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 (C)</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 (C)</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 (B)</p> Signup and view all the answers

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

<p>Define the problem (B)</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 (D)</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 (D)</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 (A)</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 (B)</p> Signup and view all the answers

What information must be presented in every analytical result?

<p>The precision of the analytical method (A)</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 (D)</p> Signup and view all the answers

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

<p>Hollow cathode lamp (B)</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 (C)</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 (A)</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 (A)</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 (D)</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 (B)</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 (A)</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 (C)</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 (A)</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 (B)</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 (B)</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) (C)</p> Signup and view all the answers

What were the two most common matrices used in FAB?

<p>Glycerol and 3-nitrobenzoic acid (D)</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 (D)</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) (A)</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 (A)</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 (C)</p> Signup and view all the answers

Flashcards

What is the purpose of chemical analysis?

The objective is to obtain useful information to address a problem or make a decision.

Describe the steps involved in chemical analysis.

A process involving the collection, preparation, and analysis of a sample to measure the presence and quantity of a specific analyte.

What are the two main categories of chemical analysis methods?

Classical (wet chemical) methods rely on chemical reactions and separations, while instrumental methods use specialized equipment.

What is Atomic Absorption Spectroscopy (AAS)?

The use of a beam of light to excite atoms in a sample, generating a characteristic signal that can be measured.

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What is the principle of Atomic Absorption Spectroscopy (AAS)?

A technique using the characteristic absorption of electromagnetic radiation by atoms to determine the concentration of a specific element in a sample.

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What is a Hollow Cathode Lamp (HCL)?

A source of radiation used in Atomic Absorption Spectroscopy (AAS).

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What is Flame Atomic Absorption Spectroscopy (FAAS)?

A type of AAS where the sample is atomized in a flame.

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What is Graphite Furnace Atomic Absorption Spectroscopy (GFAAS)?

A type of AAS where the sample is atomized in a graphite tube.

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What is the role of an atomizer in Atomic Absorption Spectroscopy (AAS)?

An atomizer is a device that converts the sample into free atoms in the gas phase.

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What is a monochromator?

A component in an Atomic Absorption Spectrophotometer that isolates the specific wavelength of light emitted by the Hollow Cathode Lamp.

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What is a Mass Spectrometer?

A device that separates ions based on their mass-to-charge ratio (m/z).

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Explain the function of a Quadrupole Mass Analyzer.

A type of mass analyzer that uses radio-frequency (RF) and direct current (DC) voltages to select ions with a specific m/z or range of m/z.

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Describe the function of an Ion Trap Mass Spectrometer.

A type of mass analyzer that traps and manipulates ions in a 3D quadrupole field.

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What is Tandem Mass Spectrometry (MS/MS)?

A type of mass spectrometry where precursor ions are fragmented and the fragment ions are measured.

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What is Selected Reaction Monitoring (SRM)?

A form of tandem mass spectrometry that selectively monitors specific fragment ions.

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What are Electroanalytical Methods?

Methods that measure electrical signals or properties of a solution.

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What is Potentiometry?

A technique that measures the electric potential difference between two electrodes.

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What is Amperometry?

A technique that measures the electric current flowing between two electrodes.

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What is Conductometry?

A technique that measures the electrical conductivity of a solution.

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Explain Fast Atom Bombardment (FAB) Ionization.

A technique used to ionize non-volatile compounds by bombarding the sample with a beam of atoms.

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What is Secondary Ion Mass Spectrometry (SIMS)?

A technique similar to FAB but using a beam of ions to ionize the sample.

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Describe Electrospray Ionization (ESI) in Mass Spectrometry.

A method that uses high voltage to create an electrospray of charged droplets from a liquid sample.

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What is Desolvation in Electrospray Ionization (ESI)?

The process of removing solvent molecules from charged droplets in ESI.

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What is Mass Spectrometry (MS)?

A technique used to analyze the chemical composition of a sample by measuring the mass-to-charge ratio (m/z) of ions.

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What is Mass Analysis?

The separation and detection of ions based on their m/z values.

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What is an Analyte?

A compound that is analyzed using an analytical technique.

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What are Standards in Chemical Analysis?

A standard used for calibration and comparison during analysis, providing a reference for evaluating the accuracy of an analysis.

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What is Accuracy?

The agreement between the measured value and the true value.

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What is Precision?

The reproducibility of measurements.

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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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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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