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Instrumental Analysis – Exam 2 Questions with Verified Answers – GC, HPLC, Detectors, Ionization Sources, and Mass Spectrometry Fundamentals

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This document presents a highly detailed and fully verified set of questions and answers for Exam 2 in Instrumental Analysis, with emphasis on chromatography and mass spectrometry. It covers principles and instrumentation for gas chromatography (GC) and high-performance liquid chromatography (HPLC), including column types, stationary and mobile phases, gradient elution, and temperature programming. The content also explores detector technologies (FID, TCD, ECD, fluorescence, UV-Vis), ionization techniques (EI, CI, ESI, MALDI), mass analyzers (TOF, quadrupole), and hybrid systems. Additionally, it addresses sample introduction methods, eluent strength, system components, and signal response mechanisms, making it ideal for in-depth exam prep.

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Institution
Instrumental Analysis
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Instrumental Analysis

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Uploaded on
June 6, 2025
Number of pages
16
Written in
2024/2025
Type
Exam (elaborations)
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Questions & answers

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Instrumental Analysis Exam 2 questions with
verified answers
Advantage to desorption sources? Ans✓✓✓ applicable to nonvolatile
and thermally unstable samples.


advantage to ECD? Ans✓✓✓ - extremely sensitive


advantages and disadvantages of hard-ionization sources; example?
Ans✓✓✓ Advantage: provides useful information about the kinds of
functional groups/structure of the analytes
Disadvantage: too much fragmentation
**Electron ionization (EI)


advantages and disadvantages of soft-ionization sources; example?
Ans✓✓✓ Advantages: little fragmentation and provides accurate info
about the molecular mass of the analyte
Disadvantage: limited information about the structure
**Chemical ionization (CI)


Advantages to FID detectors? Ans✓✓✓ - insensitive to noncombustible
gases (CO2, CO, SO2, noble gases)
- high sensitivity
- large linear response

,- low noise
- easy to use


Advantages to hyphenated MS? Ans✓✓✓ - gain ret. time and mass
spectrum for each solute eluted
- spectrometer can be highly selective for analyte of interest
- selectivity eases requirements for sample prep or complete
chromatographic separation of components in mixture


Advantages to TCD? Ans✓✓✓ - simple and universal
- large linear range
- responds to organic and inorganic species
- nondestructive to sample


Common support material in HPLC column? Ans✓✓✓ *Silica is most
common
- surface modified with thin polymer layers to create desired
interaction chemistry


Construction of GC column? Ans✓✓✓ - from fused silica and stainless
steel or glass and teflon
- formed as coils 10-30cm diameter

, def. base peak Ans✓✓✓ most abundant peak in the mass spectrum
assigned a value of 100


def. detector (transducer) mass spec Ans✓✓✓ (Detector amplifies ion
current as a funct. of m/z) amplifies ion current when different species
of ions impinge on detector at different times. mass spec shows
detector current as func. of m/z.


def. eluent strength Ans✓✓✓ the measure of the solvent adsorption
energy on the S phase


def. Gas-liquid chromatography (GLC/GC) Ans✓✓✓ - based on liquid S
phase
- retention of analyte due to partition between gaseous M phase and
liquid S phase
- wide applications; most widely used separation technique


def. Gas-solid chromatography (GSC) Ans✓✓✓ - based on solid S phase
- retention of analyte due to physical adsorption
- limited application


def. hyphenated MS Ans✓✓✓ separation coupled with MS detection

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