oru.sePublikationer
Change search
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf
Examination of technical mixtures of halogen-free phosphorus based flame retardants using multiple analytical techniques
Örebro University, School of Science and Technology. Wellington Laboratories Inc., Guelph ON, Canada. (MTM Research Centre)
Örebro University, School of Science and Technology. Norwegian Institute for Water Research, Oslo, Norway. (MTM Research Centre)ORCID iD: 0000-0001-6217-8857
Örebro University, School of Science and Technology. (MTM Research Centre)ORCID iD: 0000-0002-6330-789X
Wellington Laboratories Inc., Guelph ON, Canada; Chemistry Department, University of Guelph, Guelph ON, Canada.
Show others and affiliations
2017 (English)In: Chemosphere, ISSN 0045-6535, E-ISSN 1879-1298, Vol. 176, no June 2017, 333-341 p.Article in journal (Refereed) Published
Abstract [en]

The application of phosphorus based flame retardants as replacements for commonly used halogenated flame retardants has been gaining interest due to the possibility that these compounds may have a less significant impact on human and environmental health. Unfortunately, little is known about the chemical compositions of many of the technical products (which often are mixtures) and a single separation technique for concurrent analysis of these types of compounds has not been identified. This paper reports the results of an investigation into the constituents of three halogen free organophosphate flame retardants (OPFRs), resorcinol bis(diphenyl phosphate) (RDBPP), bisphenol A bis(diphenyl phosphate) (BPA-BDPP), and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO). The major components of commercial samples of RDBPP and BPA-BDPP were isolated by preparative TLC and characterized by NMR. A commercial sample of DOPO was found to be essentially pure, but its analysis is complicated by the fact that it can exist in ring-open and ring-closed forms. With the structures of the components confirmed by NMR, multiple analytical separation techniques (gas chromatography (GC), liquid chromatography (LC), and packed column supercritical fluid chromatography (pSFC)) were investigated for the analysis of these three technical products. Packed column supercritical fluid chromatography allows the separation of the components of all three OPFRs, including the two forms of DOPO, in a single run.

Place, publisher, year, edition, pages
Elsevier, 2017. Vol. 176, no June 2017, 333-341 p.
Keyword [en]
Organophosphate flame retardants (OPFRs); pSFC/MS method; NMR; RDBPP; BPA-BDPP; DOPO
National Category
Other Chemistry Topics Environmental Sciences
Identifiers
URN: urn:nbn:se:oru:diva-57461DOI: 10.1016/j.chemosphere.2017.02.129ISI: 000399849300038PubMedID: 28282639Scopus ID: 2-s2.0-85015851681OAI: oai:DiVA.org:oru-57461DiVA: diva2:1090752
Available from: 2017-04-25 Created: 2017-04-25 Last updated: 2017-09-11Bibliographically approved
In thesis
1. Packed Column Supercritical Fluid Chromatography: Applications in Environmental Chemistry
Open this publication in new window or tab >>Packed Column Supercritical Fluid Chromatography: Applications in Environmental Chemistry
2017 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Although gas and liquid chromatography have emerged as dominant separation techniques in environmental analytical chemistry, these methods do not allow for the concurrent analysis of chemically diverse groups of persistent organic pollutants (POPs). There are also a small number of compounds which are not easily amenable to either of these traditional separation techniques. The main objective of this thesis was to address these issues by demonstrating the applicability of packed column supercritical fluid chromatography (pSFC) coupled to mass spectrometry (MS) in various aspects of environmental chemistry.

First, pSFC/MS analytical methods were developed for legacy POPs (PCDDs, PCDFs, and PCBs) as well as the emerging environmental contaminant Dechlorane Plus (DP), and issues relating to the ionization of target analytes when pSFC was coupled to MS were explored. Novel APPI and APCI reagents (fluorobenzene and triethylamine) were optimized and real samples (water and soil) were analyzed to demonstrate environmental applicability.

The possibility of chiral and preparative scale pSFC separations was then demonstrated through the isolation and characterization of thermally labile hexabromocyclododecane (HBCDD) stereoisomers. The analytical pSFC separation of the α-, β-, and γ-HBCDD enantiomers as well as the δ and ε meso forms was shown to be superior to results obtained using a published LC method.

Finally, technical mixtures of phosphorus flame retardants (RBDPP, BPA-BDPP, and DOPO; a group of related compounds which are challenging to analyze concurrently) were examined using multiple analytical techniques and pSFC was found to be the only method which facilitated the accurate determination of the components of all 3 mixtures. This thesis confirms the potential of pSFC/MS as a fast, green, and cost effective means of separating and analyzing environmental contaminants.

Place, publisher, year, edition, pages
Örebro: Örebro University, 2017. 87 p.
Series
Örebro Studies in Chemistry, ISSN 1651-4270 ; 19
Keyword
Supercritical Fluid Chromatography, Mass Spectrometry, Ionization, POPs, APPI, APCI, chiral, achiral, packed column
National Category
Other Chemistry Topics
Identifiers
urn:nbn:se:oru:diva-56826 (URN)978-91-7529-184-0 (ISBN)
Public defence
2017-05-12, Örebro universitet, Billbergska huset, Hörsal B, Fakultetsgatan 1, Örebro, 10:15 (English)
Opponent
Supervisors
Available from: 2017-03-27 Created: 2017-03-27 Last updated: 2017-04-25Bibliographically approved

Open Access in DiVA

No full text

Other links

Publisher's full textPubMedScopus

Search in DiVA

By author/editor
Riddell, Nicolevan Bavel, BertEricson Jogsten, Ingrid
By organisation
School of Science and Technology
In the same journal
Chemosphere
Other Chemistry TopicsEnvironmental Sciences

Search outside of DiVA

GoogleGoogle Scholar

Altmetric score

Total: 90 hits
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf