New Chromatography Columns and Accessories at the 2001 ...

368 LCGC VOLUME 19 NUMBER 4 APRIL 2001 www.chromatographyonline.com 

Column 

Watch 

This column is the second 

of a two-part series in 

which Ron Majors 

examines the trends in 

column introductions at 

Pittcon 2001. In part II, 

he describes gas and 

supercritical fluid 

chromatography columns, 

sample preparation 

products, and accessories 

for chromatography and 

sample preparation. 

Ronald E. Majors 

Column Watch Editor 

New Chromatography 

Columns and Accessories 

at the 2001 Pittsburgh 

Conference, Part II 

This month’s “Column Watch” is the 

second of a two-part installment 

describing new products introduced 

at Pittcon 2001 — the 52nd Pittsburgh 

Conference on Analytical Chemistry and 

Applied Spectroscopy — on 4–9 March 

2001 in New Orleans. Last month I discussed 

introductions in high performance 

liquid, reversed-phase, normal and bondedphase, 

ion-exchange and ion, size-exclusion, 

large- and preparative-scale, and specialty 

chromatography columns. This month, I 

will look at gas chromatography (GC) and 

supercritical fluid chromatography (SFC) 

columns, sample preparation products, and 

small hardware and accessories for chromatography 

and sample preparation. 

The purpose of this report is to provide 

information about many of the new separation 

products displayed at Pittcon 2001. In 

some cases, products that were introduced 

during 2000 but after Pittcon 2000 may be 

included for reasons of completeness. The 

information is based on manufacturers’ 

responses to a questionnaire mailed in 

December 2000. Because of space limitations 

and the fact that some of the manufacturers 

did not respond to the questionnaire, 

this report cannot be considered an 

exhaustive listing of all new products that 

were introduced in New Orleans. However, 

over the years, these Pittcon introduction 

summaries have proved a good source of 

information that would be difficult for 

individuals to gather during the exhibition. 

In addition, the products introduced at 

Pittcon have shown definite correlation to 

current research, development, and application 

activity in the separation sciences. 

As in previous years, columns recommended 

by their manufacturers primarily 

for biomolecular separations are denoted in 

the tables with the designation BIO. Some 

of these products can be used for generalpurpose 

separations as well, but their main 

applications are in biochromatography. 

I will cite specific information about 

bioapplications where appropriate. Manufacturers 

introduced many products for 

drug discovery and combinatorial chemistry 

this year; I will discuss these products in 

the sections that best fit the manufacturers’ 

intended applications. 

Gas and Supercritical Fluid 

Chromatography Columns 

Nine companies contributed new GC 

and SFC column information for Pittcon 

2001, presenting 23 new phases (Table I). 

Capillary columns with inner diameters 

ranging from 0.10 mm (small bore) to 0.53 

mm (large bore or megabore) were the 

most popular introductions. The majority 

of the introduced columns were wall-coated 

open tubular (WCOT), but three new 

porous-layer open tubular (PLOT) column 

lines also were presented. Selerity Technologies 

debuted three micropacked columns 

suitable for use in SFC. To demonstrate the 

capabilities of SFC, Figure 1 depicts the 

high-resolution separation of two mixtures 

of fluorocarbon lubricants using supercritical 

carbon dioxide. Pressure programming 

was used to change the density of the 

supercritical fluid, which changed the relative 

retention, analogous to temperature 

programming in GC. 

General-purpose columns: Many of the 

general-purpose GC capillary columns displayed 

at Pittcon 2001 were cross-linked 

alternatives to popular coated phases. 

Cross-linked, chemically bonded, or immobilized 

phases are more stable, have lower 

bleed, and usually can operate at higher 

temperatures than coated phases. Another 

advantage of bonded phases is their ability 

to be rinsed by solvent. These columns can 

be disconnected, washed (outlet to inlet 

direction) with various solvents, and 

returned to gas chromatographs for further 

use if they become contaminated by highboiling-point 

compounds, inorganic


Table I: New Gas and Supercritical Fluid Chromatography Columns 

Product Name Supplier Type Phase Film Thickness (m) Inner Diameter (mm) 

AT-AquaWax capillary Alltech Associates WCOT Polyethylene glycol based 0.25 0.25, 0.32 

columns 

AT-FAME capillary columns Alltech Associates WCOT Polyethylene glycol based 0.25 0.25, 0.32 

Chiraldex G-DP/B-DP Advanced Separation Chiral See comments 0.125 Not specified 

columns 

Technologies 

cP-Volamine columns Varian Chrompack WCOT Polydimethylsiloxane Not specified 0.32 

Fluoro-Phase columns Selerity Technologies Packed Fluorooctylsilane Not applicable 1.00 

Optima FFAP columns Macherey-Nagel WCOT Free fatty acid phase 0.25, 0.50 0.25, 0.32 

Optima-Wax columns Macherey-Nagel WCOT Polyethylene glycol based 0.25, 0.5 0.25, 0.32 

OV-5 capillary columns Ohio Valley WCOT 5% Phenyl, 95% 0.1, 0.25, 0.5, 1.0, 0.25, 0.32, 0.53 

Specialty Chemicals dimethylpolysiloxane 1.5, 3, 5 

Petro-Ag columns Selerity Technologies Packed Silica–polymer Not applicable 1.00 

Petro-Sil columns Selerity Technologies Packed Silica Not applicable 1.00 

PoraBond U columns Varian Chrompack PLOT PS–DVB* 7 0.32 

Rapid-MS columns Varian Chrompack WCOT CP-Sil 8 CB low bleed–MS 0.12, 0.25, 0.5, 1.0 0.53 

RT-Pro Gas X columns Restek PLOT Not specified Not specified 0.32 

Rtx-HT1 columns Restek WCOT Not specified 0.10 0.25, 0.32 

Rtx-OPP2 columns Restek WCOT Not specified 0.25, 0.50 0.25, 0.32, 0.53 

Rtx-Sol Gel Wax columns Restek WCOT Polyethylene glycol based Not specified Not specified 

SolGel-1 MS columns SGE WCOT 100% Dimethylpolysiloxane 0.25 0.25 

Stx-CLP, Stx-CLP2, and Restek WCOT Not specified Various 0.25, 0.32, 0.53 

Stx-CLP kits 

ValcoBond VB-1 columns VICI Gig Harbor WCOT 100% Dimethylpolysiloxane 0.10–5.0 0.25, 0.32, 0.53 

ValcoBond VB-5 columns VICI Gig Harbor WCOT 5% Phenyl 0.1–5.0 0.25, 0.32, 0.53 

dimethylpolysiloxane 

ValcoBond VB-50 columns VICI Gig Harbor WCOT 50% Phenyl 0.25–1.0 0.25, 0.32, 0.53 

methylpolysiloxane 

ValcoBond VB-Wax VICI Gig Harbor WCOT Polyethylene glycol 0.15–1.0 0.25, 0.32, 0.53 

columns 

ValcoPlot VP-Alumina VICI Gig Harbor PLOT Aluminum oxide Not applicable 0.53 

columns 

* PS–DVB poly(styrene–divinylbenzene).

www.chromatographyonline.com 

APRIL 2001 LCGC VOLUME 19 NUMBER 4 371 

Length (m) 

Comments 

30, 60 Carbowax column recommended for analyzing foods, flavors, and alcoholic beverages in aqueous matrices; stable for 

aqueous injections; 280 °C upper-temperature limit; 250 and 320 phase ratios. 

30, 60 Recommended for fatty acid methyl ester (FAME) analysis, especially from fats and edible oils such as American Oil Chemists’ 

Society (AOCS) method CE 1b-89 and AOCS method 991.39; 280 °C upper temperature limit; 250 and 320 phase ratios; tested 

with fatty acid methyl ester samples. 

Not specified Phase is 2,3-di-O-propionyl-6-O-O-butyl-silyl--cyclodextrin and --cyclodextrin in 50% ratio; separation column designed for 

polar racemates, especially amines such as amphetamine, 1-aminoindan, and diaminocyclohexane; display large increase in 

selectivity for polar racemates; smaller racemates and saturated ring amines prefer beta version; bulkier structures separate 

best on gamma version; 200 °C upper temperature limit. 

60 Recommended for analyzing volatile amines in combination with alcohols, water, or ammonia; tolerate water-containing 

samples; 265 °C upper temperature limit; special deactivation and stabilizing. 

0.25 SFC column based on 5-m d p packed silica with a bonded phase; recommended for separating fluorinated compounds; 

provides higher molecular weight compound resolution than GC; stainless steel construction. 

25, 30, 50, 60 Recommended for analyzing polar compounds, solvents, and fatty acid methyl esters; upper temperature limits of 250 °C 

isothermal and 270 °C in temperature program, identical selectivity to standard free fatty acid phases. 

25, 30, 50, 60 Recommended for use with polar analytes and solvents; upper temperature limits of 250 °C isothermal and 270 °C in 

temperature program; identical selectivity to standard Carbowax phases. 

15, 30, 60, 105 Bonded and cross-linked phases that provide low bleed; solvent rinsable; equivalent to U.S. Pharmacopeia (USP) G27 column 

standard; general-purpose use; 60 to 330 or 350 °C temperature limits, upper limit decreases with higher film thicknesses. 

0.05 SFC columns with dimethylsilylpropyl silver sulfonate stationary phase on 5-m d p silica; designed to meet requirements for 

the determination of olefins by American Society for Testing and Materials (ASTM) method 6550; optimized for specific 

application of olefin trapping; stainless steel construction with 1 ⁄16-in. outer diameter. 

0.75 SFC columns for the determination of aromatic compounds in diesel and jet fuel by ASTM method 5186 and olefin 

determination by ASTM method 6550; exceed resolution requirement of methods; columns with 0.5 and 0.75 mm inner 

diameters available in a variety of lengths; 1 ⁄16-in. o.d. stainless steel construction; 5-m particles. 

25 PS–DVB porous-polymer stationary phase with dimethacrylate modification; 290–300 °C upper temperature limit to allow 

analysis of high-boiling-point compounds with carbon chains as long as C 14 ; minimal or no particle loss for increased 

analytical reliability; recommended for solvent analysis according to USP method 467; also recommended for analyzing 

impurities in chemical and solvent streams and separating hydrochloric acid and water. 

10 Columns recommended for GC–MS applications; different film thicknesses allow faster analyses and high loadability; lower 

elution temperatures, therefore, less bleed; applications include pesticide, drug, estrogen, and steroid analysis. 

15, 30 Specialty column for permanent gases and hydrocarbon gases; separates carbon monoxide from carbon dioxide. 

15, 30 A high-temperature phase that can withstand temperatures as high as 390 °C; columns have optimized column tubing, a 

deactivation layer, and a new high-temperature polymer to ensure low bleed; recommended for GC–MS applications. 

15, 30 A specialty phase recommended for analyzing organophosphorus pesticides; provide improved resolution and faster analysis 

time compared with previous organophosphorus pesticide phases. 

Not specified Recommended for separation of solvents, organic compounds and benzene, toluene, ethylbenzene, and xylene (BTEX) by 

purge-and-trap; 280 and 290 °C temperature limits; higher thermal stability than traditional Carbowax 20M phase; water 

resistant. 

30 Recommended for all GC–MS applications; provide lower bleed and better sensitivity compared with regular 100% 

polydimethylsiloxane phases; 380 °C upper temperature limit. 

30 Recommended for analyzing organochloro pesticides, chlorophenoxy herbicides, atrazine herbicides, and chloroacetic acids; 

computer-optimized stationary phase and column dimensions. 

15, 30, 60 General-purpose capillary columns designed to replace other 100% dimethylpolysiloxane columns; 60 to 360 or 370 °C 

operating temperatures; bonded and cross-linked, solvent rinsable; recommended for GC–MS and a wide variety of 

applications, including pesticide and phenol analysis and U.S. Environmental Protection Agency (EPA) and National Institute 

for Occupational Safety and Health (NIOSH) methods; equivalent to USP G2 column standard. 

15, 30, 60 Recommended as a replacement for other 5% phenyl phases; 60 to 360 or 370 °C operating temperature; bonded and 

cross-linked, solvent rinsable; recommended for GC–MS and a wide variety of applications, including herbicide, pesticide, 

polychlorinated biphenyl, semivolatile compound analysis. 

15, 30, 60 Midpolarity columns that are replacements for other 50% phenyl phases; applications include herbicide, polynuclear aromatic 

hydrocarbon (PAH), pharmaceutical, and tocopherol analysis; 40 to 340 or 360 °C temperature range; bonded and crosslinked, 

solvent rinsable; equivalent to USP G3 column standard; can be used for GC–MS. 

15, 30, 60 A Carbowax phase recommended for solvent, alcohol, aromatic compound, flavor, and fragrance applications; replacement 

for other polyethylene glycol columns; bonded and cross-linked; solvent rinsable; equivalent to USP G16 column standard. 

15, 30 Recommended for the analysis of light hydrocarbons; separates C 1 –C 4 saturated and unsaturated hydrocarbons; 20 to 

200 °C temperature range; available in electroformed nickel tubing.


Companies Introducing 

Products at Pittcon 2001 

Advanced Separation Technologies Inc. 

(Astec), Whippany, New Jersey 

Agilent Technologies Inc., Wilmington, 

Delaware 

Air Liquide America Corp., Houston, Texas 

Alltech Associates, Inc., Deerfield, Illinois 

Ansys Technologies, Inc., Lake Forest, 

California 

Aura Industries, Staten Island, New York 

Crescent Chemical Co., Islandia, New York 

Dionex Corp., Sunnyvale, California 

Domnick Hunter, Gateshead, United 

Kingdom 

Dr. Ehrenstorfer GmbH, Augsburg, 

Germany 

EST Analytical, Cincinnati, Ohio 

Interchim, Montluçon, France 

International Sorbent Technology Ltd., 

Hengoed, United Kingdom 

Joint Analytical Systems, Inc., Burlington, 

Kentucky 

Jordi Associates, Inc., Bellingham, 

Massachusetts 

Keco R&D Inc., Navasota, Texas 

Macherey-Nagel GmbH & Co. KG, Düren, 

Germany 

Marcel Dekker, New York, New York 

Micro-Tech Scientific Inc., Sunnyvale, 

California 

MicroSolv Technology Corp., Long Branch, 

New Jersey 

Millipore Corp., Bedford, Massachusetts 

Ohio Valley Specialty Chemical Inc., 

Marietta, Ohio 

Phenomenex Inc., Torrance, California 

Restek Corp., Bellefonte, Pennsylvania 

Selerity Technologies, Inc., Salt Lake City, 

Utah 

SGE, Inc., Austin, Texas 

Showa Denko KK, Osaka, Japan 

Silica Physics, LLC, Glendale, Arizona 

Spark-Holland, Emmen, The Netherlands 

Sun International, Wilmington, North 

Carolina 

Thermo Hypersil, Runcorn, United 

Kingdom 

3M Co. Filtration Products, St. Paul, 

Minnesota 

United Chemical Technologies, Inc., 

Bristol, Pennsylvania 

Valco Instruments Co., Inc., Houston, 

Texas 

Varian Chrompack International, BV, 

Middelburg, The Netherlands 

Varian, Inc., Harbor City, California 

VICI Gig Harbor Group Inc., Gig Harbor, 

Washington 

Waters Corp., Milford, Massachusetts 

compounds, or other nonvolatile impurities 

that can cause drifting baselines, bleed, and 

other undesirable occurrences. 

Many column suppliers have been introducing 

increasingly lower-bleed columns 

for trace analysis, GC–mass spectrometry 

(MS) applications, and better baselines and 

increased column life. This trend continues 

this year, and several of the manufacturers 

introduced low-bleed phases that also have 

higher temperature limits. Temperature 

ranges are specified in Table I from the 

lowest recommended temperature to the 

highest temperatures. The initial high temperature 

specified in Table I is the highest 

recommended temperature for isothermal 

analysis; although the second designated 

temperature usually is 20 °C higher, it is 

the highest temperature that can be tolerated 

for short time periods such as the end 

of a temperature program. 

Specialty columns: One of the largest 

application areas for GC is petroleum 

analysis. Therefore, new columns for the 

separation of hydrocarbons and permanent 

gases always are being introduced and this 

year was no exception. PLOT columns are 

promoted as replacements for classic 

porous-polymer packed columns. With the 

smaller inner diameter columns, separations 

are faster, conditioning times are shorter, 

bleeds are lower, and efficiencies are higher. 

The sample capacities are lower because of 

the reduced amount of stationary phase in 

Detector response (mV) 

50 

40 

30 

20 

10 

a PLOT column relative to classic packed 

columns. Most importantly, the selectivity 

and elution patterns remain the same. SFC 

also has been used in the separation of 

hydrocarbon mixtures. 

Sample Preparation Products 

As Table II indicates, new sample preparation 

products were very popular at Pittcon 

2001. Companies displayed 19 products or 

families of products. Most of these products 

fit into the solid-phase extraction 

(SPE) category with formats ranging from 

traditional cartridges (the majority of introductions) 

and disks, SPE pipette tips, and 

96-well plates. Both polymeric and silicabased 

packings were represented. This year 

saw some new players enter the SPE market. 

In the past couple of years, the 96-well 

SPE plates have proliferated. The predominant 

driving force in their development has 

been the high-throughput requirements 

placed on sample preparation, chromatography, 

and mass spectrometry laboratories 

by the pharmaceutical industry for drug 

screening and combinatorial chemistry 

analyses. As sample loads increase to hundreds 

per day, the need for rapid turnaround 

of analytical results dictates automation, 

robotics, and faster liquid-handling 

systems to meet the demand. This year four 

new products or product families debuted. 

In a typical 96-well configuration, 96 small 

0 10 15 20 25 30 35 40 45 50 55 60 65 70 

Time (min) 

Figure 1: Separation of Krytox fluorocarbon lubricant (Du Pont, Wilmington, Delaware) samples 

by SFC. Column: 150 mm 1 mm, 5-m d p FluoroPhase; mobile phase: supercritical carbon 

dioxide; temperature: 150 °C; pressure program: 10 min hold at 100 atm, then 7.5 atm/min to 150 

atm, 2.5 atm/min to 210 atm, 1.5 atm/min to 325 atm; injection: time-split, 3 s. (Chromatogram 

courtesy of Selerity Technologies, Salt Lake City, Utah.)


Table II: New Sample Preparation Products 

Product Supplier Product Type Modes Base Material Functional Group 

Chromabond Easy cartridges Macherey-Nagel SPE cartridge Reversed phase Hydrophilic PS–DVB Unspecified polar 

polymer 

Copolymeric SPE columns United Chemical SPE cartridge Mixed phase Silica Strong cation or 

Technologies 

anion exchange 

and C8 

DPX disposable pipette EST Analytical SPE pipette tips Mixed Silica Unspecified 

extraction tips 

Empore universal resin 3M Filtration 96-Well plate Reversed phase Polymer Not specified 

96-well plates 

Products 

HySphere hydrophobic Spark Holland SPE method Reversed phase Silica and polymer Various 

method development kit 

development kit 

Isolute PAH HC cartridges International Sorbent SPE cartridge Normal phase Silica Proprietary 

Technology 

Isolute SCX-3 cartridges and International Sorbent SPE cartridge, Cation exchange Silica Sulfonic acid 

well plates Technology 96-well plate 

J-Clean SPE columns Jordi Associates SPE cartridge Reversed phase PDVB* PDVB 

Oasis method development Waters SPE method Reversed phase, ion N-Vinylpyrrolidone– Hydrophilic– 

kit development kit exchange DVB (hydrophilic– lipophilic balance, 

lipophilic balance) sulfonic acid, 

quaternary amine 

Oasis Prospekt 2 cartridges Waters SPE cartridge Reversed phase N-Vinylpyrrolidone– Hydrophilic– 

DVB (hydrophilic– lipophilic balance 

lipophilic balance) 

Shodex MSpak PK columns Showa Denko Concentration Reversed phase Hydrophilic polymer Not specified 

column 

Shodex SPEC EDS-1 cartridges Showa Denko SPE cartridge Reversed phase Hydrophilic polymer Not specified 

SPE method development Thermo Hypersil SPE kit Reversed and Silica, DVB, porous Various 

kits normal phase graphitic carbon 

Strata SPE products Phenomenex SPE cartridge Reversed and phase, Silica, Florisil, polymer See comments 

ion exchange 

SuperClean SPE columns Alltech Associates SPE cartridge Reversed phase Carbon based Proprietary 

Upti-Clean cartridges Interchim Cartridge Reversed and normal Silica Various 

phase, ion exchange, 

size exclusion 

VersaPlate method Varian 96-Well plate Reversed and Silica, polymer C2, C8, C18, phenyl, 

development plates normal phase silica, PS–DVB, 

copolymer 

ZipTip MC pipette tips Millipore SPE pipette tip Affinity Silica Immobilized metal 

Zorbax SPE cartridges Agilent Technologies SPE cartridge, Reversed and Silica C8, C18, silica 

and well plates 96-well plate normal phase 

* PVDB polydivinylbenzene.



Dimensions 

Comments 

1-, 3-, and 6-mL cartridges, Polymer has 50-m average particle diameter; recommended for sample preparation of drugs from blood, serum, 

96-well plates 

plasma, or environmental samples such as soil and water; reduced or no need for preconditioning (can load water 

samples directly); can run dry without problems; high capacity; pH 1–14 stable. 

1, 3, 6, 10, 15, 75 mL Dual-functionality bonded-phase silicas on a single particle optimized for extracting drugs of abuse from biological 

matrices; permit separation of charged and neutral compounds simultaneously; both 40–60 m and 125–210 m 

particle size ranges; base silica has a 60-Å pore size; sorbents also available. 

1 mL volume 

Recommended for extracting drugs of abuse from serum and urine according to the definitions of the Substance 

Abuse and Mental Health Services Administration (SAMHSA, formerly known as NIDA [National Institute on Drug 

Abuse]); sample is drawn into tip and mixed with stationary phase; next, the matrix is sent to waste and adsorbed 

analytes are eluted into 0.1–0.3 mL of solvent to be analyzed by GC–MS. 

Disk 

Recommended for SPE for bioanalytical applications; universal resin provides retention for acidic, basic, and neutral 

compounds; BIO. 

See comments 

Kit developed for automated and manual method development, primarily for the company’s Prospekt-2 automated 

SPE system; 10–40 mg of phase in 10 mm 2 and 3 mL cartridges; provide fully automated fast method development 

for SPE procedures; PC control software supports method development with different phases and parameters, 

including temperature control and validation protocols; wide range of phases with increasing hydrophobicity 

available. 

1 g/3 mL, 1 g/6 mL Recommended for cleanup of hexane extracts of oil-contaminated soils for PAH analyses; fractionates aliphatic 

hydrocarbons from aromatic hydrocarbons; based on 50-m d p irregular silica with 60-Å pores. 

25 mg/1 mL to Ion-exchange capacity 0.6 mequiv/g; based on 60-Å irregular silica of 50-m average particle size; recommended 

10 g/70 mL; 96-well for extracting basic drugs from biological fluids and cleaning up reaction mixtures; strong cation-exchange 

plate (25–100 mg) sorbent with strong hydrophobic characteristics. 

200 mg in 6 mL; Particle-size range of 5–38 m with 1000 Å pores; recommended for analytical and preparative cleanup; typical 

25, 10 g in 60 mL applications include analyzing phenols and acidic pesticides from environmental samples, nucleic acids, protein and 

peptide preparations, and polar drug metabolites; syringe-barrel format with 0.5-m frits; polymeric packing has 

greater capacity than silica- and PS–DVB-based packings. 

60 mg/3 mL A method development kit comprising a polymeric reversed-phase cartridge (hydrophilic–lipophilic balance) and 

cation- and anion-exchange cartridges; analysts can use the kit’s 30-m polymeric phases to develop methods for 

acids, bases, and neutral compounds. 

10 mm 1 and 2 mm Small cartridges made to fit Spark Holland’s Prospekt2 automated SPE system; recommended for SPE of small 

molecules from water and biological matrices; retain wide variety of polar to nonpolar compounds; designed for 

high-throughput analyses; 30-m particles with 80-Å pores and 1.3-cm 3 /g pore volume. 

10 mm 2 and 4 mm Short columns for sample pretreatment; recommended for use with hydrophilic compounds at low concentrations that 

are retained on polar gels; large molecular weight compounds such as proteins are unretained on the packing 

because of a size-exclusion effect. 

Not specified 

SPE cartridges for sample pretreatment; recommended for use with hydrophilic compounds at low concentrations that 

are retained on polar gels; large molecular weight compounds such as proteins are not retained on the packing 

because of a size-exclusion effect. 

Various 

Family of kits with four chemistries per kit; available in polar, hydrophobic, and ion-exchange versions; based on 

50-m d p irregular silica gel with 60-Å pores; 10–100 mg of packing bed weight in individual cartridges or modular 

96-well plates available. 

50–1000 mg in 1-, 3-, Phases bonded to irregular silica include C8, C18, phenyl, cyano, amino, strong cation and anion exchange, Florisil, and 

6-mL volumes 

PS–DVB; 50-m d p packing in medical-grade polypropylene syringe barrels with Luer-tip connections; recommended 

for general sample cleanup. 

Not specified 

Replaces earlier product that was a carbon-impregnated polytetrafluoroethylene (PTFE) matrix; recommended for 

HPLC mobile-phase cleanup; remove particulates and dissolved organic contaminants in one step; can be used for 

general SPE as hydrophobic phase. 

Standard SPE 

Family of SPE cartridges based on irregular silica; 50-m average particle size; use 2,4-dinitroanilinopropyl specialty 

phase for hydrocarbon group separations. 

10 and 25 mg Nonpolar packings in 96-well arrays for fast method development, especially helpful for pharmaceutical laboratories 

in which high throughput and low elution volumes are needed; plates’ removable arrays (loose tubes) allow 

customization; copolymer is methyl methacrylate–PS–DVB. 

0.6 L Pipette tips with an immobilized metal affinity chromatographic phase that has characteristics recommended for the 

enrichment of phosphopeptides from protein digests before matrix-assisted laser-desorption time-of-flight (MALDI- 

TOF) and electrospray MS and purification of 6 His-tagged proteins before MALDI-TOF MS; can be charged with 

different metal ions such as iron, gallium, copper, and nickel; compatible with manual and automated liquidhandling 

systems; can work with very small sample volumes and masses; provide low elution volumes of 2–4 L for 

rapid evaporation and buffer exchange; BIO. 

100–500 mg in 1-, 3-, Based on spherical Zorbax low-trace-metal, ultrahigh-purity Type B silica; spherical particles provide high permeability, 

6-mL tubes; 30–100 mg low pressure drop, consistent flow rates and gravity feed; silica, endcapped, and unendcapped alkyl phases available; 

in plates 

fixed- and removable-well arrays available.


Alltech 

1/3 Page Vert Ad 

Circle 17 

SPE disks or packed beds are embedded 

into a plastic holder, which can be fed 

sample or solvent manually or automatically. 

The holder fits over a standard 96- 

well microtiter or collection plate, so fractions 

can be eluted directly from the 

96-SPE wells into the collection plate for 

further characterization or analysis. One 

trend in 96-well plates is the availability of 

individual, removable wells that analysts 

can configure for their own arrays of SPE 

phases based upon sorbent or bed mass 

requirements. These products frequently 

are called arrays or flexible well plates. For 

example, three new products provide both 

fixed- and array-plate configurations that 

permit the construction of customized 

plates well suited for method development 

and optimization. Loose tubes or wells that 

have prepacked stationary phases and base 

plates can be purchased separately or as 

assembled plates. 

An alternate form suitable for automation 

— the SPE pipette tip — was introduced 

previously, but an additional product 

appeared on the Pittcon floor this year. 

Millipore expanded its ZipTip SPE pipette 

tip line to include an immobilized metal 

(a) 

1.3 

Counts ( 10 4 ) 

0 

(b) 

1.3 

Counts ( 10 4 ) 

2062 

2062 

3121 

3121 

0 

1000 1700 2400 3100 3800 4500 

Mass (m/z) 

Figure 2: MALDI-TOF spectra of phosphopeptides 

from a -casein tryptic digest 

obtained (a) before and (b) after enrichment of 

phosphopeptides with ZipTip MC immobilized 

metal affinity chromatography device. (Courtesy 

of Millipore Corp.) 

affinity phase for enriching phosphopeptides 

from protein digests. Figure 2 shows 

this selective phase’s ability to concentrate 

analyte and removal contaminants. Note 

the cleaner mass spectra obtained after 

using the ZipTip MC pipette tip for cleanup 

and concentration. Analysts can isolate low 

picomole-to-femtomole quantities using 

this selective device. 

Another approach for high-throughput 

sample preparation is using column switching 

or short high performance liquid chromatography 

(HPLC) columns to accomplish 

the same goal as 96-well plates. 

Manufacturers introduced specialty SPE 

phases for environmental, drugs of abuse, 

and pharmaceutical biological fluid extractions 

and protein digests. Method development 

kits are another area that seems to be 

catching on. Manufacturers are combining 

SPE phases, usually with diverse polarities, 

that will provide users the best chance to 

develop robust methods. Some manufacturers 

also make validation kits that have 

SPE phases from three different batches. 

Chromatography and 

Sample Preparation Accessories 

Table III lists 29 new hardware products 

and accessories for HPLC, GC, capillary 

electrophoresis (CE), and sample preparation. 

All of the products are practical 

devices designed to make chromatographers’ 

lives easier. I will cover each area 

individually. 

HPLC and ion chromatography products: 

Guard columns always are popular 

products. They protect analytical columns 

by trapping contaminants from sample or 

mobile phases before they get to the analytical 

columns. Some guard columns fit 

only one manufacturer’s columns; others 

are universal. 

For use in ion chromatography (IC), 

Dionex’s Atlas electrolytic suppressor is a 

suppressor bed that contains an ionexchange 

monolith, which neutralizes carbonate 

and methanesulfonic acid eluents 

before detection by electrical conductance. 

It offers an improvement in detection limits 

and lowers baseline noise. In addition, it 

provides for automatic electrolytic generation 

of the regenerant ions. Figure 3 shows 

a schematic of this electrolytic suppressor. 

One of the introductions was empty 

flash chromatography reservoirs (housings) 

that have various frit materials. Users can 

fill these housings with their own packing 

material or purchase standard packings 

from the supplier. This approach offers 

another alternative to the more expensive


Table III: New Chromatography and Sample Preparation Accessories 

Product Name Supplier Application Areas Product Type Suggested Applications 

Analytical reference standards Crescent Chemical GC, HPLC, CE Environmental reference standards Quantitative analysis 

Atlas electrolytic suppressors Dionex IC Electrolyte suppression carbonate or IC using carbonate of 

methanesulfonic acid eluents 

methanesulfonic acid eluents 

Captiva 96-well filter plates Ansys Technologies Filtration 96-Well filtration plate Filtering biological samples 

CaptiVac vacuum collars Ansys Technologies SPE Vacuum manifold Use with 96-well SPE and filtration 

plates 

Duo-Seal 96-well plate seals Ansys Technologies SPE 96-Well plate cover Protecting samples inside wells 

Electronic decapper Agilent Technologies Sample preparation Decapper for crimped capped vials Easy removal of crimped caps 

Enhanced performance United Chemical SPE, flash chromatography Polypropylene column housings SPE, flash chromatography, filtration 

reservoirs 

Technologies 

EZ:faast kit Phenomenex Amino acid analysis Analysis kit Physiological amino acid analysis 

EZ-Grip column cages Varian Chrompack GC Column cage system Convenient column installation 

HPLC column jackets Aura Industries HPLC Column water jackets Temperature control of columns 

Flashvac-10, Flashvac-20 International Sorbent Flash chromatography, SPE Vacuum manifold Flash chromatography 

vacuum manifolds 

Technology 

Micro-GC calibration kit Air Liquide America GC Calibration kit Field calibration of micro-GC system 

Microbore Column Microtech Scientific HPLC Book Learning about micro-LC columns 

Chromatography 

MicroMat CLR plate covers Sun International SPE 96-Well plate cover Protecting samples inside wells 

MS Guard column tubing Alltech Associates GC Guard column (retention gap) Trapping nonvolatile compounds 

before GC–MS 

Nanovolume injectors Valco Instruments HPLC Low-volume injector Ultralow-flow microfluidics 

Nitrox UHP gas generators Domnick Hunter GC Gas generator Making pure gases for GC carriers 

and detectors 

Precision flexible capillaries Silica Physics GC, CE, CEC Fused-silica capillary Use as capillary columns, retention 

gaps 

Protein precipitation plates International Sorbent Filtration 96-Well filtration plate Removing proteins from biological 

Technology 

samples 

Quad injectors Valco Instruments HPLC Injection system Automatic multiple-sample injection 

Ranger sample transfer units Keco R&D GC Sample transfer system Impurity removal from gas streams 

Scotti 2 sample tracking system Joint Analytical Systems Sample preparation Sample tracking system Maintaining audit trail through 

analytical process 

Secure-Fit column connectors Selerity Technologies LC, SFC Low-dead-volume connector Connecting 1 ⁄16- and 1 ⁄32-in. 

tubing 

Silanes United Chemical GC, HPLC, SPE Chemicals Use with bonded phases, 

Technologies 

deactivation 

Silica sieves for CEC Silica Physics CEC Fused capillary frit Improving packing retention in 

packed capillary 

Solid-Phase Extraction: Principles, Marcel Dekker SPE Book Learning about SPE fundamentals 

Techniques, and Applications 

Synergi column selectors Phenomenex HPLC Column-switching system Method development and 

column screening 

Trident direct guard column Restek HPLC filtration Guard columns, in-line filters Protecting analytical columns 

system 

Window Maker MicroSolv Technology CE Optical window in CE capillaries Burning polyimide layer of 

CE capillaries



Comments 

Available as neat pesticides, herbicides, metabolites, polychlorinated biphenyls, and single and multicomponent solutions; custom solutions available; available in 

Europe from Dr. Ehrenstorfer GmbH. 

For use in neutralizing and desalting ion-exchange eluents; automatic generation of regenerant ions; 10 mm 4 mm suppression bed is made of ion-exchange 

monolith and flow distribution disks; 25 mN suppression capacity at 1.0 mL/min; lower baseline noise and improve detection limits by a factor of 3; can be used with 

2-, 3-, and 4-mm IC columns. 

Recommended for filtering precipitated plasma proteins, thawed plasma, and general analytical filtration; polypropylene or glass microfiber construction; 8.0 mm 

diameter 2.0 mm depth (polypropylene) or 8.0 mm diameter 1.0 mm depth (glass fiber) filter bed size; 0.45–7.0 m depth filter for polypropylene version and 

10-m depth filter for glass fiber version; depth filter improves sample flow by reducing clogging; provides clean filtrates; BIO. 

Portable vacuum manifold; unique tip design aligns and sets the tip distance of the 96-well plate with and into the collection plate preventing sample mixup and 

cross-contamination. 

Works with both the company’s Captiva and Spec 96-well plates; unique design allows analysts to seal top of the plates as well as the tips. 

Complements the company’s sister product, an electronic crimper; fits 11-mm capped 2-mL vials (12 mm 32 mm); handheld, motor-driven, rechargeable batteryoperated 

decapper automatically removes crimped caps; can remove caps from vials placed in autosampler tray; replaces manual decappers. 

Solvent-resistant polypropylene housings have 1.5-, 4-, 8-, and 15-mL volumes; fitted with polyethylene, PTFE, or stainless steel frits; can be assembled with silica, 

carbon, or polymeric packings; low extractables; tip design minimizes or eliminates spattering. 

A kit for the sample preparation, derivatization, and GC analysis of 38 aliphatic and aromatic physiological (free) amino acids in blood, plasma, urine, and cerebral 

spinal fluid in 15 min; GC column is 10 m 0.25 mm; SPE phase has an amino acid binding and is packed in a pipette tip; no plasma protein or urine urea removal is 

necessary; kit handles 400 samples; protein hydrolysis kit also available; BIO. 

Chrompack columns with new column cage designed for easy column installation and coupling of the precolumn (with a retention gap as long as 15 m) and two other 

columns; columns held in place tightly and transfer line connections are secured; column outlet and inlets easily identifiable for reinstallation. 

Series of plastic jackets for various sizes of HPLC columns from microbore to process-scale; 30–90 °C temperature control; can be used with circulating water bath. 

Primary uses for flash chromatography, large-capacity SPE, or large-volume filtration; allows collection of large fraction volumes; rack accommodates 19- and 25-mm 

diameter collection vials; 15-cm maximum height and 50-mL maximum collection volume. 

Kit provides field calibration, including BTU 1298 rich gas mix, BTU 1054 lean gas mix, and C 1 –C 4 gas mixture analysis; predesigned kits are specific to end user 

applications; portable calibration standards with wide range of detectable components. 

Written by Frank Yang; covers packing materials and techniques, gradient elution, detection, and hyphenated techniques in micro-LC, SFC, and MS. 

Constructed for microwell plates to eliminate cross-contamination and evaporation; can be pierced and resealed multiple times; constructed of autoclavable, 

translucent, flexible silicone; large target area; available in preslit form for easy needle penetration and to reduce vacuum inside of well; manual or automatic 

operation; available for 96- (square and round well) and 384-well plates and in 8-well strips. 

Inert tubing connects to injector side of capillary column and traps nonvolatile compounds, pyrolyzables, and other contaminants and for solvent focusing during 

splitless injection; 350 °C upper temperature limit; 5 m 0.25 or 0.32 mm dimensions. 

Have unique one-piece connectors that permit use of various capillary tubing sizes; can withstand pressures as high as 5000 psi; 100-m (0.004-in.) bore sizes are 

standard; versions available with 4-, 6-, and 10-port configurations; port-to-port volume is less than 25 nL. 

Two gas generators: zero air and high-flow LC–MS nitrogen; zero air generator uses in-house low-pressure compressed air supply, can remove methane 0.1 ppm, and 

performs pre- and postfiltration; high-flow LC–MS nitrogen generator provides flows of as much as 24 L/min, provides nitrogen purity 99%, and has an integral oilfree 

air compressor and acoustic cabinet for quiet operation (5 db); both units replace high-pressure gas cylinders. 

Fused-silica capillaries with standard dimensions and polyimide coating; tight dimensions; capillary arrays for 96-multichannel CE also available. 

Recommended for high-throughput protein precipitation; fast, nonselective sample preparation; dual-frit system does not become blocked and centrifugation is 

unnecessary; polypropylene plates; both fixed-well and flexible removal formats available; BIO. 

Recommended for applications with increased throughput; use single high-torque motors for automated actuation of the quad six-port design that can inject four 

discrete samples simultaneously; 0.5-mm (0.020-in.) standard bore has a dynamic sealing system that operates at pressures as high as 3000 psi. 

Polymeric permeation membrane separates continuous sample stream — gas mixture, liquid, or slurry — from a clean, dry carrier-gas stream; impurities and 

contaminants are removed and do not contaminate the GC instrument to protect the GC column and valves. 

Replaces bar coding; electronic transmitter chip is located in sample container; chip communicates with a receiver that is interfaced with a data system; sample 

information is retained in each step of analysis process from collection to final analysis; chain of custody or audit trails established; users can store additional 

information about the samples; the sample and insert can be sealed in crimp-top vials. 

Provides finger-tightened connections to columns and injector valves that can withstand pressures as great as 10,000 psi; spring tension ensures minimum dead volume 

connection; available in variety of tubing lengths with single- or double-ended fittings. 

More than 900 silanes for surface modification and functionization; mono-, di-, and trifunctional silanes, as well as custom silanes available. 

Available porosities include 1, 3, 5, and 10 m; available diameters include 20, 25, 30, 40, 50, 75, 100, and 150 m; sieves (frits) can be purchased individually, fused 

within a capillary, or within zero-dead-volume unions and endcaps; capillaries available with polyimide or UV-transparent coatings and inner diameters of 90, 105, 

165, 190, 240, and 365 m. 

Written by Nigel Simpson; covers introduction, format and sorbents, matrix effects, method development, theory, applications, matrix SPE, automation, SPE 

hyphenated techniques, and future directions; discussed applications include drug screening, veterinary, biological samples, and immunoaffinity. 

Have three- or six-column automated selectors and stainless steel construction; built-in drip tray; employ multiport valves; covered to ensure environmental isolation 

and temperature stabilization; tubing connectors organized with side tubing fasteners; PEEK tubing; has RS-232 ports. 

Reusable holder that connects directly to any HPLC column; available packed with any of company’s HPLC phases in 5-m particles; has three levels of protection: 

in-line filter, in-line filter with 1-cm guard, and frit in 2-cm guard cartridge; 10 and 20 mm 2.1 and 4.0 mm i.d. dimensions. 

Product burns the protective polyimide layer with a controlled area of approximately 2 mm of capillary length.


prepacked flash columns covered in 

“HPLC Column and Packing Series” in 

last month’s issue (1), but it is less convenient. 

Another company displayed a vacuum 

manifold and rack system for processing 

large-volume columns that can speed 

flash chromatography experiments and 

provide more operational convenience. 

GC products: A manufacturer introduced 

a guard column that is placed 

between the injector and the capillary column. 

This 5-m piece of tubing prevents 

high-boiling-point and undesirable compounds 

from entering GC capillary 

columns and improves the detection performance 

of GC–MS systems when working 

with dirty samples. 

Sample preparation products: Several 

of the sample preparation accessories 

related to 96-well plates. Two companies 

debuted flexible silicone plate covers that 

fit over the 96-wells and prevent evaporation 

and cross contamination. Sun International’s 

plate cover is preslit to allow needles 

and pipette tips to penetrate easily, 

and the cover reseals itself. Figure 4 shows 

cover mats that can be used with 96-well 

and 384-well plates. 

Rather than use SPE to remove proteins 

and other excipients from biological fluids, 

some workers prefer to precipitate them 

with acetonitrile. Then, the plasma can be 

filtered using a 96-well filtration plate or 

the precipitated protein can be removed by 

centrifugation in which the entire plate is 

placed in a modified centrifuge. Two companies 

introduced their products for this 

growing area of filtration automation. 

CE and capillary electrochromatography: 

A couple of introductions touched 

on making these techniques more user 

friendly. One was a capillary burner that 

removes a small and precise amount of the 

polyimide coating of a fused-silica CE column 

for on-column UV detection. For 

capillary electrochromatography (CEC), 

Stellar Phases 

1/3 Page Vert Ad 

Regenerant out 

Electrode 

Eluent in 

Eluent out 

Electrode 

Regenerant in 

Ion-exchange 

MonoDisc 

Regenerant out 

Eluent in 

Cation-exchange 

monolith 

Eluent out 

Regenerant in 

 

 

Cation-exchange 

membrane 

Flow distributor 

disk 

Regeneration 

chamber 

Eluent 

chamber 

Regeneration 

chamber 

Figure 3: Cross-sectional diagram of an electrolytic suppressor for IC. The suppression bed has 

10 mm 4 mm dimensions. The cation-exchange flow distributor membranes are impermeable to 

liquid flow except at small holes at their perimeter, which results in a serpentine flowpath. (Courtesy 

of Dionex Corp.) 

Circle 19


fused-silica tubing and small synthetic 

fused-silica sieves can be placed inside and 

can hold small HPLC packing materials 

inside of the capillary. The manufacturer 

can provide the silica sieves that are fused 

within the capillary or within both ends of 

a zero-dead-volume union, as well as 96- 

capillary arrays for multichannel CE from 

microwells. 

Acknowledgment 

I would like to thank the manufacturers 

and distributors that kindly furnished the 

requested information in advance of 

Pittcon 2001, thus allowing a timely report 

on new product introductions. For those 

manufacturers that would like to be considered 

for inclusion in Pittcon 2002 coverage, 

please send the name of the primary 

company contact, mailing address, fax 

number, and e-mail address to “Column 

Watch” Pittcon 2002, LCGC, 859 

Willamette Street, Eugene, OR 97401. 

Reference 

(1) R.E. Majors, LCGC 19(3), 272–288 (2001). 


“Column Watch” editor 


is business development 

manager, consumables 

and accessories 

business unit, 

Agilent Technologies, 

Wilmington, 

Delaware, and is a 

member of LCGC’s 

editorial advisory board. Direct correspondence 

about this column to “Column Watch,” 

LCGC, 859 Willamette Street, Eugene, OR 

97401, e-mail lcgcedit@lcgcmag.com. 

Figure 4: 

Sealing system for 96- and 384-well microplates. (Courtesy of Sun International.) 

JM Science 

1/4 Page Ad 

CAMAG 

1/4 Page Ad 

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