Selection Use of Capillary ColumnsGC Capillary columns 1



































- Slides: 35
Selection & Use of Capillary Columns(GC)
Capillary columns 1. 2. 3. 4. Stationary phase Inner Diameter(mm) Length(m) Film Thickness(um)
목차 1… Resolution & Capacity(Column ID) 2… Film Thickness 3… Column Length 4… Polarity 5… Conclusion
1) Resolution 과 Capacity에 미치는 Column ID의 영향 a) Sample 조건 - sample중 목표성분의 농도 Range 한번 주입에 정량 하고자 하는 성분의 최저농도와 최고 농도의 범위 Ex 1) 목적성분의 최저 농도 목적성분의 최고농도 Detector Split Ratio Injection volumn 0. 1 mg/ml Ex 2) 100 mg/ml 1000 배 Dilution FID ECD 100 : 1 1 ul 농도 Range = 1 ng – 1000 ng 농도 Range = 1 pg – 1000 pg
Typical Column Characteristic Table
• Capacity & Resolution
Others Point (Column ID) • Dirty Sample large ID column 이 유리 비휘발성 잔류물질에 의한 영향 최소화 • Splitless, On-column Mode large ID column 정량성과 Sample transfer 효율 향상 Mass, MSD, ITD interface small ID column
Capacity에 영향을 주는 Factor • Capacity 초과 는 leading peak 발생 (Tailing Peak 는 column에 Active compound 가 흡착되어 있을 경우에 발생) 1) 2) 3) 4) Column ID Film 두께 K value 고정상에 대한 용질의 용해도
고정상에 대한 용해도 • 비극성 시료 DB-1(HP-1, OV-1, SPB-1), DB-5(HP-5, OV-5, SPB-5) 높은 Capacity DB-2330, DB-Wax, Carbowax 낮은 Capacity
Best film thickness • Low b. p 물질 • 실온, 저온 분석 thicker film 3 – 5 um • 100 – 200 ℃정도 • 300 ℃정도 1 – 1. 5 um 0. 25 – 0. 5 um • 300 ℃이상 0. 1 um
Column length ∎ Short column -단순한 화합물 분리, -High Mw sample -빠른 시간 내에 screen 목적에 응용 ∎ Long column -High resolution, -복잡한 혼합 시료 High polarity sample 두꺼운 Film의 short column이 유리
Comparision of the structure • DB-1(HP-1, OV-1) SE-30 100% dimethyl polysiloxane CH 3 Si O CH 3 100% Polarity : non-polar General purpose column High temp limit DB-1 ms, DB-1 ht • DB-5(HP-5, OV-5) (5% phenyl)methyl polysiloxane � CH 3 Si O � CH 3 5% 95% Polarity : non-polar Wide range of application High temp limit DB-5 ms, DB-5 ht, DB-XLB
DB-35(HP-35, OV-35) DB-17(HP-50, OV-17) (35% phenyl)methyl polysiloxane CH 3 � Si O Si CH 3 � O � CH 3 35% 65% Polarity : Midpolarity Ideal for confirmational analysis High temp limit DB-35 ms (50% phenyl)methyl polysiloxane Si O � CH 3 50% Polarity : Midpolarity Slightly more polar than HP-50 Solvent rinsable DB-17 ms , DB-17 ht
• DB-23(SP-2330) • DB-200(Rtx-200) -210 (50% Trifluoro- (50% Cyanopropyl)-methyl polysiloxane (35% Trifluoropropyl)-methyl polysiloxane CN * High polarity CF 3 * Mid polarity CH 2 * Designed for FAMEs CH 2 * High temp 300/320 CH 2 O Si CH 3 CH 2 * Excellent Resolution cis- transisomer * Low ECD bleed O Si CH 3 * Unique s isomer
• DB-1301 1701 225 6% low/mid 14 % mid/high 50 % mid/high (Cyanopropyl phenyl)-dimethyl polysiloxane CN CH 2 O Si � CH 3 O Si CH 3
Polyethylene Glycol(PEG) Columns
Mixture columns • DX-1 : 90% Dimethylpolysiloxane 10% Polyethylene Glycol DX-3 : 50% Dimethylpolysiloxane 50% Polyethylene Glycol DX-4 : 15% Dimethylpolysiloxane 85% Polyethylene Glycol
Special columns • • DB-ALC 1, Alc 2 DB-EVDX DB-PAS 5, 1701 P DB-Dioxin DB-VRX HP-VOC DB-Prosteel : Blood alcohol : Drug : Pesticide : PCDDs, PCDFs : Volatiles method : more polar than DB-VRX : Virtually unbreak (0. 53 mm id만 공급)
5) CONCLUSIONS
Column rinse
080 -004 -5090