Agilent Ultra-Inert chemistry for Trace Level Analysis Manual
Contents
1. Ku Aa 223 00000 193 000000 01 T8 D 102 247 00000 gt 207 00000 Fd D1 16 D 1 DB 5ms Ultra Inert 15 m x 0 25 mm x 0 25 Agilent part 122 5512UI Helium 43 8 cm sec constant flow 70 C 1min to 310 C at 20 C min splitness at 250 C 7000A Triple Quadrupole GC MS ion source at 300 C and Quadrupole at 150 C By Frank David RIC and Matthew Klee Agilent Nitro pyrene Mitra fluaranthene Z 92 94 96 99 10 102 104 106 108 11 112 114 116 118 12 122 124 mro eu e chromatograms of nitro PAHs in extract of urban air particulate sample where the concentrations for nitro naphthalene nitro anthracene nitro fluranthene and nitro pyrene were 21 pg m3 10 pg m3 77 pg m3 and 14 pg m3 respectively Deliver high sensitivity Reliable determination of trace level nitro PAHs in complex air particulate extract matrices without labor intensive sample preparation The solutes are selectively detected at pg uL level corresponding to pg m3 in air XE Agilent Technologies ISCC 2010 Vendor Seminar Column Technology for Reliable Trace Analysis Column bleed is only half the story in trace analysis e Only when a column exhibits both low bleed and low activity are results reliable e Ultra Inert columns set a new industry standard for column inertness QC testing Best columns available for reactive analytes and trace analysis Ac2. 087 8 196 8 342 8 612 8 739 8 996 9 579 9 808 11 159 11 219 11 798 12 363 12 432 12 591 13 140 14 008 14 600 14 741 14 892 16 255 17 070 17 163 17 223 17 913 18 088 19 176 19 250 20 177 20 316 20 755 20 873 21 754 21 806 21 835 21 904 21 928 22 632 24 720 24 936 25 725 25 824 26 789 26 991 30 470 30 635 31 414 RSD of RT 0 068 0 061 0 059 0 065 0 071 0 074 0 080 0 076 0 088 0 085 0 098 0 088 0 095 0 090 0 092 0 088 0 091 0 091 0 089 0 090 0 095 0 085 0 088 0 083 0 081 0 078 0 076 0 075 0 074 0 075 0 078 0 078 0 073 0 084 0 082 0 070 0 033 0 039 0 036 0 034 0 081 0 077 0 080 0 064 0 067 0 064 0 067 0 077 0 086 0 088 5 57 2 6 5 44 12 21 4 65 24 87 1 14 9 78 9 28 1 16 2 66 9 27 14 36 9 99 2 51 2 50 22 89 13 17 1 49 0 87 11 03 2 79 7 54 1 17 14 76 2 39 7 17 1 95 13 80 1 18 0 74 0 94 0 80 9 44 35 23 3 58 12 10 1 30 12 69 2 60 40 75 1 69 7 74 m z 82 134 109 237 163 165 152 164 188 165 149 166 222 152 284 266 188 178 178 256 100 149 292 197 97 326 176 160 212 202 246 360 235 165 235 165 149 235 165 129 326 325 394 396 228 240 430 428 228 149 183 183 252 252 252 264 276 278 276 Nitro PAHs Oven Inlet MSD 410 173 00000 gt 127 00000 fd 16 0 Mitra naphthalene 75 Mw 5 i m i LA
3. 8 10 Sampler Agilent 7683B 0 5 uL syringe Agilent part 5188 5246 0 02 pL split injection Carrier Hydrogen constant pressure 38 cm s Inlet Split splitless 250 C 1 4 ml min column flow split flow 900 ml min gas saver flow 75 ml min on at 2 0 min Liner Deactivated single taper w glass wool Agilent part 5183 4647 Oven 65 isothermal Detection FID at 325 C 450 ml min air 40 ml min hydrogen 45 ml min nitrogen makeup RE Agilent Technologies ISCC 2010 Vendor Seminar Ultra Inert Test Probe on an Agilent J amp W DB 5ms Ultra Inert column 18 16 14 12 ce o Sampler Carrier Inlet Liner Oven Detection 1 Propionic acid 1 Octene n Octane 4 Picoline fully probative n Nonane Trimethyl phosphate 11 1 2 Pentanediol 5 n Propylbenzene 1 Heptanol 6 7 8 0 3 Octanone a 11 n Decane pem p 8 10 min ae D OT s YS Im x Agilent 7683B 0 5 pL syringe Agilent part 5188 5246 0 02 uL split injection Hydrogen constant pressure 38 cm s Split splitless 250 C 1 4 ml min column flow split flow 900 ml min gas saver flow 75 ml min on at 2 0 min Deactivated single taper w glass wool Agilent part 5183 4647 65 C isothermal FID at 325 C 450 ml min air 40 ml min hydrogen 45 ml min nitrogen makeup Test Probes What Do We Learn est probes can highlight or mask the deficiencies of column activity e Grob type mix
4. is not probative for inertness e DB 5ms text mix is a good test for the 90s Ultra Inert test mix probes inertness and differentiates an excellent column from a mediocre one e Well designed test mix uncovers potential adsorption of acid and base analytes and raises the bar in inertness QC Column Inertness Proof in EVERY GC column box Performance Summary Sheet RE Agilent Technologies ISCC 2010 Vendor Seminar Excellent Inertness and Same Selectivity 37 30 p 26 4 15 a 19 40 9 12 H 44 45 13 18 22 2 19 29 38 5 om 1 46 50 2l l 34 41 49 23 18 x 28 32 n 10 42 FEN L l M 1 h l B 0 10 0 12 0 14 0 16 0 18 0 20 0 ff 24 26 0 260 30 0 10 overlaid TIC for semivolatiles 2 ng on column black DB 5ms Ultra Inert red DB 5ms RE Agilent Technologies ISCC 2010 Vendor Seminar Table 2 Peak number c 4A e d m nt m WH O h o4 o4 4 oq fF 4d 4 dq CO Co CO CO CO CO CO CO CO MH MH MH MHF MH PH 4 Co Ch CO OOF rs C do 1 OTF e O 50 RSD 6 was calculated by using the retention times for each compound on the DB 5 ms and DB 5 ms Ultra Inert columns Fifty Semivolatile Compound Separation using DB 5 ms and DB 5 ms Ultra Inert Columns Compound Isopho
5. to interact with any active sites on the columns ISCC 2010 Vendor Seminar Grob Type Test Mixture Not Probative Agilent J amp W DB 5ms Ultra Inert 30m x 0 25mm x 0 25um P N 122 5532UI Elevated oven temperature at 120 C Probes sweep past 30 active sites and can 25 mask solute column 20 interactions 7 Least probative probes for column d i activity Sampler Carrier Inlet Liner Oven Detection 1 1 Octanol 2 n Undecane 3 2 6 Dimethylphenol 4 2 6 Dimethylaniline 5 1 6 4 5 n Dodecane 6 Naphthalene 8 7 1 Decanol 9 8 n Tridecane 9 Methyl decanoate Competitive 5ms column I 30m 0 25mm 0 25 3 4 5 6 7 8 9 Agilent 76836 5 uL syringe Agilent part 5181 1273 1 5 uL split injection 4 ng each component Hydrogen constant pressure 37 cm s Split splitless 250 C 1 4 ml min column flow split flow 100 ml min Deactivated single taper w glass wool Agilent part 5183 4647 120 C isothermal FID at 325 450 ml min air 40 ml min hydrogen 45 ml min nitrogen makeup DB 5ms Test Mix More Probative 1 2 Ethylhexanoic acid 3 2 1 6 Hexanediol Agilent J amp W DB 5ms i 2 y 3 4 Chlorophenol Ultra Inert 4 Tridecane 30m x 0 25mm x 0 25um 25 4 5 1 Methylnaphthalene P N 122 5532UI 6 1 Undecano 7 Tetradecane 8 Dichlorohexylamine 10 5 2 4 8 10 min PA 1 Competitive 5ms column 30m x
6. 0 25mm x 0 25 25 B 7 to Dicyclohexylamine 5 H 0 2 4 6 8 10 H Sampler Agilent 7683B 5 pL syringe Agilent part 5181 1273 1 5 pL split injection 4 ng each component Carrier Hydrogen constant pressure 38 cms Inlet Split amp plitless 250 C 1 4 ml min column flow split flow 75 ml min Liner Deactivated single taper w glass wool Agilent part 5183 4647 Oven 125 C isothermal Detection HID at 320 C 450 ml min air 40 ml min hydrogen 45 ml min nitrogen makeup Ultra Inert Test Probe Mixture QC Testing for Today s Demanding Applications Column Probe ng on functional test column 1 Propionic acid Basicity 2 1 Octene Polarity 3 n Octane Hydrocarbon marker 4 4 Picoline Acidity 3 n Monane Hydrocarbon marker B Irnmethyl phosphate Acidity 1 1 2 Pentanediol 8 n Propylbenzene Hydrocarbon marker 9 1 Heptanol 10 3 ctanone Polarity 11 Hydrocarbon marker RE Agilent Technologies ISCC 2010 Vendor Seminar Ultra Inert Test Probe Mixture on a Competitive Column 1 1 Propionic acid pA Fully Probative 2 1 Octene 0 D 3 3 n Octane 4 4 Picoline _ 8 5 n Nonane 16 l 6 Trimethyl phosphate i T 1 2 Pentanediol 14 li 8 n Propylbenzene n 9 b 9 1 Heptanol _ 10 3 Octanone ig 11 n Decane 2 6 ie 0 2
7. Ultra Inert chemistry for Trace Level Analysis Cikui Liang Ph D Challenges and Needs of Today s Laboratories Challenges Qualification quantification of trace samples Keep instrument up and running e Needs Lower detection limits Improved stability in GC or GC MS system Reduce noise Injection system septa liners connections Carrier gas and detector gases Leaks Temperature settinc Stationary phase and column bleed RE Agilent Technologies ISCC 2010 Vendor Seminar What Does Column Activity look like column activity Peak tailing and 1055 reduce sensitivity of response COLUMN 01 7 D Competitive 5ms 1 Propionic acid 30m x 0 25mm x 0 25um 1 Octene n Octane 4 Picoline n Nonane Trimethyl phosphate 1 2 Pentanediol n Propylbenzene 1 Heptanol 10 3 Octanone 11 n Decane 67 nd 2 4 Column activity is the loss of detectable analytes to the GC column through non ideal chemical reactions and interactions o O NAH AWD RE Agilent Technologies ISCC 2010 Vendor Seminar How Important Column Inertness to Overall Flow Path Inertness 3C Flow Path Surface Areas Cm d cm DI Liner l 0 2 3 142 4 Seal 0 4 0 8 3 142 1 S Column 3000 0 025 3 142 23 RE Agilent Technologies What is an Ultra Inert GC Column e Not just another column claims better performance e Not hand picked from standard pr
8. oduction based on exceptional performance New approach to column manufacturing with significantly improved sensitivity and accuracy for trace samples Treated with new proprietary processes for surface treatment and deactivation resulting in much better peak shape for acidic basic and other active compounds The deactivated surface coupled with the low bleed bonded phases lead to much improved analyses and lower detection limits RE Agilent Technologies ISCC 2010 Vendor Seminar Test Probes and Column Activity QC Testing Test probes are vital to ensure the quality and reproducibility of GC columns Properly deactivated Contain the correct amount of stationary phase consistent column to column relative retention time Test probes can either highlight or mask the deficiencies of a column An organic acid e Abase e An alcohol e Non active probes e g alkanes Peak tailing or loss response of an acid or base indicates the column is basic or acidic RE Agilent Technologies June 8 2010 Weak Probes vs Strong Probes OH H3C CH3 2 6 Dimethylphenol H3C CH3 2 6 Dimethylaniline Weak Probes Acidic and basic portion of the molecules are shielded by the methyl groups of the 2 6 dimethyl substituted phenyl ring RE Agilent Technologies H C AL M 1 Propionic acid CH3 bs N 4 Picoline Strong Probes Active end of each compound is available
9. rone 1 3 Dimethyl 2 nitrobenzene SS Dichlovos Hexachlorocyclo pentadiene Dimethyl phthalate 2 6 Dinitrotoluene Acenaphthylene Acenaphthylene d10 IS 1 2 Chlorobiphenyl 2 4 Dinitrotoluene Diethyl phthalate Fluorene 2 3 Dichlorobiphenyl Hexachlorobenzene Pentachlorophenol Phenanthrene d10 IS 2 Phenanthrene Anthracene 2 4 5 Trichlorobiphenyl Heptachlor Di n butyl phthalate 2 2 4 4 Tetrachlorobiphenyl chlorpyrifos 2 2 3 4 6 Pentachlorobipheny Butachlor Pyrene d10 SS Pyrene p p DDE 2 2 4 4 5 6 Hexachlorobiphenyl p p DDD o p DDT Benzyl butyl phthalate p p DDT bis 2 Ethylhexyl adipate Triphenylphosphate SS 2 2 3 3 4 4 6 Heptachrolobipheny Ben a anthracene Chrysene d12 IS 3 2 2 3 3 4 5 6 6 Octachlorobiphenyl Chrysene bis 2 Ethylhexyl phithalate cis Permethrine trans Permethrin Benzo b fluoranthene Benzo k fluoranthene Benzo a pyrene Perylene d12 SS Indeno 1 2 3 c d pyrene Dibenz a h anthracene Benzo g h i perylene Ava RT of DB 5 ms n 5 5 647 6 047 6 351 7 129 8 084 8 195 8 342 8 611 8 737 8 993 9 572 9 804 11 153 11 218 11 795 12 357 12 426 12 585 13 133 14 001 14 587 14 733 14 882 16 247 17 058 17 153 17 214 17 901 18 077 19 162 19 235 20 157 20 301 20 731 20 851 21 737 21 805 21 834 21 903 21 928 22 605 24 692 24 906 25 704 25 802 26 766 26 966 30 434 30 594 31 373 Ava RT of DB 5 ms Ultra inert n 5 5 642 6 044 6 349 7 126 8
10. tive analytes adsorbing on the column stops productivity in its tracks Start with an Ultra Inert Column for guaranteed performance upon installation ISCC 2010 Vendor Seminar RE Agilent Technologies
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Agilent Ultra Inert chemistry for Trace Level Analysis Manual