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1 Restek
2
3 time time time increasing time
4 μ
5
6 = = k = t r t o t o = t r ' t o
7 van Deemter Equation H A B H = height equivalent theoretical plate (HETP) A = Eddy diffusion term B = Molecular diffusion in column axis division (contributes to band broadening) C = Resistance to mass transfer (contributes to band broadening) C H (mm) R = 1 4 N 2 He H 2 (cm/s) optimum 10cm/s N optimum = 20cm/s 40cm/s HeH 2 2 L H k X X k+1-1
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9 (R) (t R ) R t R t R R t R
10 Dimethyl CH 3 Si O Phenylmethyl Si CH 3 O Diphenyl Si O Trifluoropropyl methyl CF 3 C 2 H 4 Si CH 3 O Cyanopropyl Phenyl C N (CH 2 ) 3 Si O H C H Polyethylene glycol (PEG) H C H O Biscyanopropyl C N (CH 2 ) 3 Si O (CH 2 ) 3 C N CH 3
11 CH 3 Si O CH 3 Si O Si CH 3 O C N (CH 2 ) 3 Si O CF 3 C 2 H 4 Si O CH 3 Rxi-1ms/Rtx % Rxi-5ms/Rtx -5 Rtx -20 Rtx -35 / Rtx -35MS Rtx % 80% 65% 50% 5% 20% 35% 50% Rtx % Rtx % 65% Rtx % Rtx -624 or % 6% Rtx % 14% 11
12 (%) (Rtx 5 vs. Rtx 35) Likes dissolve likes( )
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14 0.25µm Rtx -1 30m, 0.32mm ID, 0.25µm min McReynolds probes 1. 1 butanol 2. benzene 3. 2 pentanone 4. C nitropropane 6. pyridine 7. C 8 8. C 9 9. C min 70 o C isothermal
15 min 30m, 0.32mm ID, 1.0µm µm Rtx -1 McReynolds probes 1. 1 butanol 2. benzene 3. 2 pentanone 4. C nitropropane 6. pyridine 7. C 8 8. C 9 9. C min o C isothermal
16 3.0µm Rtx m, 0.32mm ID, 3.0µm min 1,2,3 5 6 All are baseline resolved McReynolds probes 1. 1 butanol 2. benzene 3. 2 pentanone 4. C nitropropane 6. pyridine 7. C 8 8. C 9 9. C min. 70 o C isothermal
17 4 30m, 0.32mm ID, 5.0µm 1,2, µm Rtx -1 7 McReynolds probes 1. 1 butanol 2. benzene 3. 2 pentanone 4. C nitropropane 70 o C isothermal 8 6. pyridine 7. C 8 8. C 9 9. C min. 9 min
18 Rtx 1: 30m, 0.53mm ID, 0.25mm Rtx 1: 30m, 0.53mm ID, 5.0mm The supplier reported the purity as 99% using this column. Pentane 40 o C isothermal A closer look on a thick film column revealed that it was not. 1mL direct injection
19 0.10mm ID 0.18mm ID 0.25mm ID 0.28mm ID 0.32mm ID 0.45mm ID 0.53mm ID GC/MS 0.1mm ID fast GC &
20 ( EPA 604 Phenols min min Rtx 5: 30m, 0.25mm ID, 0.25mm Rtx 5: 30m, 0.53mm ID, 0.25mm
21 21
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23 30.7m x 0.25mm x 0.25µm Rxi-5ms 1.4 ml/min; 8.5 C/min 15.45min 2.0 ml/min; 10.1 C/min 13.00min 4.0 ml/min; 14.3 C/min 9.23min
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25 High Bleed 25
26 High Bleed
27 High Bleed 1ng 8270 compounds small leak leaking press tight front excessive MeCl
28 High Bleed
29 Bleed fixed 1.3e e e+07 1e
30 PEG vs. PDMS Spectral Background Rtx 5Sil MS 30mx0.25mmx 1.0df ser# Spectral Background Stabilwax 30mx0.25mmx0.25df ser#
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32 TIC: C D TIC: C D Bis(2 ethylhexyl)phthalate m/z 149, 167, 279 Triphenylphosphine Oxide m/z PAH Carryover m/z 278
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34 1 Figure: Stabilwax column isothermal at 35 C. 5 C below the solid liquid phase transition temperature. Notice the differences in retention for the three overlaid chromatograms Peaks 1 Air 2 chloromethane 3 vinyl chloride 4 ethylene oxide
35 Pyridine m/z 79 10ng 2.5ng 1.0ng Fluorophenol m/z Fails 8270D Revision 4 Criteria for RRT 0.06 min
36 10ng 3.25 Pyridine m/z ng Fluorophenol m/z ng
37 Rtx-Volatile Amine 1.Pyridine 2.1,2 Butanediol 3.Nonane 4.Diethylenetriamine 5.Diethanolamine 6.2 Nonanol 7.2,6 Dimethylamine 8.Dodecane Column: Rtx Volatile Amine, 60 m, 0.32 mm ID (cat.# 18078) Sample: Volatile amine column test mix (cat.# 35008) Diluent: Methanol:dichloromethane (50:50) Conc.: 900 1,800 µg/ml snap and shoot Inj. Vol.: 1 µl split (split ratio 17.8:1)
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39 m/z--> TIC: GR3028E8.D
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45 * * * * Dichlobenil Dichlobenil in Acetonitrile Peak Splitting Oven Temperature Start 40 C
46 1 Naphthol Dichlobenil THPI OPP Pebulate Mevinphos
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溶媒 工業溶媒 Column : Equity-, 0 m x 0. mm ID,.0 µm Cat. No. : 0- Column : SPELCOWAX 0, 0 m x 0. mm ID,.0 µm Cat. No. : Column : Equity-0, 0 m x 0. mm ID,.0 µm Cat. No. : - Oven : ( min), /min to 0 ( min) Inj.:
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1,2,4-1,2,4-Trimethylbenzene Pseudocumene 1,3,5-1,3,5-Trimethylbenzene Mesitylene CH 3 CH 3 CH 3 CH 3 CH 3 CH 3 1,2,4-trimethylbenzene 1,3,5-trimethylbenzene CAS 95-63-6 CAS 108-67-8 C 9 H 12 C 9 H 12
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CONTENTS 1 004 005 006 2 008 010 010 010 011 011 012 012 013 013 014 014 3 016 016 017 018 019 019 020 020 020 021 021 022 022 022 023 023 023 023 024 024 025 025 025 025 4 028 030 031 032 032 032 032
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Isobutyl alcohol IUPAC 2-methylpropan-1-ol 2--1-2-Methyl-1-Propanol, Isobutanol CH 3 H 3 C OH CAS 78-83-1 C 4 H 10 O log P ow ( C) ( C) (kpa) (g/l) 74.12 74.14 1) -108 2) 108 2) 1.2 2) 87 2) 0.8 2) (74.1214)
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N- 1) 2) 1) GC/MS HPLC GC/MS 2) 0.01~0.05µg/l 0.5~50µg/kg GC/MS SIM GC/MS SIM GC/MS SIM a) b) -d 10 -d 10 -d 12 -d 12 c) d) 600 C 4 e) 1 99.999% f) a) b) - IX-1 - c) (ODS) 200-1,000mg 5ml 5ml 5ml d) e)
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...1...3 (Direct Injection)...5 OCI...7 PTV (...9 FID...11 ECD...13 AOC-20i/s...15...17...19 10 1 10 1 2µL 1µL 1mL 0.10.2mL He (He) 25cm/sec40cm/sec 30mL/min 1:501:100 Table Ex. Rtx-1, 515m :Ex. 100cm/sec
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N,N- N,N-Dimethylacetamide Acethyldimethylamine CAS 127-19-5 C 4 H 9 NO 87.12 ~ 87.14 87.68413 163-165 C 1) - 18.59 C 2) 1 mg/l 25 C 3) 3.3 hpa 2 C 4) log P ow -.77 2).9429 2/4 C 1) 3.1 4) 1.31E - 8 atm-m
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2,2-2,2 -Iminodiethanol Diethanol amine CAS 111-42-2 C 4 H 11 NO 2 105.1356-105.0790-28 C 1) 1.0881 g/cm 3 1)
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2,2-2,2 -Iminodiethanol Diethanol amine CAS 111-42-2 C 4 H 11 NO 2 105.1356-105.0790-28 C 1) 1.0881 g/cm 3 1)
Adenosine Triphosphate Adenosine Monophosphate min min Fig.2 Chromatograms of Nucleotides Peak
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