Analytical Techniques: Mass Spectrometry

Leo A. Raphaelian, Chemical Technology Division, Argonne National Laboratory

General Use

- Analysis of complex mixtures of volatile compounds

- In mass spectrometry/mass spectrometry, analysis of nonvolatile compounds

- In pyrolysis gas chromatography/mass spectroscopy, analysis and quality control of polymers

- In liquid chromatography/mass spectrometry, analysis of heat-sensitive and degradable compounds, such as biological materials

Examples of Applications

- Gas chromatography/mass spectrometry: Mixtures of volatile compounds in petroleum oil, coal gasification and liquefaction products, oil shale, and tar sands; pollutants in air, waste water, and solid waste; drugs and metabolites; pesticides; and additives, such as antioxidants and plasticizers in plastics

- Liquid chromatography/mass spectrometry: Mixtures of nonvolatile and heat-sensitive compounds

- Mass spectrometry/mass spectrometry: Mixtures of nonvolatile and high molecular weight solids

- Pyrolysis gas chromatography/mass spectrometry: Analysis of polymers and their additives

Samples

- Form: Solids, liquids, and gases; all organics and some inorganics

- Size: For gas chromatography/mass spectrometry, a 1- to 5-error-file:tidyout.log L injection in which each compound of interest is in the 20- 200-ng range or, when split in the injection port, is in that range. For selected ion monitoring gas chromatography/mass spectrometry, 1.5 error-file:tidyout.log L in which each compound of interest is in the 100- to 500-pg range; in some cases, down to 0.5 pg. For liquid chromatography/mass spectrometry and mass spectrometry/mass spectrometry, sample sizes are 20 to 500 ng per compound of interest and 10 to 500 ng per compound of interest, respectively.

- Preparation: Samples should be prepared to conform to the sample size restrictions given above

Limitations

- Compound(s) must be ionizable

- Detection limit is from 5 to 20 ng, depending on the compound. In selected ion monitoring gas chromatography/mass spectrometry, the detection limit can be as low as 0.5 pg

Estimated Analysis Time

- When analyzing one compound, direct introduction of sample takes 10-20 min per analysis. For gas chromatography/mass spectrometry, analysis of 1 to 2 compounds takes approximately 15 min, while analysis of 20 or more compounds takes 180 min or more

- Analysis and interpretation of data: Variable (15 min to days depending on the number of compounds analyzed)

Capabilities of Related Techniques

- Gas chromatography/Fourier-transform infrared spectroscopy: Functional group analysis, but at least an order of magnitude less sensitive

- Nuclear magnetic resonance: Only single compounds and at least two orders of magnitude less sensitive

- Secondary ion mass spectroscopy: A mass spectrometry method for looking only at surfaces of materials


Reprinted with permission of ASM International®.

 

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