Agilent PBDE Analysis Using an Agilent J W DB-5ms Ultra inert GC Column
Contents
1. Authors Kenneth Lynam and Doris Smith Agilent Technologies 2850 Centerville Road Wilmington DE 19808 USA PBDE Analysis Using an Agilent J amp W DB 5ms Ultra Inert GC Column Application Brief Environmental Introduction Polybrominated diphenyl ether PBDE analyses are important tools for understand ing food supply and environmental quality worldwide In this application trace level PBDE analysis is demonstrated using electron impact GC MS For these challeng ing separations knowing that each GC column has been thoroughly tested for col umn inertness gives the analyst higher confidence in the accuracy of the results Agilent has implemented new testing procedures to more effectively evaluate GC column inertness performance These new testing procedures employ deliberately aggressive probes to thoroughly investigate column inertness and quality These extremely active probes including 1 propionic acid 4 picoline and trimethyl phos phate are used to verify each column s inertness performance Capillary GC column activity as a potential source of result uncertainty has been virtually eliminated with the Ultra Inert series of columns PBDE Analyses PBDE 209 is a particularly challenging analyte because of its long retention and ten dency to degrade with high temperature exposure High temperature thermal stabil ity is an issue for this class of compounds but is more pronounced for BDE 209 as it is highly brominated and we2. lium 72 cm s constant flow i H Inlet Pulsed splitless 325 C 20 psi until 1 5 min purge flow GC MSD Triple Axis Detector coupled with an Agilent J amp W 50 mL min at 2 0 min DB 5ms Ultra Inert GC capillary column Inlet liner Deactivated dual taper direct connect Agilent p n G1544 80700 Access the full application note at Column Agilent J amp W DB 5ms Ultra Inert 15 m x 0 25 mm 0 25 pm http www chem agilent com Library applications Agilent p n 122 5512UI 5989 9571EN pdf Oven 150 to 325 C 17 C min hold 5 min Detection MSD source at 300 C quadrupole at 150 C transfer line at 300 C scan range 200 1000 amu This application successfully demonstrates the use of a 15 m Agilent J amp W DB 5ms Ultra Inert capillary GC column for trace level BDEs in a 15 min analysis Linearity was excellent for all eight BDEs studied yielding 0 997 or greater R values down to a 0 005 ng 0 025 ng for BDE 209 on column loading of each component One of the reasons for the excellent lin earity and high R values is the highly inert surface of the col umn The lack of chemically active sites makes these columns an excellent choice for trace level applications The Agilent 6890 5975B GC MSD SIM mode equipped with an inert electron impact source had excellent sensitivity with even the most challenging BDE in this set BDE 209 The sig nal to noise ratio for a 0 025 ng on column loading of BDE 209 was greater than three to one with this
3. ll retained One key to successful BDE analysis is to limit the time that these compounds are exposed to high temperatures A 15 m long column as opposed to a typical 30 m long column was used in this instance to limit residence time for BDE 209 Fortunately the BDEs resolve well with symmetrical peak shapes when using Agilent J amp W DB 5ms ultra inert phase enabling success ful separation on the shorter column Figure 1 shows a total ion chromatogram of the eight BDEs investigated in this study Agilent Technologies a l 1404 7 A 1 BDE 47 5 BDE 153 1204 2 BDE 100 6 BDE 183 4 3 BDE 99 7 BDE 205 1007 4 BDE 154 8 BDE 209 E 804 T 694 ME 204 0 E 4 m e amaa m _ 6 00 7 00 8 00 9 00 10 00 11 00 12 00 13 00 14 00 Time Figure 1 Total ion chromatogram SIM mode of a 0 005 ng BDEs 47 100 99 154 153 183 and 205 and 0 025 ng BDE 209 on column loading on an Agilent J amp W DB 5ms Ultra Inert 15 m x 0 25 mm 0 25 pm capillary GC column p n 122 5512UI Table1 Chromatographic Conditions shows clearly the power of using an Agilent J amp W DB 5ms GC Agilent 6890N 5973B MSD Ultra Inert capillary GC column for trace level BDE analysis Sampler Agilent 7683B 5 0 uL syringe Agilent p n 5188 5246 1 0 pL Lower limits of quantification are expected when using one of splitless injection s ng gach comporient on column Agilent s latest GC MS offerings such as the 6890N 5975C Carrier He
4. system This result www agilent com chem Agilent shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing performance or use of this material Information descriptions and specifications in this publication are subject to change without notice Agilent Technologies Inc 2011 Printed in the USA February 11 2011 5990 5651EN j Agilent Technologies
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Agilent PBDE Analysis Using an Agilent J W DB 5ms Ultra inert GC Column