Section: 8 | Solid-Phase Microextraction Sorbents |
Help Manual

Page of 2
Type a page number and hit Enter.
/2
  Back to Search Results
Type a page number and hit Enter.
Additional Information
Summary of table differences
No records found.
How to Cite this Reference
The recommended form of citation is:
John R. Rumble, ed., CRC Handbook of Chemistry and Physics, 102nd Edition (Internet Version 2021), CRC Press/Taylor & Francis, Boca Raton, FL.
If a specific table is cited, use the format: "Physical Constants of Organic Compounds," in CRC Handbook of Chemistry and Physics, 102nd Edition (Internet Version 2021), John R. Rumble, ed., CRC Press/Taylor & Francis, Boca Raton, FL.

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

  1. Bruno, T. J., and Svoronos, P. D. N., CRC Handbook of Basic Tables for Chemical Analysis, 3rd Edition, CRC Press, Boca Raton, FL, 2011. [https://doi.org/10.1201/b10385]
  2. Haynes, W. M., Ed., CRC Handbook for Chemistry and Physics, 95th Edition, CRC Press, Boca Raton, FL, 2011.
  3. NIST Chemistry Web Book, /www.webbook.nist.gov/chemistry/, 2009.
  4. Machata, G., Clin. Chem. Newsletter 4, 29, 1972.
  5. Ioffe, B. V., and Vitenberg, A. G., Head Space Analysis and Related Methods in Gas Chromatography, Wiley Interscience, New York, 1983.
  6. 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)

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



FiberType of fiberPolarityRMM range
7 μm PDMSAbsorbentNonpolar150–700
30 μm PDMSAbsorbentNonpolar80–600
85 μm PolyacrylateAbsorbentModerately polar60–450
100 μm PDMSAbsorbentNonpolar55–400
50 μm Carbowax (PEG)AdsorbentPolar50–400
PDMS-DVBAdsorbentBipolar50–350
Carbowax-DVBAdsorbentPolar50–350
PDMS-DVB-CarboxenAdsorbentBipolar40–270
PDMS-CarboxenAdsorbentBipolar35–180
Carbopak Z-PDMSAdsorbentNonpolar50–500


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.

 

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



FiberAcetone 10 min exta (FID)4-Nitrophenol 20 min extb (GC/MS)Benzo[ghi]perylene 20 min ext
7 μm PDMS100 ppm and upNot extracted100 ppt to 500 ppb
30 μm PDMS10 ppm and up10 ppm and up100 ppt to 10 ppm
85 μm Polyacrylate1 ppm to 1000 ppm5 ppb to 100 ppm500 ppt to 10 ppm
100 μm PDMS500 ppb to 1000 ppm500 ppb to 500 ppm500 ppt to 10 ppm
50 μm Carbowax (PEG)1 ppm to 1000 ppm5 ppb to 50 ppm25 ppb to 10 ppm
PDMS-DVB50 ppb to 100 ppm25 ppb to 10 ppm10 ppb to 1 ppm
Carbowax-DVB100 ppb to 100 ppm5 ppb to 10 ppm50 ppb to 5 ppm
PDMS-DVB-Carboxen25 ppb to 10 ppm50 ppb to 10 ppm100 ppb to 1 ppm poorly desorbed
PDMS-Carboxen5 ppb to 5 ppm100 ppb to 10 ppmNot desorbed
Carbopak Z-PDMS10 ppm to 500 ppm5 ppm to 100 ppm500 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


Table 3. Typical Phase Volumes of SPME Fiber Coatings



Fiber coating thickness/typeType of fiber coreFiber core diameter/mmPhase volume/mm3
Continued on next page...
PDMSFused silica0.1100.612
100 μm PDMSMetal0.1300.598
30 μm PDMSFused silica0.1100.132
30 μm PDMSMetal0.1300.136
7 μm PDMSFused silica0.1100.028
7 μm PDMSMetal0.1300.030
85 μm PAFused silica0.1100.543
60 μm PEGMetal0.1300.358
15 μm Carbopack Z/PDMSMetal0.1300.068
65 μm PDMS/DVBFused silica0.1200.418
65 μm PDMS/DVBProprietary0.1300.440
65 μm PDMS/DVBMetal0.1300.440
75 μm Carboxen-PDMSFused silica0.1200.502
85 μm Carboxen-PDMSProprietary0.1300.528
85 μm Carboxen-PDMSMetal0.1300.528
50/30 μm DVB/CarboxenMetal
Carboxen layer0.1300.151
DVB layer0.1900.377
50/30 μm DVB/CarboxenMetal


Page 1 of 2
1/2

Entry Display
This is where the entry will be displayed

Log In - Individual User
You are not within the network of a subscribing institution.
Please sign in with an Individual User account to continue.
Note that Workspace accounts are not valid.

Confirm Log Out
Are you sure?
Log In to Your Workspace
Your personal workspace allows you to save and access your searches and bookmarks.
Username
Password
Remember Me
This will save a cookie on your browser



If you do not have a workspace Log In click here to create one.
Forgotten your workspace password? Click here for an e-mail reminder.
Log Out From Your Workspace
Are you sure?
Create your personal workspace
Title
First Name (Given)
Last Name (Family)
Email address
Username
Password
Confirm Password


Incorrect login details
You have entered your Workspace sign in credentials instead of Individual User sign in credentials.
You must be authenticated within your organisation's network IP range in order to access your Workspace account.
Click the help icon for more information on the differences between these two accounts.
Incorrect login details
You have entered your Individual User account sign in credentials instead of Workspace credentials.
While using this network, a personal workspace account can be created to save your bookmarks and search preferences for later use.
Click the help icon for more information on the differences between Individual User accounts and Workspace accounts.
My Account

Change Your Workspace Password
Username
Current Password

New Password
Confirm New Password


Update your Personal Workspace Details
Username
Title
First Name (Given)
Last Name (Family)
Email address


Workspace Log In Reminder
Please enter your username and/or your e-mail address:

Username
Email Address


Searching for Chemicals and Properties

The CRC Handbook of Chemistry and Physics (HBCP) contains over 700 tables in over 450 documents which may be divided into several pages, all categorised into 17 major subject areas. The search on this page works by searching the content of each page individually, much like any web search. This provides a challenge if you want to search for multiple terms and those terms exist on different pages, or if you use a synonym/abbreviation that does not exist in the document.

We use metadata to avoid some of these issues by including certain keywords invisibly behind each table. Whilst this approach works well in many situations, like any web search it relies in the terms you have entered existing in the document with the same spelling, abbreviation etc.

Since chemical compounds and their properties are immutable, a single centralised database has been created from all chemical compounds throughout HBCP. This database contains every chemical compound and over 20 of the most common physical properties collated from each of the >700 tables. What's more, the properties can be searched numerically, including range searching, and you can even search by drawing a chemical structure. A complete list of every document table in which the compound occurs is listed, and are hyperlinked to the relevant document table.

The 'Search Chemicals' page can be found by clicking the flask icon in the navigation bar at the top of this page. For more detailed information on how to use the chemical search, including adding properties, saving searches, exporting search results and more, click the help icon in to top right of this page, next to the welcome login message.

Below is an example of a chemical entry, showing its structure, physical properties and document tables in which it appears.

image of an example chemical entry
We use cookies to improve your website experience. To learn about our use of cookies and how you can manage your cookie settings, please see our Cookie Policy. By continuing to use the website, you consent to our use of cookies.
Cookie Policy

Cookie Policy

We have developed this cookie policy (the “Cookie Policy”) in order to explain how we use cookies and similar technologies (together, “Cookies”) on this website (the “Website”) and to demonstrate our firm commitment to the privacy of your personal information.

The first time that you visit our Website, we notify you about our use of Cookies through a notification banner. By continuing to use the Website, you consent to our use of Cookies as described in this Cookie Policy. However, you can choose whether or not to continue accepting Cookies at any later time. Information on how to manage Cookies is set out later in this Cookie Policy.

Please note that our use of any personal information we collect about you is subject to our Privacy Policy.

What are Cookies?

Cookies are small text files containing user IDs that are automatically placed on your computer or other device by when you visit a website. The Cookies are stored by the internet browser. The browser sends the Cookies back to the website on each subsequent visit, allowing the website to recognise your computer or device. This recognition enables the website provider to observe your activity on the website, deliver a personalised, responsive service and improve the website.

Cookies can be ‘Session Cookies’ or ‘Persistent Cookies’. Session Cookies allow a website to link a series of your actions during one browser session, for example to remember the items you have added to a shopping basket. Session Cookies expire after a browser session and are therefore not stored on your computer or device afterwards. Persistent Cookies are stored on your computer or device between browser sessions and can be used when you make subsequent visits to the website, for example to remember your website preferences, such as language or font size.

Cookies We Use and Their Purpose

We use three types of Cookies - ‘Strictly Necessary’ Cookies, ‘Performance’ Cookies and ‘Functionality’ Cookies. Each type of Cookie and the purposes for which we use them are described in this section. To learn about the specific Cookies we use, please see our List of Cookies.

1. Strictly Necessary Cookies

‘Strictly Necessary’ Cookies enable you to move around the Website and use essential features. For example, if you log into the Website, we use a Cookie to keep you logged in and allow you to access restricted areas, without you having to repeatedly enter your login details. If you are registering for or purchasing a product or service, we will use Cookies to remember your information and selections, as you move through the registration or purchase process.

Strictly Necessary Cookies are necessary for our Website to provide you with a full service. If you disable them, certain essential features of the Website will not be available to you and the performance of the Website will be impeded.

2. Performance Cookies

‘Performance’ Cookies collect information about how you use our Website, for example which pages you visit and if you experience any errors. These Cookies don’t collect any information that could identify you – all the information collected is anonymous. We may use these Cookies to help us understand how you use the Website and assess how well the Website performs and how it could be improved.

3. Functionality Cookies

‘Functionality’ Cookies enable a website to provide you with specific services or a customised experience. We may use these Cookies to provide you with services such as watching a video or adding user comments. We may also use such Cookies to remember changes you make to your settings or preferences (for example, changes to text size or your choice of language or region) or offer you time-saving or personalised features.

You can control whether or not Functionality Cookies are used, but disabling them may mean we are unable to provide you with some services or features of the Website.

First and Third Party Cookies

The Cookies placed on your computer or device include ‘First Party’ Cookies, meaning Cookies that are placed there by us, or by third party service providers acting on our behalf. Where such Cookies are being managed by third parties, we only allow the third parties to use the Cookies for our purposes, as described in this Cookie Policy, and not for their own purposes.

The Cookies placed on your computer or device may also include ‘Third Party’ Cookies, meaning Cookies that are placed there by third parties. These Cookies may include third party advertisers who display adverts on our Website and/or social network providers who provide ‘like’ or ‘share’ capabilities (see the above section on Targeting or Advertising Cookies). They may also include third parties who provide video content which is embedded on our Website (such as YouTube). Please see the website terms and policies of these third parties for further information on their use of Cookies.

To learn about the specific First Party and Third Party Cookies used by our, please see our List of Cookies.

Managing Cookies

You always have a choice over whether or not to accept Cookies. When you first visit the Website and we notify you about our use of Cookies, you can choose not to consent to such use. If you continue to use the Website, you are consenting to our use of Cookies for the time being. However, you can choose not to continue accepting Cookies at any later time. In this section, we describe ways to manage Cookies, including how to disable them.

You can manage Cookies through the settings of your internet browser. You can choose to block or restrict Cookies from being placed on your computer or device. You can also review periodically review the Cookies that have been placed there and disable some or all of them.

You can learn more about how to manage Cookies on the following websites: www.allaboutcookies.org and www.youronlinechoices.com.

Please be aware that if you choose not to accept certain Cookies, it may mean we are unable to provide you with some services or features of the Website.

Changes to Cookie Policy

In order to keep up with changing legislation and best practice, we may revise this Cookie Policy at any time without notice by posting a revised version on this Website. Please check back periodically so that you are aware of any changes.

Questions or Concerns

If you have any questions or concerns about this Cookie Policy or our use of Cookies on the Website, please contact us by email to [email protected]

You can also contact the Privacy Officer for the Informa PLC group at [email protected].


Our Cookies

Here is a list of cookies we have defined as 'Strictly Necessary':

Taylor and Francis 'First Party' Cookies

JSESSIONID

TandF.ACCT.CNB.cookieId

TandF.WS.CNB.cookieId

TandF.SU.CNB.cookieId

TandF.PORTAL.cookiesAgreed

TandF.LOGIN.cookiesAgreed

TandF.HBCP.cookiesAgreed

TandF.CCD.cookiesAgreed

TandF.DNP.cookiesAgreed

TandF.DOC.cookiesAgreed

TandF.DOD.cookiesAgreed

TandF.DIOC.cookiesAgreed

TandF.POLY.cookiesAgreed

TandF.DFC.cookiesAgreed

TandF.DMNP.cookiesAgreed

TandF.DCCC.cookiesAgreed

TandF.POC.cookiesAgreed

Here is a list of the cookies we have defined as 'Performance'.

'Third Party' Cookies

Google Analytics:

_ga

_gid

_gat

Accessibility

The Voluntary Product Accessibility Template (VPAT) is a self-assessment document which discloses how accessible Information and Communication Technology products are in accordance with global standards.

The VPAT disclosure templates do not guarantee product accessibility but provide transparency around the product(s) and enables direction when accessing accessibility requirements.

Taylor & Francis has chosen to complete the International version of VPAT which encompasses Section 508 (US), EN 301 549 (EU) and WCAG2.1 (Web Content Accessibility Guidelines) for its products.

Click here for more information about how to use this web application using the keyboard.


This is replaced with text from the script
This is replaced with text from the script
Top Notification Bar Dialog Header
Your Session is about to Expire!
Your session will expire in seconds

Please move your cursor to continue.