TOPIC: Gradient Analysis of PAH's using an Alliance System
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1 L * t MILLENNIUM APPLICATION BRIEF TOPIC: Gradient Analysis of PAH's using an Alliance System AUTHOR: Stuart Oehrle Date: 07/12/96 INTRODUCTION: Analysis of the 16 common PAH's was done using an Alliance system. This gradient HPLC method was done using a Supelcosil PAH colmn and A waters developed ternary gradient. Figure 1 is a chromatgram of the separation of the 16 common PAH's. As can be seen all PAH's are separated in less than 20 minutes. Total analysis times of less than 25 minutes is possible using this method. Figures 2 and 3 are overlay plots for six (6) replicate injections of this mixture. As shown in these plots very good gradient reproducibility is found. This is further shown in figure 4 which is a summary report for retention times of all 16 PAH's. Retention time percent RSD's of less than 0.1% were achieved EXPE_NTAL: HPLC Analysis Mobile phase: Flow rate: Detection: Colunm: Temperature: A: Water B: Methanol C: Acetonitrile 1.0 ml/min 254nm Supelcosil PAH (4.6 X 150mm) 30 degrees Celsius GradientTable FIGURES: Time Flow %A %B %C %D # (min) (ml) (%) (%) (%) (%) Curve Ii i ii i ii o.oo o.o o.o 1oo.o o.o 11 Figure 1: Chromatogram of PAH Mix Figure 2 and 3: Overlay of 6 injections of PAH Mix Figure 4: Summary Report for 6 injections. MB52_.,_
2 W a t e r s C o r p o r a t i o n ' Sample Information P_ 2690 Sample T_e: UnSown 2 -- Vol_e (_): Run T_e: 25.0 _n 996 Date Processed: 06/03/96 01:22:59 PM Acquired: 06/01/96 04:58:48 PM Dilution: Method: Stu P_01 S_l_ame: P_ Std (.075-3_)-7_ Channel Name: 254_ Col,m_Bts : S_elco P_-4.6X150_n-I. 0mL/_n-Waters Grad-30C _ n d _ m _,, ' i ' ' ' ' I ' ' ' ' I ' ' ' ' 5.00 i _nu_s Pe_Re_ Ret Time _ea Height # N_e (mn) (uv*sec) (uv) 1 Napthalene Acenaphthylene Acenapthene Fluorene Phenanthrene Anthracene FiuOranthene Pyrene Benzo(a)anthracene i0 Chrysene Ii Benzo(b)fluoranthene Benzo(k)fluoranthene Benzo(a)pyrene Dibenzo(a,h)anthracene Benzo(g,h,i)perylene Indeno(l,2,3-cd)pyrene r n K e n t u c k y L a b R e p o r t Page: 1 of 1
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4 1 Acenaphthylene 254nm PAH Std (.075-3mL)-7uL Acenaphthylene 254nm PAH Std (.075-3mL)-7uL Acenaphthylene 254nm PAH Std (.075-3mL)-7uL Acenaphthylene 254nm PAH Std (.075-3mi) -7uL IAcenaphthylene 254nm PAH Std (.075-3mL) -7uL Acenaphthylene 254nm PAH Std (.075-3mL) -7uL Summary -- Min: min Max: min Average: / min Std. Deviation: min %RSD: li Acenapthene 254nm PAH Std (.075-3mL)-7uL Acenapthene 254nm PAH Std (.075-3mL)-7uL Acenapthene 254nm PAH Std (.075-3mL)-7uL Acenapthene 254nm PAH Std (.075-3mL)-7uL Acenapthene 254nm PAH Std (.075-3mL)-7uL Acenapthene 254nm PAH Std (.075-3mL)-TuL Summary-- Min: min Max: min Average: / min Std. Deviation: min %RSD: Anthracene 254nm PAH Std (.075-3mL)-7uL Anthracene 254nm PAH Std (.075-3mL) -7uL Anthracene 254nm PAH Std (.075-3mL)-7uL Anthracene 254nm PAH Std (.075-3mL)-7uL Anthracene 254nm PAH Std (.075-3mL)-7uL Anthracene 254nm PAH Std (.075-3mL)-7uL Summary -- Min: min Max: min Average: / min Std. Deviation: min %RSD: K e n t u c k y L a b R e p o r t Page: 1 of 6
5 & ,_ o " 1, '_"-,/ i i, oooo- _-_--,,_'-_._.i! i_i '-_ ' ' " : ' ' ' ' i ' ' ' ' I ' ' ' ' I ' ' ' ' 0. O0.5. O0 10. O O0 Minutes Sam_les # Sample Name Channel Channel Name Date Processed 1 PAH Std (.075-3mL)-7uL nm 06/03/96 01:22:01 PM 2 PAH Std (.075-3mL)-7uL nm 06/03/96 01:22:59 PM 3 PAH Std (.075-3mL)-7uL nm 06/03/96 01:24:20 PM 4 PAH Std (.075-3mL)-7uL nm 06/03/96 01:25:32 PM 5 PAH Std (.075-3mL)-7uL nm 06/03/96 01:26:59 PM 6 PAH Std (.075-3mL)-7uL nm 06/03/96 01:27:41 PM i N o r t h e r n K e n t u c k y L a b R e p o r t Page: 1 of 1
6 Peak Results # Name Channel Name SampleName (min) 1 Benzo(a)anthracene 254nm PAH Std (.075-3mL)-7uL Benzo (a) anthracene 254nm PAH Std (.075-3mL) -7uL ii Benzo(a)anthracene 254nm PAH Std (.075-3mL)-7uL Benzo (a) anthracene 254nm PAH Std (.075-3mL)-7uL Ii Benzo(a)anthracene 254nm PAH Std (.075-3mL)-7uL Benzo (a) anthracene 254nm PAH Std (.075-3mL)-7uL ii Summary-- Min: rain Max: min Average: / min Std. Deviation: min %RSD: # Name Channel Name S amplename (rain) 1 Benzo(a)pyrene 254nm PAH Std (.075-3mL)-7uL Benzo (a) pyrene 254nm PAH Std (.075-3mL)-7uL Benzo(a)pyrene 254nm PAH Std (.075-3mL)-7uL Benzo (a) pyrene 254nm PAH Std ( mL)-7uL Benzo(a)pyrene 254nm PAH Std (.075-3mL)-7uL Benzo(a)pyrene 254nm PAH Std (.075-3mL)-7uL Summary-- Min: min Max: min Average: / min Std. Deviation: min %RSD: # Name Channel Name S amplename (min) 1 Benzo(b)fluoranthene 254nm PAH Std (.075-3mL)-7uL Benzo (b) fluoranthene 254nm PAH Std (.075-3mL) -7uL Benzo(b)fluoranthene 254nm PAH Std (.075-3mL)-7uL Benzo (b) fluoranthene 254nm PAH Std (.075-3mL) -7uL Benzo (b) fluoranthene 254nm PAH Std (.075-3mL) -7uL Benzo (b) fluoranthene 254nm PAH Std (.075-3mL) -7uL Summary-- Min: min Max: min Average: / min Std. Deviation: min %RSD: K e n t u c k y L a b R e p o r t Page: 2 of 6
7 Peak Re_lts #! Name Channel Name SampleName (rain) 1 Benzo(g,h,i)perylene 254nm PAH Std (.075-3mL)-7uL Benzo (g, h, i) perylene 254nm PAH Std (.075-3mL)-7uL Benzo (g, h, i) perylene 254nm PAH Std (.075-3mL)-7uL Benzo (g, h, i) perylene 254nm PAH Std (.075-3mL)-7uL Benzo (g, h, i) perylene 254nm PAH Std (.075-3mL)-7uL Benzo (g, h, i) perylene 254nm PAH Std (.075-3mL)-7uL Summary-- Min: rain Max: min Average: / min Std. Deviation: min %RSD: Benzo (k) fluoranthene 254nm PAH Std (.075-3mL) -7uL Benzo (k) fluoranthene 254nm PAH Std (.075-3mL)-7uL Benzo (k) fluoranthene 254nm PAH Std (.075-3mL)-7uL Benzo (k) fluoranthene 254nm PAH Std (.075-3mL)-7uL Benzo (k) fluoranthene 254nm PAH Std (.075-3mL) -7uL Benzo (k) fluoranthene 254nm PAH Std (.075-3mL) -7uL Summary-- Min: min Max: min Average: / min Std. Deviation: min %RSD: # Name Channel Name S amplename (min) 1 Chrysene 254nm PAH Std (.075-3mL) -7uL ii Chrysene 254nm PAH Std (.075-3mL)-7uL Chrysene 254nm PAH Std (.075-3mL)-7uL II Chrysene 254nm PAH Std (.075-3mL)-7uL ii Chrysene 254nm PAH Std (.075-3mL)-7uL ii Chrysene 254nm PAH Std (.075-3mL) -7uL ii Summary -- Min: ii. 930 min Max: ii. 967 min Average: / min Std. Deviation: min %RSD: K e n t u c k y L a b R e p o r t Page: 3 of 6
8 l 1 Dibenzo (a, h) anthracene 254nm PAH Std ( mL) -7uL Dibenzo (a, h) anthracene 254nm PAH Std ( mL)-7uL Dibenzo (a, h) anthracene 254nm PAH Std ( mL) -7uL Dibenzo (a, h) anthracene 254nm PAH Std ( mL) -7uL Dibenzo (a, h) anthracene 254nm PAH Std ( mL)-7uL Dibenzo (a, h) anthracene 254nm PAH Std ( mL) -7uL Summary -- Min: rain Max: min Average : / min Std. Deviation: min %RSD: Fluoranthene 254nm PAH Std (.075-3mL)-7uL Fluoranthene 254nm PAH Std (.075-3mL)-7uL Fluoranthene 254nm PAH Std (.075-3mL)-7uL Fluoranthene 254nm PAH Std (.075-3mL)-7uL Fluoranthene 254nm PAH Std (.075-3mL)-7uL Fluoranthene 254nm PAH Std (.075-3mL)-7uL Summary-- Min: min Max: min Average: / min Std. Deviation: min %RSD: # Name Channel Name S amplename (rain) 1 Fluorene 254nm PAH Std (.075-3mL)-7uL Fluorene 254nm PAH Std (.075-3mL)-7uL Fluorene 254nm PAH Std (.075-3mL)-7uL Fluorene 254nm PAH Std (.075-3mL)-7uL Fluorene 254nm PAH Std (.075-3mL)-7uL Fluorene 254nm PAH Std (.075-3mL)-7uL Summary-- Min: min Max: min Average: / min Std. Deviation: min %RSD: K e n t u c k y L a b R e p o r t Page: 4 of 6
9 Peak Results # Name Channel Name S amplename (min) 1 Indeno(l,2,3-cd)pyrene 254nm PAH Std (.075-3mL)-7uL Indeno(l,2,3-cd)pyrene 254nm PAH Std (.075-3mL)-7uL Indeno(l,2,3-cd)pyrene 254nm PAH Std (.075-3mL)-7uL Indeno(l,2,3-cd)pyrene 254nm PAH Std (.075-3mL)-7uL Indeno(l,2,3-cd)pyrene 254nm PAH Std (.075-3mL)-7uL Indeno(l,2,3-cd)pyrene 254nm PAH Std (.075-3mL)-7uL Summary -- Min: min Max: rain Average: / min Std. Deviation: min %RSD: # Name Channel Name S amplename (min) 1 Napthalene 254nm PAH Std (.075-3mL)-7uL Napthalene 254nm PAH Std (.075-3mL)-7uL Napthalene 254nm PAH Std (.075-3mL) -7uL Napthalene 254nm PAH Std (.075-3mL)-7uL Napthalene 254nm PAH Std (.075-3mL)-7uL Napthalene 254nm PAH Std (.075-3mL)-7uL Summary-- Min: min Max: min Average: / min Std. Deviation: min %RSD: 0.I01 # Name Channel Name S amplename (rain) 1 Phenanthrene 254nm PAH Std (.075-3mL)-7uL Phenanthrene 254nm PAH Std (.075-3mL)-7uL Phenanthrene 254nm PAH Std (.075-3mL)-7uL Phenanthrene 254nm PAH Std (.075-3mL)-7uL Phenanthrene 254nm PAH Std (.075-3mL)-7uL Phenanthrene 254nm PAH Std (.075-3mL)-TuL Summary-- Min: min Max: min Average: / min Std. Deviation: min %RSD: K e n t u c k y L a b R e p o r t Page: 5 of 6
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