Analytical Techniques: Classical Wet Analytical Chemistry

Thomas R. Dulski, Carpenter Technology Corporation

General Use

- Quantitative elemental composition analysis

- Qualitative identification of material type

- Qualitative detection of component moieties

- “Umpire” check on quantitative instrumental methods

- Isolation and characterization of inclusions and phases

- Characterization of coatings and surfaces

- Determination of oxidation state

Examples of Applications

- Quantitative determination of alloy matrix elements for which instrumental methods are unavailable or unreliable

- Complete characterization of a homogeneous sample for use as an instrument calibration standard

- Quantitative determination of composition when sample is too small or of unsuitable shape for instrumental approaches

- Gross average composition determination of inhomogeneous samples

- Isolation of compounds and stoichiometric phases from metal alloy matrices for compositional analysis or examination by instrumental techniques

- Coating weight determination of plated metals, lubricant films, and other surface layers

- Partitioning of element oxidation states

- Sorting of mixed materials based on qualitative detection of one or more key matrix components

Samples

- Form: Crystalline or amorphous solids (metals, ceramics, glasses, ores, and so on) and liquids (pickling and plating bats, lubricants, and so on)

- Size: Depends on extent of required analyses—generally 1 to 2 g per element for solids and 20 mL total for process liquids, although requirements vary widely with technique

- Preparation: Solids are milled, drilled, crushed, or similarly dissociated into particles typically 2 mm (0.08 in.) in diameter or smaller. Machined alloys are solvent degreased. Materials lacking high order homogeneity require special care to ensure a representative laboratory sample

Limitations

- Slow compared to alternate instrumental techniques

- Except in rare cases, relatively large sample weights are required

Estimated Analysis Time

- 2 to 80 h per element (8 h per element is typical)

Capabilities of Related Techniques

- X-ray spectrometry: Rapid for major component elements with Z>9

- Optical emission spectroscopy: Can be rapid for minor and trace components

- Atomic absorption spectrophotometry: Somewhat more rapid; better ultimate detection limits for trace components

- Atomic absorption spectrophotometry: Somewhat more rapid; better ultimate detection limits for trace components


Reprinted with permission of ASM International®.

 

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