, dioxins, drugs, essentialoils/favors, EPA Methods, FAMEs, halo-hydrocarbons,

PCBs/aroclors, pesticides/herbicides, phenols, polyaromatichydrocarbons (PAH), residual solvents, semi-volatiles,solvent impurities

5 %-Phenyl Arylene95 %-Dimethylpolysiloxane


ZB-5HT

InernoHigh boiling petroleum products, simulated distillationmethods, long-chained hydrocarbons, high molecular weightwaxes, triglycerides, diesel uel, motor oils, suractants,polymers/plastics

5 %-Phenyl95 %-Dimethylpolysiloxane


ZB-624 Specically designed or the separation o volatile organiccompounds (VOCs). Widely used phase to separate residualsolvents in industrial or pharmaceutical products (OVIs).

Excellent or US EPA Met hods 501.3, 502.2, 503.1, 524.2,601, 602, 624, 8010, 8015, 8020, 8240, 8260, 8021

6 %-Cyanopropylphenyl94 %-Dimethylpolysiloxane

Intermediate -20 to 260 C

ZB-35 Aroclors, amines, nitrogen containing pesticides,organochlorine pesticides, organophosphorous pesticides,pharmaceuticals, semi-volatiles, EPA Method 508, 608,8081, 8141, 8151

35 %-Phenyl65 %-Dimethylpolysiloxane

Low-MidPolar

50 to 340/360 C

ZB-1701 Alcohols, amines, aromatic hydrocarbons,PAHs, PCBs, pesticides/herbicides, phenols, steroids,tranquilizers


P ol ar -20 to 280/300 C

ZB-1701P Organochlorine pesticides, nitrogencontaining pesticides, organophosphorous pesticides,

aroclors


P ol ar -20 to 280/300 C

ZB-50 Antidepressants, aroclors, cholesterols, drugs o abuse

(especially basic), glycols, pesticides/herbicides, steroids,triglycerides, EPA Methods 508, 608, 8081, 8141, 8151

50 %-Phenyl

50 %-Dimethylpolysiloxane

Intermediate 40 to 320/340 C

ZB-WAX

PLUS

Alcoholic beverages, alcohols, aldehydes, aromatics,essential oils, favors/ragrances, glycols, pharmaceuticalsOVIs, solvents, styrene, xylene isomers

Polyethylene Glycol Polar 20 to 250/260 C

ZB-WAX Alcohols, aldehydes, aromatics, essential oils, favors& ragrances, glycols, OVIs, pharmaceuticals, solvents,styrene, xylenes isomers, basic compounds

Polyethylene Glycol Polar 40 to 250/260 C

ZB-FFAP Acrylates, alcohols, aldehydes, ree atty acids, ketones,organic acids, phenols, volatile ree acids

Nitroterephthalic AcidModied Polyethylene Glycol

Polar 40 to 250/260 C

Organochlorine pesticides, nitrogen containing pesticides,insecticides, haloacetic acids, organophosphorous pesticides,herbicides, aroclors/PCBs, multi-pesticide residue methods

Proprietary Intermediate -60 to 320/340 C

Organochlorine pesticides, nitrogen containing pesticides,insecticides, haloacetic acids, organophosphorous pesticides,herbicides, aroclors/PCBs, multi-pesticide residue methods

Proprietary Intermediate -60 to 320/340 C

5

8

13

18

19

24

52

57

COLUMN PHASE SELECTION GUIDE

MultiResidue Columns(MR)-1

Non

-P

ol

ar

Polar

PhasePolarity Scale

58

COLUMN DIMENSION SELECTION GUIDE

MultiResidue Columns(MR)-2

7/28/2019 5220_gc_poster

2/2

www.phenomenex.com

Phenomenex products are available worldwide. For the distributor in your country, contactPhenomenex USA, International Department by telephone, ax or email: [email protected].

AustraliaPO Box 4084Lane Cove, NSW 2066Australia

[email protected]

ail:

el.:

ax:

ail:

AustriaZeppelinstr. 563741 AschaffenburgGermany

[email protected]

Canada411 Madrid Ave.Torrance, CA90501-1430USA

(800) 543-3681(310) [email protected]

DenmarkGydevang 39-413450AllerdDenmark


FranceParc des Grillons, Bat.360 route de Sartrouville78232 Le Pecq CedexFrance

01 30 09 21 1001 30 09 21 [email protected]

GermanyZeppelinstr. 563741 AschaffenburgGermany

[email protected]

IrelandQueens Avenue,Hurdseld Ind. Est.,Maccleseld, CheshireSK10 2BN, UK

01 247 5405+44 [email protected]

ItalyVia Emilia, 51/C40011 Anzola dellEmilia (BO)Italy


New ZealandP O Box 31-601Milford 0741North Shore CityNew Zealand

[email protected]

Puerto Rico273 Sierra Morena,Suite #104San Juan,Puerto Rico 00926

(800) 541-HPLC(310) [email protected]

United KingdomQueens Avenue,Hurdseld Ind. Est.,Maccleseld, CheshireSK10 2BN, UK

[email protected]

USA411 Madrid Ave.Torrance, CA90501-1430USA

(310) 212-0555(310) [email protected]

BASELINE

SYSTEM

Leaks, O2 infux

Column bleed Septum bleed Contaminated gases Unequilibrated

Dirty detector

Dirty inlet Improper fow rates Pneumatic temperature change

SAMPLE

Carry over

Depolymerization agents(HCl, KOH, etc.)

POSSIBLE CAUSES

FOR BASELINE INSTABILITY

PEAKS

REFERENCE

to

NO PEAKSPossible Cause:

System

Clogged syringe ............................................................ Leaks ............................................................................

No carrier gas ............................................................... Detector OFF or not lit ................................................... Wrong i njection port ...................................................... Clogged i nlet sleeve ......................................................Column

Broken column .............................................................. Plugged column ............................................................

Suggested Remedy:

Clean or replace syringe.Check injector or leaks. Make sure column is properly installed in detector.

Turn on carrier gas.Ignite or turn on detector. Reduce sample size or gas fows i solvent blew out detector.

Veriy correct injection port.Replace inlet liner.

Inspect column and veriy fow at column outlet.Cut o 5-10 cm o column ends and reinstall column. Veriy fow at column outlet.

GHOST PEAKSPossible Cause:

System

Septum bleed ................................................................ Carry over ..................................................................... Dirty inlet ......................................................................

Contaminated gas ......................................................... Outgassing rom traps .................................................. Contaminated gas l ines .................................................Column

Sample contaminated ...................................................

Sample

Contaminated sample ................................................... Contaminated fush solvent ........................................... Possible sample degradation .........................................

Suggested Remedy:

Replace septum with high-temperature, low-bleed septum.Increase nal temperature and hold. Rinse syringe better.Replace inlet liner.

Replace lters, scrubbers, or service puriers. Use higher purity gasses.Replace traps.Replace or clean gas lines.

Cut 50-100 cm rom injector side o column. Perorm an extended conditioning step. Solventrinse column. Use glass wool in liner or decrease injection temperature, or replace column.

Remake sample with higher purity/resh solvents and clean glassware.Replace syringe fush solvent with resh/pure solvent.Make new sample. Store samples using proper procedures. Reduce introduction o catalystsor reactive analytes in sample. Store samples in opaque or dark containers.

TAILING PEAKSPossible Cause:

C ontaminated or active injector liner or column ............

Dead volume due to poorly installed liner or column .....

Ragged column end ......................................................

A bad match between the polariti es o stationary .........phase and the solvent

A cold region in the sample fow path ........................... Debris in the liner or column ......................................... Injection takes too long ................................................. Split ratio is too low ....................................................... Overloading the inlet .................................................... Some types o compounds such as alcoholic ...............

amines and carboxylic acids tend to tail

Suggested Remedy:

Clean or replace injector liner. Dont use glass wool in the liner. Solvent rinse or replacethe column.Conrm by injecting inert peak (methane). I it tails, column is not properly installed.

Reinstall liner and column as necessary.Score the tubing lightly with a sapphire scribe or a ceramic scoring waer beore breaking it.Examine the end. I the break i s not clean and the end square, cut the column again. Pointthe end down while breaking it, and reinstall the column while installing a nut and errule.This will prevent ragments rom entering the column.Change the stationary phase. Usually polar analytes tail on non-polar columns,or dirty columns.

Remove any cold zones in the fow path.Clean or replace the liner. Cut 10 cm o the end o the column and reinstall it.Improve injection technique.Increase split ratio to at least 20:1.Decrease the sample volume or dilute sample.Try a more polar column. Make a derivati ve o the sample.

BROAD SOLVENT FRONTSPossible Cause:

Bad column installation ................................................. Injector leak .................................................................. Injection volume too large ............................................. Injection temperature too low ........................................

Split ratio is too low ......................................................

Column temperature too low ......................................... Initial column temperature too high................................

or splitless injection Purge time too long (splitless injection) .........................

Suggested Remedy:

Reinstall column.Find and x leak.Decrease sample size or dilute 1:10.Increase injection temperature so the entire sample is vaporized instantly. An injectiontemperature higher than the temperature limit o the column will not damage the column.Increase split ratio.

Increase column temperature. Use a lower boiling point solvent.Decrease the initial column temperature. Use a less volatile solvent so the initial column temper-ature is at least 10 C below the boiling point o the solvent. Use a shorter purge activation time.Use a shorter purge activation time.

FRONTING PEAKSPossible Cause:

Column overloading .......................................................Suggested Remedy:

Reduce the injection volume (increasing sensitivity, i necessary), increase splitratio, or use a column with greater capacity. Columns with larger diameters

or thicker stationary phase coatings generally have larger sample capacities;however, resolution may be reduced.

NON-REPRODUCIBLE RETENTION TIMESPossible Cause:

System

Leaks ............................................................. Erratic fow controller ...................................... Unstable oven temperature .............................. Pneumatic temperature change ...................... Line pressure change ...................................... Injection technique ..........................................

Column

Polarity changing rom contamination ..............

Adsorption .......................................................

Sample

Concentration solute/stationary .......................phase insolubility

Suggested Remedy:

Check injector or leaks. Make sure column is properly installed in detector.Veriy fows. Fix/replace fow controller i necessary.Calibrate oven. Possibly replace thermocouple.Redirect oven exhaust. Regulate room temperature.Install dual stage regulator.Standardize a reproducible injection technique.

Cut 50-100 cm rom injector side o column; perorm an extended

conditioning step. Solvent rinse column. Use glass wool in liner or decreaseinjection temperature; or replace column.

Increase nal temperature in program with hold time. Remove 50-100 cmrom injector side o column.

Use retention gap. Change column phase.

ContactPhenomenexto get yourFREECOPYo our GC Troubleshooting Guide

SPLIT PEAKS Possible Cause: Poor (jerky or erratic) injections ..................................... Bad column installation .................................................

Fluctuations in column temperature .............................. Mixed sample solvent or splitless ................................

or on-column injections When using injection techniques that ............................

require solvent eect reocusing such as splitlessinjection, the solvent must orm a compact, continuousfooded zone in the column. I the solvent does not wet

the stationary phase (column lining) suciently, asmight be the case or methanol used with a nonpolarstationary phase, the solvent fooded zone may beseveral meters long and not o uniorm thickness. Thiswill result in broad and distorted peaks because thesolutes will not be reocused into a narrow band nearthe beginning o the column.

Suggested Remedy:

Use smooth, steady plunger depression. Use autosampler.Reinstall column.

Repair temperature control system. Calibrate GC oven.Use single solvent.

Installing a retention gap (5 meters o uncoatedbut deactivated column) ahead o the c hromatographiccolumn may reduce or eliminate this problem.

COLUMN

Bleed contamination

Liquid leak detectorcontamination

PARAMETERS UNIT SYMBOLS

Retention Time oan Unretained Solute

s to

HOW TO

DECREASE

PEAK WIDTH

1. Use a More

Efcient Column Packed -smaller particles, packedmore tightly

Capillary -smaller ID, thinner lm

2. Optimize Method

Parameters

See van DeemterPlots or optimal fowrates o carrier gases

Optimize temperatureproles

3. Reduce Sample Size

To avoid columnoverloading

4. Reduce Dead

Volume in System

Follow manuacturers

recommendedInstallation Instructions

Eliminate any leaks

Optimize detector fows

Retention Time,Measured rom the Start

s tR

Adjusted Retention Time s tR = tR - to

Peak Width

(Base)s

W

Peak Width(Hal Height)

s W

Capacity Factor(Retention Factor)

k =tR

Selectivity Factor a =k2

=

t R2

Resolution Rs = 2t

R2-

t,R1

Number o Theoret ical Plates N = 5 .54tR

= 16tR

Numb er o Eective Plates Neff = 5.54tR

= 16tR

Column Length cm L

Height Equivalent o a

Theoretical Plate (Plate Height) cm H =

L

Eective Plate Height cm Heff =L

Linear Velocity o theMobile Phase

cm s-1 U =L

Pressure Conversions1 bar = 100 kPa

1 atm = 101.3 kPa

1 psi = 6.9 kPa

to

k1 tR1

to

Neff

N

( )W1 + W2(W

)

2

(W )2

(W)

2

(W)2

Vespel is a registered trademark o E.I. du Pont de Nemours and Co. Arylene Matrix Technology, Engineered Sel Cross-linking, Inerno,MultiResidue, and Zebron are trademarks o Phenomenex, Inc. 2007 Phenomenex Inc. All rights reserved.

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