HT8: THE PERFECT PCB COLUMN Retention data for all 209 chlorinated biphenyl congeners Peak identification for Aroclor 1242, 1254 and 1260 Congener specific selectivity, extremely low column bleed, excellent signal to noise ratio and reliable is how many describe the performance of SGE s carborane modified HT8 capillary column when applied to Aroclor and PCB analysis. Carborane based phases have long been recognised for the unique selectivity they exhibit towards complex isomer mixtures, particularly those containing aromatic ring systems. Their extremely high thermal stability and resultant compatibility with sensitive detector systems like electron capture and mass spectrometry make HT8 "the" ideal choice for the analysis of PCBs. The unique selectivity of the HT8 column is attributed to the presence of the carborane unit having an affinity towards chlorinated biphenyls (CBs) with the least number of ortho-substitutions. Fewer substitutions in the ortho position increase freedom of rotation, allowing the CB moiety to have greater interaction with the carborane unit 1. This unique HT8 phenomenon causes non-ortho substituted CBs to have increased elution times compared to their ortho-substituted congeners. This allows detection and quantitation of many important CB s used to monitor PCB occurrence and distribution in the environment. HT8 Standard 5% Phenylsiloxane Column Specifications HT8: 8% Phenyl (equiv) Polycarborane-siloxane Phase Min. Operating Temp.: -20 C Max. Operating Temp.: 360 C Max. Cycling Temp.: 370 C Separation and identification by GC/MS of the seven CB used by many regulatory and government bodies to monitor PCB occurence and distribution in the environment. Congener # Cl Position Cl # Identification by GC/MS *28 24-4 3 51 24-26 4 69 246-3 4 *52 25-25 4 150 236-246 6 *101 245-25 5 131 2346-23 6 *118 245-34 5 122 345-23 5 *153 245-245 6 *138 234-245 6 *180 2345-245 7 CB69 rarely occurs in any Aroclor mixtures Figure 1 demonstrates clearly the significant difference in selectivity of the HT8 column. By GC/MS, quantitation of CB28 using a standard 5% phenylpolysiloxane column is impossible as coelution with CB31 (with the same numbers of chlorines) occurs. HT8 separates the two congeners by a full minute allowing quantitation to be performed with ease. 1. J. deboer, Q. Dao and R. van Dortmond, J. High Resolut. Chromatogr. in print. Figure 1. Separation of CB31 & CB28
AROCLOR 1242 Phase: HT8, 0.25 μm film Column: 50 m x 0.22 mm I.D. Initial Temp.: 80 C, 2 min Rate 1: 30 C/min Temp 2: 170 C Rate 2: 3 C/min Final Temp.: 300 C. Carrier Gas: Helium, 40 psi Detector: ECD, 330 C AROCLOR 1242 Congener # Cl Position Cl # Identification by GC/MS 42 23-24 4 96 236-26 5 35 34-3 3 64 235-4 4 72 25-35 4 103 246-25 5 71 26-34 4 41 234-2 4 68 24-35 4 37 34-4 3 100 246-24 5
AROCLOR 1260 Column and Oven conditions are as listed for Aroclor 1242 AROCLOR 1260 Congener # Cl Position Cl # Identification by GC/MS 130 234-235 6 178 2356-235 7 141 2345-25 6 164 236-345 6 163 2356-34 6 138 234-245 6 160 23456-3 6 175 2346-235 7 158 2346-34 6 187 2356-245 7 182 2345-246 7 129 2345-23 6
AROCLOR 1254 Column and Oven conditions are as listed for Aroclor 1242 209 PCB CONGENERS IN ELUTION ORDER 1 2 1 14.22 2 3 1 16.54 3 4 1 16.77 10 26 2 17.49 4 2-2 2 17.64 9 25 2 19.12 7 24 2 19.28 6 2-3 2 20.17 8 2-4 2 20.51 5 23 2 20.57 19 26-2 3 21.39 14 35 2 21.55 30 246 3 21.87 18 25-2 3 23.01 11 3-3 2 23.14 17 24-2 3 23.27 13 3-4 2 23.59 12 34 2 23.67 24 236 3 23.67 27 26-3 3 23.90 15 4-4 2 24.08 32 26-4 3 24.43 16 23-2 3 24.66 54 26-26 4 24.98 23 235 3 25.17 34 35-2 3 25.31 29 245 3 25.50 26 25-3 3 25.95 50 246-2 4 25.95 25 24-3 3 26.23 31 25-4 3 26.48 53 25-26 4 26.74 28 24-4 3 26.77 51 24-26 4 27.17 21 234 3 27.38 20 23-3 3 27.61 33 34-2 3 27.63 45 236-2 4 27.66 22 23-4 3 28.13 46 23-26 4 28.44 36 35-3 3 28.55 69 246-3 4 28.64 52 25-25 4 28.66 73 26-35 4 28.79 43 235-2 4 28.95 49 24-25 4 29.01 39 35-4 3 29.15 104 246-26 5 29.23 75 246-4 4 29.33 65 2356 4 29.35 47 24-24 4 29.41 48 245-2 4 29.41 62 2346 4 29.57 38 345 3 30.07 44 23-25 4 30.38 59 236-3 4 30.51 42 23-24 4 30.73 96 236-26 5 30.91 35 34-3 3 30.95 64 236-4 4 31.10 72 25-35 4 31.13 103 246-25 5 31.23 71 26-34 4 31.29 41 234-2 4 31.40 68 24-35 4 31.52 37 34-4 3 31.57
209 PCB CONGENERS IN ELUTION ORDER 100 246-24 5 31.74 40 23-23 4 32.10 57 235-3 4 32.16 94 235-26 5 32.26 67 245-3 4 32.56 63 235-4 4 32.77 58 23-35 4 32.86 102 245-26 5 32.86 93 2356-2 5 32.93 98 246-23 5 32.94 95 236-25 5 32.97 61 2345 4 33.15 74 245-4 4 33.25 88 2346-2 5 33.32 121 246-35 5 33.42 155 246-246 6 33.43 91 236-24 5 33.47 70 25-34 4 33.56 76 345-2 4 33.76 80 35-35 4 33.82 66 24-34 4 33.98 92 235-25 5 34.51 55 234-3 4 34.61 84 236-23 5 34.71 89 234-26 5 34.89 90 235-24 5 34.94 150 236-246 6 34.97 101 245-25 5 35.02 60 234-4 4 35.25 113 236-35 5 35.26 56 23-34 4 35.33 99 245-24 5 35.47 152 2356-26 6 35.56 119 246-34 5 36.02 112 2356-3 5 36.02 145 2346-26 6 36.10 83 235-23 5 36.24 79 34-35 4 36.33 109 2346-3 5 36.33 148 235-246 6 36.55 136 236-236 6 36.62 86 2345-2 5 36.69 97 245-23 5 36.73 117 2356-4 5 36.73 125 345-26 5 36.85 116 23456 5 36.91 115 2346-4 5 37.05 87 234-25 5 37.06 111 235-35 5 37.13 78 345-3 4 37.16 154 245-246 6 37.20 85 234-24 5 37.48 120 245-35 5 37.64 110 236-34 5 37.82 81 345-4 4 37.89 151 2356-25 6 37.95 135 235-236 6 38.25 144 2346-25 6 38.39 147 2356-24 6 38.49 82 234-23 5 38.78 77 34-34 4 38.85 149 236-245 6 38.87 139 2346-24 6 38.94 140 234-246 6 39.23 188 2356-246 7 39.30 124 345-25 5 39.41 143 2345-26 6 39.52 107 235-34 5 39.66 108 234-35 5 39.69 134 2356-23 6 39.69 123 345-24 5 39.90 184 2346-246 7 39.96 106 2345-3 5 40.06 133 235-235 6 40.07 142 23456-2 6 40.08 131 2346-23 6 40.13 118 245-34 5 40.17 165 2356-35 6 40.50 146 235-245 6 40.64 114 2345-4 5 40.79 161 2346-35 6 40.88 179 2356-236 7 40.92 132 234-236 6 40.94 122 345-23 5 41.20 153 245-245 6 41.22 168 246-345 6 41.32 176 2346-236 7 41.51 141 2345-25 6 42.00 186 23456-26 7 42.15 127 345-35 5 42.15 105 234-34 5 42.22 137 2345-24 6 42.49 130 234-235 6 42.68 178 2356-235 7 42.88 164 236-345 6 43.05 163 2356-34 6 43.06 138 234-245 6 43.23 160 23456-3 6 43.37 175 2346-235 7 43.38 158 2346-34 6 43.45 187 2356-245 7 43.55 182 2345-246 7 43.56 129 2345-23 6 43.73 183 2346-245 7 44.06 166 23456-4 6 44.11 126 345-34 5 44.75 185 23456-25 7 44.81 159 2345-35 6 44.82 202 2356-2356 8 44.86 162 235-345 6 45.18 174 2345-236 7 45.20 128 234-234 6 45.26 181 23456-24 7 45.38 201 2346-2356 8 45.50 177 2356-234 7 45.61 204 23456-246 8 45.67 167 245-345 6 45.72 171 2346-234 7 46.10 197 2346-2346 8 46.14 173 23456-23 7 46.55 200 23456-236 8 47.22 172 2345-235 7 47.28 156 2345-34 6 47.37 192 23456-35 7 47.59 157 234-345 6 47.79 180 2345-245 7 47.88 193 2356-345 7 47.97 191 2346-345 7 48.40 198 23456-235 8 49.46 199 2345-2356 8 49.53 170 2345-234 7 49.90 196 2345-2346 8 50.07 203 23456-245 8 50.15 190 23456-34 7 50.16 169 345-345 6 50.25 208 23456-2356 9 50.87 207 23456-2346 9 51.53 195 23456-234 8 52.17 189 2345-345 7 52.56 194 2345-2345 8 54.22 205 23456-345 8 54.79 206 23456-2345 9 55.84 209 23456-23456 10 56.63
*Oven and Column conditions used to obtain the retention times for all 209 congeners are those used for the analysis of Aroclor 1242, 1254 and 1260. Peak Identification of the three Aroclor standards are based on the elution order as shown in the 209 PCB Congeners in elution order table. HT8 (no equivalents, unique ultra high temperature technology) 8 % Phenyl (equiv.) Polycarborane-siloxane Description Part No. 10 m x 0.1 mm ID x 0.1 micron film - FAST PCB (HT8) 054690 12 m x 0.22 mm ID x 0.25 micron film - HT8 054674 12 m x 0.32 mm ID x 0.25 micron film - HT8 054679 12 m x 0.53 mm ID x 0.50 micron film - HT8 054684 25 m x 0.22 mm ID x 0.25 micron film - HT8 054675 25 m x 0.32 mm ID x 0.25 micron film - HT8 054680 25 m x 0.53 mm ID x 0.50 micron film - HT8 054685 30 m x 0.25 mm ID x 0.25 micron film - HT8 054677 50 m x 0.22 mm ID x 0.25 micron film - HT8 054676 Specifications are subject to change without notice. AP-0040-C RevB SGE Analytical Science Pty Ltd October 2008