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1 Stir Bar Sorptive Extraction (SBSE) D. Benanou, F. Acobas and M.R. De Roubin Anjou Recherche, Analytical Research Department 1 place de Turenne Saint-Maurice France ( david.benanou@generale-des-eaux.net; francoise.acobas@generale-des-eaux.net) Philip L. Wylie Agilent Technologies, Inc. 285 Centerville Road Wilmington, DE USA ( phil_wylie@agilent.com) Stir Bar Sorptive Extraction SBSE / GC/MS SIM 6 2- MIB 2,4,6-2,3,6-2,3,4-2,4,6- LOQ.1 ng/l.2 ng/l.5 ng/l MIB 1 ng/l () GC/MS 1 2 / 3 / MIB [1,2,3] MIB MIB 5 1 ng/l 1 1 ng/l [4,5]
2 [9,1,11] [6,7,8] 2,4, ng/l [12,13,14] [15] Closed Loop Stripping Analysis CLSA [16,17] 4 GC Purge and Trap CLSA 1 ng/l 2 SPME [18] MSGC SBSE sorption( ).5mm PDMS GC/MS SBSE ng/l 1. ng/l CAS 2- MIB 5 1 N/A 2,4,6-2,4,6-TCA ,3,6-2,3,6-TCA ,3,4-2,3,4-TCA ,4,6-2,4,6-TBA
![CLSA 1 ng/l 2 SPME [18] MSGC SBSE sorption( ).5mm PDMS 3 12 2 3GC/MS SBSE 6 6 1 ng/l 1.](/docs-images/42/23032966/images/page_2.jpg "ng/l CAS 2- MIB 5 1 N/A 2,4,6-2,4,6-TCA.1 2 613-75-2 2,3,6-2,3,6-TCA.")
3 SBSE 1 K O/W /ß K O/W /ß=1 5 K O/W /ß K O/W /ß 1 SPME 1 PDMS 7 1 µm 9 8 K O/W [19] SPMESBSE PDMS 2 - LLE SPME.5 µl PDMS SBSE 24 1 µl PDMS SBSESPME PDMS K PDMS/W - K O/W [19] 1 R 2 m PDMS PDMS m W ß /PDMS m 1. K o/w K PDMS/W = C PDMS = m PDMS m PDMS = m PDMS ß C W m W m W m W 2. R = mpdms = m 1 + ( K O/W) ß ( ) K O/W ß PDMS K(o/w)/ß - SPME PDMS.5 µl 1 ml2 1 4 K O/W 1 5 K O/W SBSE [2] SBSE 1 µl PDMS ß 11 ml K O/W 5 PDMS 1 5 K O/W 2SPMESBSE 1- ml SBSE SPME K O/W SBSE SBSE 3
4 SBSE SPME K(o/w) - SBSE SPME SPME PDMS.5 µl SBSE PDMS 1 µl 1. ml / CIS-4 cryofocus PTV 1 / ml/3 m.25 mm id.25 µm HP5-MS 1 / / 3 2 SIM 25 1/3 2/3 SBSE.5 1 mm 3 [21] 4 3. t 95% = d2 PDMS 2D PDMS t 95% 95 d PDMS PDMS md PDMS PDMS m 2 / D PDMS =2.5*1-1 m 2 / 3 GERSTEL GmbH, Mülheim a/d Rhur, Germany Agilent 689 -Agilent 5973 MSD Agilent Technologies, Palo Alto. CA, USA GERSTEL GmbH Mülheim a/d Rhur, Germany TDSA PTV CIS-4 PDMS.5mm 2mm GERSTEL-Twister Merck Darmstad, Germany 2-2,4,6-2,3,6-2,3,4-2,4,6-2,4,6- -d 5 Promochem France 1 µg/l MIB 4 1 2,4,6-TCA-d 5 2 µg/l ml 5 ml 125-mL Twister PDMS.5mm2mm 2,4,6-TCA-d 5 4 µl 2 Twister 2 Twister 1 MSD MSD
5 Perfluoro-5,8-dimethyl-3,6,9-trioxadodecane PFDTD PFTBA 219/69 52/ / / Probability Based Matching System NISTWiley Agilent ChemStation ,4, ,4,6- -d 5 m/z 217 MIB 3 1 SIM MIB MIB 5 2,4,6-TCA ,3,6-TCA ,3,4-TCA ,4,6-TCB
6 4 2 ng/l SIM PDMS 2 ng/l MIB 2,3,6-TCA 2 2,4,6-TCA 2,3,4-TCA 1 2,4,6-TBA SIM MIB 4 2 2,4,6-TCA ,3,6-TCA ,3,4-TCA PDMS ,4,6-TBA
7 / K O/W log K O/W KnowWin [19] 1 2 ml 1 ng 2cm Twister 47 µl PDMS 2 6 K O/W B K O/W C A 2. / K O/W log K O/W log K O/W ,4, ,3, n/a ,3, ,4, MIB A B C A B C 2,4,6-TCA A B C 2,3,6-TCA ml ml ml 2,3,4-TCA 2,4,6-TBA A B C A B C A B C ml ml ml 6. AB K O/W C K O/W 7
8 7 PDMS 1 ml 2 ml 21-mL 2 Twister PDMS ng MIB 2,4,6-TCA 2,3,6-TCA 2,3,4-TCA 2,4,6-TBA ml 7. 8
9 2 ng/l 61-mL1 Twister 21 Twister Twister Twister AFNOR XP T ng/l 7 5 2,4,6-TCA-d 5 R.999 LOQ1 RSD 2 LOQ RSD8 3 2 trueness ng/lrsd MIB 2,4,6-TCA 2,3,6-TCA 2,3,4-TCA 2,4,6-TBA 2. ng/l Twister 9
10 LOQ, R ng/l % % % MIB ,4,6-TCA ,3,6-TCA ,3,4-TCA ,4,6-TBA E+ MIB 3.E+ 2,4,6-TCA 3.E+ 2,3,6-TCA 2.E+ R 2 = E+ R 2 = E+ R 2 = E+ 1.E+1 2.E+ 1.E+1 2.E+ 1.E+1 5.E-1 5.E-1 5.E-1.E ng/l 5.E+ 5.E+ 4.E+ R 2 = E+ 3.E+ 3.E+ 2.E+ 2.E+ 1.E+1 5.E-1.E ng/l.e ng/l 2,3,4-TCA 3.E+ 3.E+ R 2 = E+ 1.E+1 5.E-1.E ng/l.e ng/l 2,4,6-TBA 3.E+ 2.E+ R 2 = E+ 1.E+1 5.E-1.E ng/l AB 1 2AB AB A B SBSE MIB SIM 1 A [C] ng/l 2- <1 <1 2,4, ,3,6- <.1 < <.5 2,3,4- <.2 <.2 2,4, B [C] ng/l
11 A B 2,4,6-TCA 2,4,6-TCA 2,4,6-TBA 2,4,6-TBA AB SIM SBSE GC/MS A 2,4,6-TCA 8 14 B 2,4,6-TBA 8 A B min 11. A 11
12 2 organoleptic quality 5 2 SBSE [C] ng/l [C] ng/l 2- <1 <1 2,4,6- <.1 <.1 2,3,6- <.1 <.1 <.5 <.5 2,3,4- <.2 <.2 2,4,6- < EIC m/z
13 6 5.6 ng/l2,4,6-2,4,6-tba GC ,4,6-TBA GC 1 ml 1g K 2 CO 3 5 L MS B ,4, ,4, ,4,6-2,4,6-TCP 2,4,6-TBP 2,4,6-TBA 2,4,6-TCP2,4,6-TBP 2,4,6-TBA 3 2 A2 BA B 1 2MIB SBSE A B2,4,6-TCA 2,3,4-TCA.1 ng/l.2 ng/l SBSE TDS/GC/MS 2,4,6-2,4,6-2,4,6-2,4,6-13. insitu TIC 13
14 B A MS B 7 7. B to to AB TIC A B A B A B A B 75 A B 1 A B AB EIC 14
15 GC/MS MIB SBSE-TD-GC/MS- TD-GC/MS SBSE AFNOR R Twister 7 SBSE MS 1. J. Mallevialle, and H. Suffet. Identification and treatment of tastes and odors in drinking water. American Water Works Association, Denver, Colorado. (1987). 2. S. E. Jensen, C. L. Anders, L. J. Goatcher, and S. E. Hrudey. Actinomycetes as a factor in odor problems affecting drinking water from the north Saskatchewan river. (1994) Wat.Res. 28(6), A. Bruchet. Solved and Unsolved Cases of Taste and Odor Episodes in the Files of Inspector Cluzeau. (1999) Wat. Sci. Tech. 4(6), H. Tuorila, T. Pyysalo, T. Hirvi. and Ad Venviläinen. Characterisation of odors in raw and tap water and their removal by ozonation. (198) Vatten 3, S. E. Hrudey, and N. J. Low. Discussion of : the effect of disinfectants on a geosmin-producing strain of Streptomyces griseus. (1992) J. appl. Bact. 73, N. N. Gerber. Volatile substances from actinomycetes : their role in odor pollution of water. (1979) CRC crit. Rev. Microbiol 7, R. C. Hoen. Causes biologiques du goût et des odeurs des approvisionnements en eau potable. OMS, (1988) Bulletin de la qualité des eaux, 13, 2 3, I. E. Suffet, K. Djanette, and A. Bruchet. The Drinking Water Taste and Odor Wheel For the Millennium: Beyond Geosmin and 2-methylisoborneol. (1999) Wat. Sci. Tech. 4(6), M. Goodfellow, and S. T. Williams. Ecology of Actinomycetes. (1983) Ann. Rev. Microbiol. 37, S. Wood, S. T. Williams, and W. R. White. Microbes as a source of earthy flavours in potable water-a review. (1983) Int. Biodetern. Bull. 19, C. P. Dionigi, D. F. Millie, A. M. Spanier, and P. B. Johnsen. Spore and geosmin production by Streptomyces tendae on several media. (1992) J. Agric. F.J. Chem. 4, L. Malleret, and A. Bruchet. A Taste and Odor Episode caused by 246-Tribromoanisole. (22) Journ AWWA. 94(7), A. Nyström, A. Grimvall, C. Krantz-Rülcker, R. Sävenhed, and K. Akerstrand. Drinking water off-flavour caused by 2,4,6-trichloroanisole. (1992) At. Sci. Tech. 25(2), A. Montiel, J. Ouvrard, S. Rigal, and G. Bousquet. Etude de l origine et du mécanisme de formation de composés sapides responsables de goûts de moisi dans les eaux distribuées. (1987) T. S.M.-L EAU 82(2), C. Anselme, K. N'Guyen, A. Bruchet, and J. Mallevialle. Can polyethylene pipes impart odors in drinking water? (1985) Environ. Technol. Let 6, E. Baltussen, P. Sandra, F. David, and C. J. Cramer. Automated Sorptive Extraction- Thermal Desorption-Gas Chromatography- Mass Spectrometry. (1999) Journ Microcol sep 11,
16 17. M. J. McGuire, and G. Izaguire. Close-Loop Stripping Analysis as a Tool for Solving Taste and Odor Problems. (1981) Jour. AWWA 73(1), L. S. De Bruin, P. D. Josephy, and J. B. Pawliszyn. Analysis of odorous compounds by SPME. (1998) Anal. Chem. 7, W. Meylan, and P. Howard. (2) Log Octanol- Water Partition Coefficient estimation Program. Syracuse Research Corporation. 2. E. Baltussen, S. Sandra, F. David, and C. J. Cramer. Stir Bar Sorptive Extraction (SBSE), a Novel Extraction Technique for Aqueous Samples: Theory and Principles. (1999) Journ Microcol sep 11, J. Pawliszyn, (1997) Solid Phase microextraction. Theory and Practice, Wiley-VCH, p Agilent GERSTELTwister GERSTEL Agilent Technologies, Inc. 23 Printed in the USA JAJP
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Isobutyl alcohol IUPAC 2-methylpropan-1-ol 2--1-2-Methyl-1-Propanol, Isobutanol CH 3 H 3 C OH CAS 78-83-1 C 4 H 10 O log P ow ( C) ( C) (kpa) (g/l) 74.12 74.14 1) -108 2) 108 2) 1.2 2) 87 2) 0.8 2) (74.1214)
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