Section: 8 | Solid-Phase Microextraction Sorbents |

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SOLID-PHASE MICROEXTRACTION SORBENTS

Thomas J. Bruno and Paris D. N. Svoronos

While trapping sorbents have been used for many years in headspace analysis (most commonly with gas chromatography), the modern techniques of solid-phase microextraction (SPME) are particularly applicable to survey analyses (Ref. 1). In the following tables, we provide information for the selection and application of the various fibers, modifications to fiber materials and data on salting out reagents (Refs. 1–5). For information on other trapping sorbents, chelating agents, resins, and polymeric phases used for headspace analysis, see Ref. 1.

References

Bruno, T. J., and Svoronos, P. D. N., CRC Handbook of Basic Tables for Chemical Analysis – Data-Driven Methods and Interpretation, Fourth Edition, CRC Press/Taylor & Francis, Boca Raton, FL, 2021. [https://doi.org/10.1201/b22281]
Rumble, J. R., Ed., CRC Handbook for Chemistry and Physics, 102nd Edition, CRC Press, Boca Raton, FL, 2021.
NIST Chemistry Web Book, <www.webbook.nist.gov/chemistry>.
Machata, G., Clin. Chem. Newsletter 4, 29, 1972.
Ioffe, B. V., and Vitenberg, A. G., Head Space Analysis and Related Methods in Gas Chromatography, Wiley Interscience, New York, 1983.
Fritz, J.S., Solid Phase Extraction, Wiley-VCH, New York, 1999.

Fiber Selection Criteria

The main fiber selection parameters are polarity and relative molecular mass. Table 1 provides general guidelines on the applicability of available fibers relative to these two parameters. The fibers are characterized by the extraction mechanism, either adsorption or absorption. Adsorbent fibers contain particles suspended in polydimethyl siloxane (PDMS) or polyethylene glycol (PEG, Carbowax). The column definitions for Table 1 are as follows.

Column heading	Definition
Fiber	Name of acronym of fiber; see below for list of acronyms
Type of fiber	Indication of whether fiber extraction mechanism is adsorption or absorption
Polarity	Indication of polarity of fiber
RMM range	Relative molecular mass range that is the ideal range for optimum extraction. Ranges can be extended by varying extraction times, but results will not be optimized

PDMS – Polydimethylsiloxane
DVB – Divinylbenzene (3 μm to 5 μm particles)
PEG – Polyethylene glycol
Carboxen – Carboxen 1006 (contains micro-, meso-, and macro-tapered pores) (3 μm to 5 μm particles)

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Table 1. Polarity and Relative Molecular Mass Range of Selected Fibers

Fiber	Type of fiber	Polarity	RMM range
7 μm PDMS	Absorbent	Nonpolar	150–700
30 μm PDMS	Absorbent	Nonpolar	80–600
85 μm Polyacrylate	Absorbent	Moderately polar	60–450
100 μm PDMS	Absorbent	Nonpolar	55–400
50 μm Carbowax (PEG)	Adsorbent	Polar	50–400
PDMS-DVB	Adsorbent	Bipolar	50–350
Carbowax-DVB	Adsorbent	Polar	50–350
PDMS-DVB-Carboxen	Adsorbent	Bipolar	40–270
PDMS-Carboxen	Adsorbent	Bipolar	35–180
Carbopak Z-PDMS	Adsorbent	Nonpolar	50–500

Phase Material Characteristics

Polydimethylsiloxane (PDMS):

Similar in properties to the OV-1 or SE-30 silicone phases (Ref. 1); nonpolar fluid suitable for nonpolar or slightly polar analytes; thicker coatings extract more analyte, but require longer extraction times; thicker coatings may show carryover effects; useful for hydrocarbons, aldehydes, ketones, and esters.

Polyacrylate:

Rigid solid material; moderate polarity; diffusion of analytes through bulk is relatively slow because of rigidity of material; relatively higher desorption temperatures required because of rigidity of material; can be oxidized easily at higher temperatures; must use oxygen-free carrier gas and ensure gas chromatographic system is leak-free; fibers are very solvent resistant; darkens to a brown color upon exposure to temperatures in excess of 280 °C, but fiber is generally still usable until color becomes black; useful for alcohols.

Carbowax (polyethylene glycol, PEG):

Similar in properties to the PEG coatings used extensively in chromatography; moderately polar; highly cross-linked to counteract water solubility; sensitive to attack by oxygen at temperatures in excess of 220 °C, at which point the fiber will darken and become powdery; requires use of high purity carrier gas (typically He at 99.999 % mass/mass) treated for oxygen contamination.

Divinylbenzene (DVB):

Similar to the properties of divinylbenzene porous polymer phases; higher polarity than Carbowax, and when combined with Carbowax results in a more polar phase; like polyacrylate, it is a solid particle that must be carried in a liquid to coat on a fiber.

Carboxen:

Similar to the material used in Carboxen porous-layer open tubular (PLOT) columns; structure has an approximately even distribution of macro-, meso-, and micropores, making it valuable for smaller analytes; larger analytes can show hysteresis that must be addressed by desorption at 280 °C; useful for hydrocarbons, ethers, aldehydes, and ketones.

Extraction Capability of Solid-Phase Microextraction Sorbents

Table 2 shows the extraction capability of the fibers for acetone, a small, moderately polar analyte, for 4-nitrophenol, a medium size polar analyte, and benzo(GHI)perylene, a large nonpolar analyte. This provides a general guideline for fiber selection.

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Table 2. Approximate Linear Concentration Ranges for Acetone, 4-Nitrophenol, and Benzo[ghi]perylene

Fiber	Acetone 10 min ext^a (FID)	4-Nitrophenol 20 min ext^b(GC/MS)	Benzo[ghi]perylene 20 min ext
7 μm PDMS	100 ppm and up	Not extracted	100 ppt to 500 ppb
30 μm PDMS	10 ppm and up	10 ppm and up	100 ppt to 10 ppm
85 μm Polyacrylate	1 ppm to 1000 ppm	5 ppb to 100 ppm	500 ppt to 10 ppm
100 μm PDMS	500 ppb to 1000 ppm	500 ppb to 500 ppm	500 ppt to 10 ppm
50 μm Carbowax (PEG)	1 ppm to 1000 ppm	5 ppb to 50 ppm	25 ppb to 10 ppm
PDMS-DVB	50 ppb to 100 ppm	25 ppb to 10 ppm	10 ppb to 1 ppm
Carbowax-DVB	100 ppb to 100 ppm	5 ppb to 10 ppm	50 ppb to 5 ppm
PDMS-DVB-Carboxen	25 ppb to 10 ppm	50 ppb to 10 ppm	100 ppb to 1 ppm poorly desorbed
PDMS-Carboxen	5 ppb to 5 ppm	100 ppb to 10 ppm	Not desorbed
Carbopak Z-PDMS	10 ppm to 500 ppm	5 ppm to 100 ppm	500 ppt to 100 ppb

Note: In each case, the concentration is expressed on a mass basis (e.g., ppm mass/mass).
^aWater sample contains 25% NaCl (mass/mass)
^bWater sample contains 2% NaCl (mass/mass) acidified to pH = 2 with 0.05 M phosphoric acid
1 ppm = 1 part in 1 × 10⁶
1 ppb = 1 part in 1 × 10⁹
1 ppt = 1 part in 1 × 10¹²

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Table 3. Typical Phase Volumes of SPME Fiber Coatings

Fiber coating thickness/type	Type of fiber core	Fiber core diameter/mm	Phase volume/mm³
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PDMS	Fused silica	0.110	0.612
100 μm PDMS	Metal	0.130	0.598
30 μm PDMS	Fused silica	0.110	0.132
30 μm PDMS	Metal	0.130	0.136
7 μm PDMS	Fused silica	0.110	0.028
7 μm PDMS	Metal	0.130	0.030
85 μm PA	Fused silica	0.110	0.543
60 μm PEG	Metal	0.130	0.358
15 μm Carbopack Z/PDMS	Metal	0.130	0.068
65 μm PDMS/DVB	Fused silica	0.120	0.418
65 μm PDMS/DVB	Proprietary	0.130	0.440
65 μm PDMS/DVB	Metal	0.130	0.440
75 μm Carboxen-PDMS	Fused silica	0.120	0.502
85 μm Carboxen-PDMS	Proprietary	0.130	0.528
85 μm Carboxen-PDMS	Metal	0.130	0.528
50/30 μm DVB/Carboxen	Metal
Carboxen layer		0.130	0.151
DVB layer		0.190	0.377
50/30 μm DVB/Carboxen	Metal

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SOLID-PHASE MICROEXTRACTION SORBENTS

References

Fiber Selection Criteria

Table 1. Polarity and Relative Molecular Mass Range of Selected Fibers

Phase Material Characteristics

Polydimethylsiloxane (PDMS):

Polyacrylate:

Carbowax (polyethylene glycol, PEG):

Divinylbenzene (DVB):

Carboxen:

Extraction Capability of Solid-Phase Microextraction Sorbents

Table 2. Approximate Linear Concentration Ranges for Acetone, 4-Nitrophenol, and Benzo[ghi]perylene

Table 3. Typical Phase Volumes of SPME Fiber Coatings

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