GC/MS 20!"#$%"&'(!"#$%&'()*+, -./01!"#$%

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1 GC/MS 20!"#$%"&'(!"#$%&'()*+, -./01!"#$% 6890/5973 GC/MSD Linda Doherty Agilent Technologies Company 1601 California Avenue Palo Alto, CA 94304!"#$%&'()*+,#-./ !"#$%&'()!"#$$%&'(!"#$%&'()*+,-!"#!"#$%&'()*+,-./0123!"#$%! (MS)!"#$%&'!" 6890!"#$ 5973!"#$%#$!"#$%&'"()*+,-./01!"#!"#$%&'!"#$%&'()*SIM!"#$! (LOD) 5 ppb!"#$%!"#$%&'()*!"#$%&'()*!"#$%&'()*+!"#$%&'()*+!!"#lod!"#$%&'()!"#$%&'()*!"#$%&'()#*+!"#$ MSD Productivity ChemStation!!"#$%&'()* GC/MS, SIM,,!!!"#$%&'()*+,-./01234!"#$%!"#$%&'()*+,!"!"#$%&'!"#$%& 20!"#!"#$%&!!"#$%&'()*+,-./01234! 1!"#$!%&'()*+,-! HPLC/DAD!"#$ /!"#

2 GC/FID!"/!"#$% GC/ MS!" /!"#$!"#!"#$%!"#$%&'HPTLC!"# LC/MS!" /! HPTLCGC/FID LC/DAD GC/MS!"#$"%&'(#)*+ LC/MS GC/MS!"#!"#$%& 6890/ 5973 GC/MSD!"#$%& 20!"#!"# $%&'()!"#$%&'!"#$%!"#$ 2 3!"!"#$%&'()*+,-./!"#$%&'()*+,-*./0 GC/MSD!"#$%&'()*+,-.!"#$%&'GC!"#$%&'(!"#$%&'()*+!"#$%& 5973 MSD!"#$%&'() (HED)!"#$%&'()*+!"#$%! Productivity ChemStation!! GC MS!"#$%&'()!"#$%&'()*+,-./0!"#$%&!"#$%&'()*GC/ MSD!"#$!"#$%&'()*+!"#$%&'()%* GC/MS!!"#$%&'()GC/MS!!"#$%&'()*+,-./012!"#$%&'!"#$%&'()!"#$%&'!()!"#$%&!"#$%&'()*!" Q-Edit!"#$%&'()*!"#$%!"#$%&'()! MS SIM!!"#$%!" MS!"#!"#$%&'()*! 20 ppb!"#$%!"#$%!"#$0.5 ppm 1/25!"# /!"#$%&'($%) (LOD)!"#$%&!"#$% 50 ppb!"#$% SIM LOD 10!"!!"# GC/MSD LOD 5:1 S/N! LOD!" 30 ppm!"#$!"#$%&'()*+!!"#$%&'()* GC!"#$!"#$%&'()*!"#!"#$%&'()*+,-.!"#$%&'(!"#$%&'()*!"#$%&'()*+ /!"#$%! 4!"#$%&'( 3-5!"#$%& 20!"#$% 5!"#$%&' 6!"#$%&!"5973 MSD!" #$%&!"# 7!"#$%&'()!"#$%& PTV!"#$%& µl!"# LVI 89!! 1-2 µl!!"#$!"#$%&'(!"!"#$!"# 10,11! 1 20!"#$ (ISTD)1-!"#$%!"CAS TexLab ChemService, Inc. (West Chester, PA, USA) 20!"#$%&!"#!"# 200 µg/ml (200 ppm)!"#$%&!"!"#$%& ppb!!"#!"#$%&100 ppm, 20 ppm, 10 ppm, 2 ppm, 1 ppm, 0.2 ppm, 0.1 ppm 0.05 ppm!"!!"#$%&'()*+!"#!"#$%&'()*!"!" 2

3 1. 20!"#$%&'!! (RT) TexLab! TexLab Q1 Q2 CAS RT 1- (ISTD) o p-! p-!"!# ,4,5-!" o , ,4-!"# ! ! ,4 -!" !"# ,4!"# o-!"# ,4 - - (o- ) ,3-!"# ,4 -!" ,3-!"#$ ,4 - - (2-!) ,3-!"!#$ !" GC!"#$!"!"!#$%!"#$%&'!"#$%&'()*+,-.!"#$ SPE!"#!"! SPE!!"#$%&'()*!"#$!!"#$%&'(!"#$%&!"#$%&'()*+,-./!"!"#$%&'(!" GC!"#!"! 50:50!!"!!"#$%&'()*!"#$%!"#$%&'!%()!"#$%$&'()*+,-./01!"!"#$%& GC!!"#( )!"#$%&'()*+,-.!!"#$%&'()*+,!"#!$!"#$ %&'()*!"#$%!!"#$%&'()!"#$%&'80!"#$%15!"# $!%&'!"#$%&!"#$%$&'!"#$%&'()!"#$%&'("#$)*+,-HP-5!"#!"#$%&'($)*!!"#$%&'()*!"#!"!"#$%&'()!"#$%&'(!"#$%&'()*+,-./012&'!"#$%&'()*+,-.!"!"#$%&'()*+P/N !"# 3

4 !!"#!"#$%&'(!)*+,-!"#$%&'()&*!"#$%&!"#$%&'(! 25!"#$!"#$%&'()!" 10 ppm!"#$%&!"#$%& SGE FocusLiner!"#$!"#$%&'()!"#$%&'FocusLiner!"#$ 20 mm!"#$!"# /!"#$%&'!"#$%&'()! Doherty 12,13!"#$%&'( GC/MSD 6890 GC 5973 MSD!"#$%!!"#$%/!"#$ALS!" MSD Productivity ChemStation! 2 3!"#$%&'()*+, GC!" MSD!"#$%&!"# GC HP-5MS: 30 m x 0.25 mm ID HP-5MS: 30 m x 0.25 mm ID x 0.25 m film; x 0.25 m film;!19091s-433!19091s-433! 1 L 1 L!"!"# FocusLiner TM! SGE P/N ! /!"# 12, 13! /!" GC!"# 80 1 min 60 1 min 112/min /min /min /min /min /min /min /min300!! 30 psi 1 min 1.6 ml/min He 1.5 ml/min He!" 1.2 min 25:1!" 7673B 7673B = 300 = 230 = 150!! AMU 2^3 a/d! SIM EMV = 200!"#! 3.2 min!" 3.5 min!!"#$% 100 ms! 14,15 35 A!" G1701BA 4

5 !!"#$%&'(!"#$%&'()! "#!"#$%&! SIM!"!"#!"#$%&'(!"#$% SIM!"#$%&'()*!"#$% &'()*+, ppm!"#$%&'(!"#$!"#$%&'()*+,!"#$ 0.1 ppm!"#$%&'() 2 2!" SIM!"# 0.05 ppm!"#$%&'()!"#$%& 100!" S/N!"!"#!"#$ S/N!"#$%& Abundance ISTD , 4, , 12, 13 14, 15, , 19, 20 0 Time--> L 0.1 ppm!"#$%&'()!"#$%&'()*+ Abundance Ion 169, Scan ppm!"#$%!"sim!"#$%! Ion 169, SIM S/N = 527 (p-p) 2175 (rms) Time-->

6 0.05 ppm!"#$%&!"#$%! S/N! 50 S/N (rms) 265!"#$ SIM! S/N! S/N (p-p) = 527S/N (rms) = 2175!"# 5 ppb!"#$%&!"#$%&!"#$%&'(sd!"#$%!"#3!"#$%!"#$% 1-µL1-ppm!"#$%&0.04 ppm!"#$%& MSD Productivity ChemStation!"#$%&!"#$%&'()*!"MSD Productivity ChemStation!!"#$%!"#$%&' 4 Abundance ISTD 3. 1 L 1-ppm!"!" 25:1!"0.04 ppm!"#$%&'()!" Time--> Banned Amines Customized Report Data File Name 2NG01.D Operator Doherty Date Acquired 01/12/97 16:58 Method File AMINESS Sample Name 2 ppm amines with 5 ppm ISTD, 1uL Misc Info 1.5 ml/min He, pulsed splitless, MeOH solvent Vial Number 33 # NAME CAS RT AMOUNT TARGET RESPONSE TEXLAB # 1) o-toluidine ppm ) p-chloroaniline ppm ) p-cresidine ppm ) 2,4,5-Trimethylaniline ppm ) 4-Chlor-o-toluidine ppm ) Toluene 2,4 diamine ppm ) 2,4-Diaminoanisole ppm Naphthylamine (ISTD) ppm ) 2-Naphthylamine ppm ) 2-Amino-4-Nitrotoluene ppm ) 4-Aminobiphenyl ppm ) 4,4'-Oxydianiline ppm ) Benzidine ppm ) 4,4'-Methylene Dianiline ppm ) o-amino Azotoluene ppm ) 3,3'Dimethyl 4,4'-Diamino ppm ) 3,3'-Dimethylbenzidine ppm ) 4,4'-Thiodianiline ppm ) 3,3'-Dichlorobenzidine ppm ) 4,4'-Methylene-bis ppm ) 3,3'-Dimethoxybenzidine ppm !"#$%& 6

7 4! MSD Productivity ChemStation!"#$!"#$%&'()*+,-!"#$%&' (TexLab)!"#$%&!"#$%&'()*+,-./()*!"#$%&'()* 6890/5973 GC/MSD!"#$%&'()*+!"#$%&'$()*+,-!"#!"#$%&'(!"#$%&' SIM!" 1-µL!"#$ MS!"# 0.1 ppm!"#$%&' ppm!!"#$%&'(sim 1 µl!"#$%&!"& 5 ppb 10 ppm!!"#$%&!"!"#$%!"#$%&'()*+&!!"#$#%&'()*+,-./!"#$%&'()*+,-./!"!"#msd Productivity Chem-Station!"#$%&'()*+ Q- Edit!"#$%&'()*+,-./012 ChemStation!"#$%&'()*!!"#$%&'(%)*+,%-.!"#$%&'()!MSD Productivity ChemStation 6890/5973 GC/MSD!!"#$%&'()*+, -"#'!"#$%&'() ppb ppm!"#$%&'()*+,-./01!"#$%&'()*+,- 7

8 ! 1. Bundesgesetzblatt, Jahrgang 1994, Teil I, Zweite Verordnung zur Änderung der Bedarfsgegenständeverordnung vom im Sinne des 5 Abs. 1 Nr. 6 des Lebensmittel- und Bedarfsgegenstände-Gesetzes (LMBG). 2. R. F. Straub, R.D. Voyksner, and J. T. Keever, Anal. Chem. 65, (1993). 3. R. D. Voyksner, R. Straub, and J. T. Keever, Environ. Sci. Technol. 27, (1993). 4. M. Klee and V. Giarrocco, Predictable Translation of Capillary Gas Chromatography Methods for Fast GC, Agilent Technology Company, Application Note , Publication Number (23) E, March Personal communciation from Peter Gautschi, Agilent Technologies GmbH, Hewlett-Packard- Str. 8, W Waldbronn, Deutschland. 6. The Method Translation software can be downloaded from the Chemical Analysis Group section of the web site at cag/servsup/usersoft/main.html. 7. P. D. Perkins, Enhanced Essential Oils Analysis Using a High Performance Benchtop GC/MS System, Application Note, Publication No. (23) E, Agilent Technologies (1997). 8. B. Wilson, P. L. Wylie, and M. S. Klee, Large Volume Injection for Gas Chromatography Using a PTV Inlet, Application Note , Publication No. (23) E, Agilent Technologies (1997) P. L. Wylie, Trace Level Pesticide Analysis by GC/MS Using Large Volume Injection, Application Note , Publication No. (23) E, Agilent Technologies Company (1997). 10. L. Doherty, Enhancing Pesticide Analysis with a Highly Sensitive GC/MSD System, Application Note, Publication No. (23) E (1997). 11. L. Doherty, Optimizing Detection of LSD: The 6890/5973 GC/MSD System, Application Note, Publication No. (23) E (1997). 12. L. Doherty, Analyzing Aromatics in Reformulated Gasoline by GC/MS, Application Note, Publication No. (23) E (1995). 13. L. Doherty, Optimizing the 6890 Series GC for High Performance Analysis, Application Note, Publication No. (23) E, Agilent Technologies Company (1997). 14. Brian Anthony, Default Emission Current for the 5973 Series MSD running G1701AA A.03.01, Service Notes G (Diffusion Pump) or G (Turbo Pump), Available from your local Service Engineer. 15. Brian Anthony, Emission Current Optimization for the 5973 Series MSD, Service Notes G (Diffusion Pump) or G (Turbo Pump), Available from your local Service Engineer.!"#$%&'()*+,-.!"!"#$%&'()*+,-./!"#$!"#$%&'!"#$!"#$%&'()2004! (23) CHCN