PMID- 11055701
OWN - NLM
STAT- PubMed-not-MEDLINE
LR  - 20191120
IS  - 1520-6882 (Electronic)
IS  - 0003-2700 (Linking)
VI  - 72
IP  - 20
DP  - 2000 Oct 15
TI  - In situ derivatization/solid-phase microextraction for the determination of 
      haloacetic acids in water.
PG  - 4865-73
AB  - An in situ derivatization solid-phase microextraction method has been developed 
      for the determination of haloacetic acids (HAAs) in water. The analytical 
      procedure involves derivatization of HAAs to their methyl esters with dimethyl 
      sulfate, headspace sampling using solid-phase microextraction (SPME), and gas 
      chromatography-ion trap mass spectrometry (GC/ITMS) determination. Parameters 
      affecting both derivatization efficiency and head-space SPME procedure, such as 
      the selection of the SPME coating, derivatization-extraction time and 
      temperature, and ionic strength, were optimized. The commercially available 
      Carboxen-poly(dimethylsiloxane) (CAR-PDMS) fiber appears to be the most suitable 
      for the determination of HAAs. Moreover, the formation of HAA methyl esters was 
      dramatically improved (up to 90-fold) by the addition of tetrabutylammonium 
      hydrogen sulfate (4.7 micromol) to the sample as ion-pairing agent in the 
      derivatization step. The precision of the in situ derivatization/HS-SPME/GC/ITMS 
      method evaluated using an internal standard gave relative standard deviations 
      (RSDs) between 6.3 and 11.4%. The method was linear over 2 orders of magnitude, 
      and detection limits were compound-dependent, but ranged from 10 to 450 ng/L. The 
      method was compared with the EPA method 552.2 for the analysis of HAAs in various 
      water samples, and good agreement was obtained. Consequently, in situ 
      derivatization/HS-SPME/GC/ITMS is proposed for the analysis of HAAs in water.
FAU - Sarrion, MN
AU  - Sarrion MN
AD  - Departament de Quimica Analitica, Facultat de Quimica, Universitat de Barcelona, 
      Spain.
FAU - Santos, FJ
AU  - Santos FJ
FAU - Galceran, MT
AU  - Galceran MT
LA  - eng
PT  - Journal Article
PL  - United States
TA  - Anal Chem
JT  - Analytical chemistry
JID - 0370536
EDAT- 2000/10/31 00:00
MHDA- 2000/10/31 00:01
CRDT- 2000/10/31 00:00
PHST- 2000/10/31 00:00 [pubmed]
PHST- 2000/10/31 00:01 [medline]
PHST- 2000/10/31 00:00 [entrez]
AID - 10.1021/ac000479d [doi]
PST - ppublish
SO  - Anal Chem. 2000 Oct 15;72(20):4865-73. doi: 10.1021/ac000479d.