Quadrex 007-1, DIMETHYLPOLYSILOXANE

The non-polar 007-1 dimethylpolysiloxane phase, which separates compounds according to boiling point, is probably the most frequently used phase type in GC. Bonding and crosslinking this general purpose GC phase increases the resistance to degradation by rinsing, large solvent injections and the deposition of non-volatiles. The 007-1 phase offers excellent efficiency and thermal stability. In addition, this non-polar phase is less susceptible to oxidation and hydrolysis than phases incorporating more polar functional groups.

• Bonded and Crosslinked
• Non polar
• Excellent thermal stability
• Comparable to: SE-30, OV-1, OV-101
• Similar phases: DB-1, Rtx -1, HP-1, Ultra-1, SPB-1, CPSil-5CB, AT-1, BP-1, DB-Petro, DB-2887, RTx-PONA, RTx-2887, HP-PONA, Petrocol-DH, Petrocol-2887, CP-SimDist-CB, At-Petro
• USP Phase Specification: G1, G2

007-1 PHAT™ Phase Columns

In addition to the standard range of column configurations offered with the 007-1 phase type, our unique coating technology allows us to extend the functional range of columns coated with the 007-1 phase by the application of very thick films. For example, films up to 3.5 microns on 0.10mm I.D. fused silica and 18.0 microns on 0.53mm I.D. fused silica are now possible. These PHAT Phase™ thick film columns are ideal for low molecular weight analyses previously performed on packed columns.

Advantages of PHAT PHASE™ fused silica capillary columns include:

• greater sample size for trace analyses of very volatile compounds
• increased retention of volatile compounds leading to higher elution temperatures

GC analyses of gases and other types of low molecular weight compounds have been traditionally accomplished on packed columns with heavy loadings or adsorbent type columns. More recently, porous layer open tubular (PLOT) capillary columns have been utilized in the separation of low molecular weight applications despite the drawbacks in using these types of columns such as sample adsorption and bead migration within the column.

Attempts have been made to use ‘thick filmed’ wall coated open tubular (WCOT) capillary columns but the films have typically been confined to a maximum of 8.0 microns due to limitations in conventional column coating technology. While these ‘traditional’ thick film columns have been used for some for low molecular weight applications, they could not attain the separations and sample loadings that could be achieved on packed columns.

By employing our proprietary coating technique we are now able to reproducibly manufacture fused silica capillary columns having phase ratios comparable to heavily loaded packed columns. The PHAT Phase™ columns are available with 007-1, dimethylpolysiloxane and our 007-5, 5% phenyl methylpolysiloxane phases in lengths up to 30 meters. These PHAT Phase™ thick film capillary columns are ideal for low molecular weight analyses previously performed on packed columns.

The two SEM photomicrographs below are of a 0.53mm I.D. fused silica column coated with 007-1 dimethylpolysiloxane PHAT Phase™. Figure 1 (at 142x magnification) clearly shows the internal diameter of the 0.53mm I.D. column and the thick film coated on the internal surface. Note that the phase coating is similar in thickness to the columns’ outer polyimide coating, which is typically 15-20 microns.

Figure 1. SEM of 0.53mm I.D. column bore showing PHAT Phase™ inner phase layer. Compare this inner phase layer to the outer polyimide layer of approximately 15-20 microns.

Figure 2. SEM measurement confirms the inner phase layer
at 18.0 microns.

007-1 dimethylpolysiloxane columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Quadrex 007-10 and 007-20,
10% and 20% PHENYL METHYLPOLYSILOXANE

007-10 and 007-20 (10% and 20% phenyl substitution, respectively) are the Quadrex designations of phenyldimethylpolysiloxane phases. The phenyl substitutions contribute to the “induced dipole” selectivity of these phases. A column coated with either phase displays excellent efficiency and thermal stability. These phases provide an excellent alternative for drug and environmental pollutant analyses where greater retention of aromatic compounds is necessary.

• Bonded and crosslinked
• Comparable to: OV-3, OV-7
• Similar phases: Rtx -20, SPB-20
• USP Phase Specification: G32

007-10 and 007-20 Phenyl Methylpolysiloxane columns are available in all standard column I.D.’s and column lengths. The film thickness ranges are noted in the chart below.

Specifications:

Quadrex 007-1301,
(6% CYANOPROPYLPHENYL) METHYLPOLYSILOXANE

The 007-1301 is a (6% cyanopropylphenyl) methylpolysiloxane phase. Overall, 007-1301 is a low polarity phase which exhibits excellent thermal stability. The cyanopropyl (permanent dipole) and the phenyl (polarizable) substituents provide a specific selectivity for polar and polarizable compounds. More of a boiling point phase than 007-1701 (14% cyanopropyl phenyl methylpolysiloxane), the 007-1301 exhibits less retention of polyaromatic compounds than 007-17 (50% phenyl methylpolysiloxane).

Nitrogen-containing herbicides, various types of pesticides, drugs and other heteroatom-containing compounds are good candidates for separation using this phase.

As part of the 007 Series of Bonded Phases, the 007-1301 can withstand large solvent injections and rinsing to remove insoluble impurities.

• Bonded and crosslinked
• Excellent thermal stability
• Moderately polar
• Similar phases: DB-1301, Rtx -1301, HP-1301, SPB-1301
• USP Phase Specification: G43

007-1301 (6% Cyanopropylphenyl) Methylpolysiloxane columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Specifications:

Quadrex 007-17, (50% PHENYL) METHYLPOLYSILOXANE

007-17 is a 50% phenyl methylpolysiloxane phase. The presence of the 50% phenyl groups increases the overall “polarity” of the phase and enhances the selectivity of induced dipole interactions resulting in greater retention of aromatic solutes. The 007-17 phase is widely used as an EPA Method confirmation column and provides for efficient separations of PAHs, and biomedical samples such as drugs, sugars and steroids.

• Bonded and crosslinked
• Medium polarity
• Comparable to OV-17
• Similar phases: DB-17, Rtx-50, SPB-50, AT-50, HP-17, HP-50+, CPSil-20CB
• USP Phase Specification: G3

007-17, (50% Phenyl) Methylpolysiloxane columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Specifications:

Quadrex 007-1701,
(14% CYANOPROPYLPHENYL) METHYLPOLYSILOXANE

007-1701 is a (14% cyanopropylphenyl) methylpolysiloxane phase. The cyanopropyl functional groups provide a permanent dipole selectivity different from the induced dipole interactions of the phenyl groups. The overall “polarity” of this phase remains nominal when compared to the more highly cyanopropyl substituted phases such as 007-225 and 007-23. The 007-1701 phase is often used for solvents, pharmaceuticals, derivitized sugars and many environmental applications.

• Bonded and crosslinked
• Moderately polar
• Comparable to OV-1701
• Similar phases: DB-1701, Rtx-1701, SPB-1701, AT-1701, HP-1701, BPX-1701
• USP Phase Specification: G46

007-1701, (14% Cyanopropylphenyl) Methylpolysiloxane columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Specifications:

Quadrex 007-225,
(50% CYANOPROPYLPHENYL) METHYLPOLYSILOXANE

007-225 is the Quadrex designation for a 50% cyanopropylphenyl methylpolysiloxane. This phase possesses both permanent dipole interactions (nitrile) as well as induced dipole (phenyl) and dispersion interactions. It has unique selectivity for derivitized compounds such as fatty acids and carbohydrates. Non-volatile residues can be rinsed from the column to restore column performance.

Quadrex 007-225 columns have been cited in a number of estrogen assay methods. The most commonly used 007-225 column configurations are 15M. x 0.25mm x 0.25µm film, our # 007-225-15-0.25F, and 30M. x 0.25mm x 0.25µm film, our # 007-225-30-0.25F.

• Bonded and crosslinked
• Moderately polar
• Comparable to OV-225
• Similar phases: DB-225, Rtx -225, AT-225, SP-2300, BP-225, CPSil-43CB
• USP Phase Specification: G19

007-225, (50% Cyanopropylphenyl) Methylpolysiloxane columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Specifications:

Quadrex 007-23, (78% CYANOPROPYL) METHYLPOLYSILOXANE

The 007-23 is a (78% cyanopropyl) methylpolysiloxane and is our most polar phase type. The strong permanent dipole interactions of this phase with unsaturated compounds yields separations according to geometric configurations of the double bonds.

The 007-23 phase is ideal for the separation of cis/trans isomers of fatty acid methyl esters (FAMEs) as well as the isomers of dioxins and furans.  The 007-23 phase is bonded and crosslinked and the column performance can be restored by rinsing.

• Bonded and crosslinked
• Very polar
• Comparable to Silar 7CP, SP-2310
• Similar phases: DB-23, Rtx-2330, BPx-70, SP-2330, AT-Silar, CPSil 88
• FAME column

007-23, (78% Cyanopropyl) methylpolysiloxane columns are available in 30M. and 60M. lengths with 0.25µm films only.  Column I.D.’s are noted below.

Specifications:

Quadrex 007-35, (35% PHENYL) METHYLPOLYSILOXANE

007-35 is the Quadrex designation for a (35% phenyl) dimethylpolysiloxane phase. This phase is a compromise between 007-20 and 007-17 in phenyl content. It is a popular phase for drug analyses; and like the entire series of phenyl-substituted phases, columns coated with the 007-35 can be rinsed to remove non-volatile and high boiling contaminants.

• Bonded and crosslinked
• Excellent thermal stability
• Moderately polar
• Comparable to OV-11
• Similar phases: DB-35, Rtx-35, SPB-35, AT-35, HP-35, BPX-35
• USP Phase Specification: G42

007-35, (35% Phenyl) Methylpolysiloxane columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Specifications:

Quadrex 007-5, (5% PHENYL) METHYLPOLYSILOXANE

The 007-5 phase is a (5% phenyl) methylpolysiloxane polymer. Like the 007-1 dimethylpolysiloxane phase, the 007-5 phase is a widely used general purpose GC phase ideal for a broad range of applications. The presence of the phenyl groups provides induced dipole interactions leading to degrees of increased retention for aromatic solutes. A 5% phenyl substitution causes a nominal increase in polarity; yet the 007-5 phase displays the attributes of a non-polar phase.

The non-polar 007-5 phase, which separates compounds according to boiling point, is another frequently used phase type in GC. Bonding and crosslinking this general purpose GC phase increases the resistance to degradation by rinsing, large solvent injections and the deposition of non-volatiles. The 007-5 phase offers excellent efficiency and thermal stability. In addition, this non-polar phase is less susceptible to oxidation and hydrolysis than phases incorporating more polar functional groups.

• Bonded and Crosslinked
• Non polar
• Excellent thermal stability
• Comparable to: SE-52, SE-54, OV-73
• Similar phases: DB-5, Rtx -5, HP-5, Ultra-5, SPB-5, CPSil-8CB, AT-5, BP-5
• USP Phase Specification: G27

007-5 PHAT™ Phase Columns

Similar to the 007-1 dimethylpolysiloxane phase, the 007-5 is offered in very thick films as noted below. In addition to the standard range of column configurations offered with the 007-5 phase type, a new coating technology developed at Quadrex allows us to extend the functional range of columns coated with this phase type by the application of very thick films of the 007-5 phase. For example, films up to 3.5 microns on 0.10mm I.D. fused silica and 18.0 microns on 0.53mm I.D. fused silica are now possible. These PHAT phase™ thick film columns are ideal for low molecular weight analyses previously performed on packed columns.

Advantages of PHAT PHASE™ fused silica capillary columns include:

• greater sample size for trace analyses of very volatile compounds
• increased retention of volatile compounds leading to higher elution temperatures

GC analyses of gases and other types of low molecular weight compounds have been traditionally accomplished on packed columns with heavy loadings or adsorbent type columns. More recently, porous layer open tubular (PLOT) capillary columns have been utilized in the separation of low molecular weight applications despite the drawbacks in using these types of columns such as sample adsorption and bead migration within the column.

Attempts have been made to use ‘thick filmed’ wall coated open tubular (WCOT) capillary columns but the films have typically been confined to a maximum of 8.0 microns due to limitations in conventional column coating technology. While these ‘traditional’ thick film columns have been used for some for low molecular weight applications, they could not attain the separations and sample loadings that could be achieved on packed columns.

By employing our proprietary coating technique we are now able to reproducibly manufacture fused silica capillary columns having phase ratios comparable to heavily loaded packed columns. The PHAT phase™ columns are available with 007-1, dimethylpolysiloxane and our 007-5, 5% phenyl methylpolysiloxane phases in lengths up to 30 meters. These PHAT phase™ thick film capillary columns are ideal for low molecular weight analyses previously performed on packed columns.

The two SEM photomicrographs below are of a 0.53mm I.D. fused silica column coated with 007-1 dimethylpolysiloxane PHAT phase™. Figure 1 (at 142x magnification) clearly shows the internal diameter of the 0.53mm I.D. column and the thick film coated on the internal surface. Note that the phase coating is similar in thickness to the columns’ outer polyimide coating, which is typically 15-20 microns.

Application areas for these PHAT phase™ columns include the analysis of natural gas, auto emissions, light hydrocarbon refinery cuts, amines, alcohols, free fatty acids, refrigerants, residual solvents and air pollutants as defined in the EPA TOC Methods.

007-5 5% phenyl methylpolysiloxane columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Quadrex 007-5MS, SILPHENYLENE POLYSILOXANE

Traditional polysiloxane-type GC stationary phases degrade at elevated temperatures. The degradation process is well documented and consists of the thermal rearrangement of the siloxane backbone to produce cyclic groups. These groups are volatile and elute from the column as column ‘bleed’. The silphenylene units (Fig. 1) within the 007-5MS backbone act as heat sinks and limit the formation of the cyclic groups normally associated with polysiloxane degradation.

Figure 1, Silphenylene/polysiloxane phase unit.

The 007-5MS silphenylene columns offer the chromatographer a number of advantages:

• greater thermal stability
• greater resistance to oxygen degradation
• fast ramping to elevated temperatures to purge the column of residual components
• improved analysis of trace level compounds
• less baseline bleed equals less baseline noise, which results in lower detection limits
• increased column lifetimes
• reduced contamination of MS sources and other GC detector surfaces
• “cleaner” mass spectra…mass spectra with fewer extraneous ions enables the analyst to achieve more accurate compound identification and a more efficient library search

Figure 2, 007-5MS Silphenylene Baseline Bleed

A typical 007-5MS baseline bleed is shown above in Figure 2. The mass spectrum of the baseline bleed is shown below in Figure 3.

Figure 3, 007-5MS Silphenylene Mass Spectrum.
Note the low abundance of key ions.

While a typical methylpolysiloxane bleed spectrum shown below in Figure 4. yields high abundance’s of ions with m/z 207, 281, 355, the mass spectrum of the 007-5MS silphenylene column (above, Fig. 3.) yields significantly lower abundance of these ions. Additionally, it is apparent from Figure 3 that there is a reduction in the total number of ions resulting in “cleaner” spectrum and less background interference.

Figure 4, Typical Methylpolysiloxane Mass Spectrum

007-5MS Silphenylene Polysiloxane columns are available in all standard column I.D.’s and in limited column lengths. The film thickness ranges are noted in the chart below.

Specifications:

Quadrex 007-608, 007-624, and 007-502, CYANOPROPYLPHENYL METHYLPOLYSILOXANES

007-608, 007-624, and 007-502 offer three variations of cyanopropylphenyl substitutions on a methylpolysiloxane backbone. These phases have been specifically designed for the analysis of volatile organic compounds and pesticides as specified in many EPA Methods including 502.1, 502.2, 503.1, 524.1, 524.2, 601, 602, 608, 624, 8010, 8011, 8015, 8020, 8240, and 8260. By using 007-502 and 007-624 phase types on 0.53mm I.D. columns, the entire range of volatile compounds, including gases, can be analyzed beginning at ambient temperatures.

• Bonded and crosslinked
• Specifically designed for volatile organic compound analyses
• Similar phases: DB-624, DB-1301, Rtx-502, DB-608, VOCOL, RTX-Volatiles, PB-608, Rtx-35, AT-624, BP-624, CPSil-13CB
• USP Phase Specification: G43

007-608, 007-624 and 007-502 Cyanopropylphenyl Methylpolysiloxane columns are most commonly requested in the following column I.D.’s and column lengths. The film thickness ranges are noted in the chart below.

Specifications:

007-65HT, (65% PHENYL) METHYLPOLYSILOXANE

The 007-65HT phases represent a (65% phenyl) methylpolysiloxane phase composition. They are a companion phase to the 007-17 (50% phenyl methylpolysiloxane), but the additional 15% phenyl substitution provides greater selectivity toward compounds exhibiting induced dipole effects. This enhanced selectivity is most evident in the analysis of triglycerides where the resolution is “fine tuned” over that of the 50% phenyl substitution.

The 007-65HT is a bonded phase which possesses excellent thermal stability and hence can be used routinely for high temperature analyses.

Columns coated with the 007-65HT phase type are ideal for the analysis of biofuel/biodiesel total glycerin and methyl esters under ASTM Method D6584-00.

• Bonded and crosslinked
• Excellent thermal stability
• Moderately polar
• Similar phases: Rtx-65HT, TAP-CB

007-65HT, (65% Phenyl) Methylpolysiloxane columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Specifications:

007-CW and OXYGEN-RESISTANT BTR-CW, POLYETHYLENE GLYCOL (PEG) POLYMER

007-CW and BTR-CW are the Quadrex designations for an ethylene glycol/siloxane copolymer. This polymer can be used to separate compounds at temperatures not normally associated with polyethylene glycol (PEG, Carbowax™) phases. Both the lower and upper temperature limits of traditional Carbowax type columns are extended with this phase.

In addition, Quadrex offers a modified version of the 007-CW phase, designated BTR-CW, which incorporates an anti-oxidant moiety to better withstand oxygen degradation. The BTR-CW phase offers increased thermal stability and longer column lifetimes. See additional information below.

The hydrogen bonding interactions of the 007-CW and BTR-CW phases makes them well suited for the analysis of polar compounds such as solvents, flavors, perfumes, and essential oils. These phases are not recommended for the analysis of mixtures containing silylating reagents.

• Bonded and crosslinked
• Moderately polar
• Comparable to Carbowax 20M™*
• Similar phases: DB-Wax, Stabilwax, AT-Wax, HP-20M, HP-Innowax, Supelcowax-10, BP-20, CPWax-52CB
• USP Phase Specification: G16

* Carbowax is a trademark of Union Carbide Corporation

BTR-CW, OXYGEN-RESISTANT PHASE:

Columns coated with bondable PEG and, even more so with traditional Carbowax 20M, deteriorate in the presence of oxygen. It has been necessary, therefore, to maintain an oxygen-free chromatographic system. To lower the costs of maintaining such a system and to improve the chromatographic properties of the PEG-type columns, we offer the oxygen-resistant BTR-CW phase type. BTR-CW is a polyethylene glycol (PEG) phase, similar to our 007-CW phase, but which incorporates an anti-oxidant moiety to better withstand oxygen exposure and the resultant degradation. The BTR-CW also offers increased thermal stability and longer column lifetimes.

007-CW/BTR-CW, Polyethylene Glycol (PEG) columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Specifications:

007-FFAP, NITROTEREPHTHALIC ACID MODIFIED POLYETHYLENE GLYCOL (PEG) POLYMER

007-FFAP is a nitroterephthalic acid modified polyethylene glycol (PEG) polymer. This bonded acidic phase is ideal for the analysis of aqueous solutions of free fatty acids as well as fatty acid methyl esters. As with the 007-CW (and BTR-CW) polyethylene glycol phases, 007-FFAP is not recommended for the analysis of silylating reagents.

• Bonded and crosslinked
• Moderately polar
• Comparable to FFAP, OV-351, SP-1000
• Similar phases: DB-FFAP, AT-1000, HP-FFAP, Stabilwax DA, BP-21, CPWax-58CB, Nukol, CPWax-58CB
• USP Phase Specification: G25

007-FFAP, Acid-Modified Polyethylene Glycol (PEG) columns are available in all standard column I.D.’s and lengths. The film thickness ranges are noted in the chart below.

Specifications: