part i: general detector properties - welcome |...

Post on 29-Mar-2021

2 Views

Category:

Documents

0 Downloads

Preview:

Click to see full reader

TRANSCRIPT

Lecture 17:Chromatographic Detectors

CU- Boulder CHEM 5181

Mass Spectrometry & Chromatography

Prof. Jose-Luis JimenezFall 2002

Part I:General Detector

Properties

Important Detector Properties

• Signal-to-Noise Ratio– Sensitivity– Baseline noise

• Selectivity• Others

– Baseline drift– Response time– Dynamic range– Linear range

Detection Sensitivity

From Snyder

Detection Noise

From Snyder

Example of Signal-to-Noise Ratio (SNR)

From McNair

Relative Precision vs. Concentration

From Snyder

Detector Noise vs. Detector Drift

From McNair

Detection Selectivity

From Snyder

Definition of Detector Response Time

From McNair

Effect of Detector Time Constant

From McNair

Detector Dynamic Range

From McNair

Detector Linearity

From McNair

Part II:GC Detectors

Most Common Detectors

• Flame Ionization Detector (FID)– C atom counter

• Thermal Conductivity Detector (TCD)• Electron-Capture Detector (ECD)• MS• Up to 60 other types of detectors used

Flame Ionization Detector

From Rubinson

FID Response

From McNair

FID Implementations I

From Skoog

FID Implementations II

From McNair

Effect of H2 Flow Rate on FID Response

From McNair

Effect of Air Flow Rate on FID Response

From McNair

Need for Other Detectors than FID

From McNair

Thermal Conductivity Detector

From Rubinson2

Thermal Conductivity Detector (TCD)

From Schwedt

Thermal Conductivities of Carriers & Analytes

From McNair

Electron-Capture Detector (ECD)

From McNair

ECD Detector

From Rubinson2

Relative ECD Responses

From McNair

Properties of GC Detectors

From McNair

Concentration vs. Mass Flow Rate Detectors

From McNair

Nitrogen-Phosphorus Detector

From Rubinson2

Photoionization Detector

From Rubinson2

Infrared Detection

From Skoog

Atomic Emission Detector

From Skoog

Concentration Ranges for GC Detectors

From McNair

GC Detectors Comparison I

From McNair

GC Detectors Comparison II

From Rubinson

GC Detectors Comparison III

From Settle

GC Detectors Comparison IV

From Grant

Part III:HPLC Detectors

HPLC Detectors

• Most common: UV absorption• Alternative detectors when:

– Analytes don’t have UV absorption– Analyte concentrations are too low for UV abs.– Sample interferences are important– Structural information is required

UV Detectors

From Skoog & Snyder

Choosing a UV Wavelength

UV Diode Array Detection

From Snyder

UV Diode Array Detection

Micro-Capillary Absorption Detection

From Rubinson

Dual-Beam HPLC Detector

From Rubinson

UV Absorptivity of Common Organic Functional Groups

From Snyder

UV Absorption Spectra at Low UV Wavelengths

From Snyder

How to Increase SNR in UV Detection

From Snyder

Universal HPLC Detectors

• Used when – you want a response for all solutes on the

mobile phase• UV can have 100 to 1000 fold differences in

sensitivity between molecules– Analytes do not absorb UV

Refractive Index Detector

Evaporative Light Scattering Detector

From Snyder

Universal HPLC Detectors

From Snyder

Fluorescence Detector

From Snyder

Arrangement of LC Fluorescent Detector

From Rubinson

Other HPLC

Detectors

From Snyder

Light Scattering Detector

From Rubinson

Amperometric Detector

Viscometric Detector

From Rubinson

Post-Column Chemical Reaction Detection

From Schwedt

HPLC Detectors Comparison I

From Skoog

HPLC Detectors Comparison II

From Rubinson

HPLC Detectors Comparison III

From Cunico

top related