Methods of Chemical Analysis
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Questions and Answers

What is the primary purpose of radio-frequency spectroscopy of nuclei in a magnetic field?

  • To visualize the internal soft tissue of the body (correct)
  • To measure the conductance of a solution
  • To apply an electrical signal to an electrode
  • To study the remnant of the big bang
  • What type of spectroscopy was used to discover the three-degree blackbody radiation?

  • Conductometry
  • Microwave spectroscopy (correct)
  • Amperometry
  • Potentiometry
  • Which of the following is a characteristic of potentiometry?

  • Applying an electrical signal while monitoring current
  • Maintaining a constant potential while monitoring current
  • Measuring electric potential while maintaining a constant current (correct)
  • Applying a constant alternating-current potential while measuring conductance
  • Which of the following is a characteristic of amperometry?

    <p>Monitoring electric current while keeping the potential constant</p> Signup and view all the answers

    What is the primary purpose of electroanalytical methods?

    <p>To apply an electrical signal to an electrode while measuring a different electrical property</p> Signup and view all the answers

    What is the primary purpose of conductometry?

    <p>To measure conductance (the ability of a solution to carry an electric current) while a constant alternating-current (AC) potential is maintained between the electrodes</p> Signup and view all the answers

    What is the first step in the process of chemical analysis?

    <p>Define the problem</p> Signup and view all the answers

    What is the purpose of method modeling and plan in chemical analysis?

    <p>To develop a model representing the complex steps of the analytical method</p> Signup and view all the answers

    What step is typically the most time-consuming in the implementation of an analytical method?

    <p>Sample preparation</p> Signup and view all the answers

    What is the purpose of performing replicate measurements in chemical analysis?

    <p>To establish the precision of the method</p> Signup and view all the answers

    What step involves comparing the analyte's signal to standards of known concentration and a calibration blank solution?

    <p>Compare results with standards</p> Signup and view all the answers

    What information must be presented in every analytical result?

    <p>The precision of the analytical method</p> Signup and view all the answers

    What is the purpose of an atomizer in atomic absorption spectroscopy?

    <p>To break analytes into free atoms</p> Signup and view all the answers

    Which type of lamp emits many narrow emission lines in atomic absorption spectroscopy?

    <p>Hollow cathode lamp</p> Signup and view all the answers

    What is the purpose of a monochromator in atomic absorption spectroscopy?

    <p>To isolate a single resonance emission line</p> Signup and view all the answers

    In Flame Atomic Absorption Spectroscopy (FAAS), where does atomization of the sample occur?

    <p>In the presence of a gaseous mixture of an oxidant and a fuel</p> Signup and view all the answers

    What is the function of the graphite tube in Graphite Furnace Atomic Absorption Spectroscopy (GFAAS)?

    <p>To atomize the sample as its temperature rises</p> Signup and view all the answers

    What does the detector do in Graphite Furnace Atomic Absorption Spectroscopy?

    <p>Determines the absorbed fraction of the analytes</p> Signup and view all the answers

    What is the main purpose of the quadrupole mass analyzer described in the text?

    <p>To allow only ions with a specific m/z or range of m/z to transmit through</p> Signup and view all the answers

    What is the advantage of using a quadrupole as the first part of a tandem mass spectrometer?

    <p>It can act as a mass selector</p> Signup and view all the answers

    What is the purpose of using selected reaction monitoring (SRM) in a tandem mass spectrometer with a quadrupole?

    <p>To quantitate analytes by selecting a precursor ion and its fragment ion</p> Signup and view all the answers

    How is an ion trap mass spectrometer different from a quadrupole mass spectrometer?

    <p>It can store and manipulate ions</p> Signup and view all the answers

    What is the advantage of an ion trap mass spectrometer over a quadrupole for full scan mode?

    <p>It is more sensitive</p> Signup and view all the answers

    What is the purpose of the second analyzer in a tandem mass spectrometer with a quadrupole?

    <p>To act as a collision cell, allowing all the products to be transmitted to a third analyzer</p> Signup and view all the answers

    What technique was popular in the 80's to early 90's for ionizing non-volatile compounds?

    <p>Fast Atom Bombardment (FAB)</p> Signup and view all the answers

    What were the two most common matrices used in FAB?

    <p>Glycerol and 3-nitrobenzoic acid</p> Signup and view all the answers

    What types of adducts could form with the analyte ions in FAB?

    <p>Protons, sodium ions, potassium ions, or ammonium ions</p> Signup and view all the answers

    What technique involved replacing the atom beam in FAB with a beam of ions, typically cesium ions?

    <p>Secondary Ion Mass Spectrometry (SIMS)</p> Signup and view all the answers

    What is the principle behind Electrospray Ionization (ESI)?

    <p>Creating a spray of charged droplets by applying a high voltage to a liquid flow</p> Signup and view all the answers

    What process occurs in ESI to eject the ions from the charged droplets?

    <p>The ions are ejected by a combination of heat, vacuum, and acceleration into gas by voltages</p> Signup and view all the answers

    Study Notes

    Methods of Chemical Analysis

    • The objective of chemical analysis is to provide information to solve a problem or make a decision, whether using classical (wet chemical) or instrumental methods.

    Steps of Chemical Analysis

    • Define the problem, requiring understanding of analytical techniques, problem-solving skills, experience, and intuition.
    • Model the method, including a specific statement of the problem, information about the sample and analyte.
    • Obtain and store the sample.
    • Prepare the sample, which usually requires the largest investment of time.
    • Perform measurements, including replicates to establish precision.
    • Compare results with standards, involving a proper comparison of the analyte's signal to that of appropriate standards.
    • Refine data and perform statistical treatment, presenting the precision of the analytical method.

    Radiation Sources

    • Deuterium lamps (DL) and electrodeless discharge lamps (EDL) are popular radiation sources.

    Atomizers

    • Atomizers break analytes into free atoms to analyze elements for their atomic constituents.
    • Flame atomizers and graphite tube atomizers are commonly used in atomic absorption spectroscopy.
    • Flame Atomic Absorption Spectroscopy (FAAS) involves nebulizing a solution of the sample into a flame.
    • Graphite Furnace Atomic Absorption Spectroscopy (GFAAS) involves atomization in an open-ended graphite tube.

    Monochromators

    • A monochromator isolates a single resonance emission line from the hollow cathode lamp's many narrow emission lines.
    • It collects light with many wavelengths and selects a narrow wavelength band.

    Quadrupole Mass Analyzer

    • A quadrupole mass analyzer uses a combination of radio-frequency (RF) and direct current (DC) voltages to select ions with a specific m/z or range of m/z.
    • It is a low-resolution analyzer, often used in GC-MS and LC-MS applications.
    • Quadrupole mass analyzers can be used in tandem mass spectrometry with selected reaction monitoring (SRM).

    Ion Trap Mass Spectrometer

    • Ion trap mass spectrometers are a type of three-dimensional quadrupole that can store and manipulate ions.
    • They are more sensitive than simple quadrupole mass analyzers and can acquire tandem mass spectra.

    Electroanalytical Methods

    • Electroanalytical methods measure electrical signals or properties of a solution.
    • Techniques include potentiometry (measuring electric potential), amperometry (measuring electric current), and conductometry (measuring conductance).

    Fast Atom Bombardment (FAB) and Secondary Ion Mass Spectrometry (SIMS)

    • FAB involves bombarding a sample with a beam of atoms, typically Ar or Xe, to ionize non-volatile compounds.
    • The sample is mixed with a matrix, such as glycerol or 3-Nitrobenzoic acid, which allows the sample to refresh itself.
    • SIMS replaces the atom beam with a beam of ions, typically cesium ions.

    Electrospray Ionization (ESI)

    • ESI creates an electrospray by applying a high voltage to a flow of liquid at atmospheric pressure, sometimes assisted by a concurrent flow of gas.
    • The created spray is directed into the vacuum system of the mass spectrometer, where the droplets are de-solvated and ions are ejected and accelerated into the mass analyzer.

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    Description

    Learn about the steps involved in chemical analysis, from defining the problem to method modeling and planning. Understand the objectives behind performing chemical analysis using classical or instrumental methods.

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