Adsorption of small hydroxy acids on glass: a pitfall in quantitative urinary organic acid analysis by GC-MS

In IR spectroscopy of carboxylic acids, the C=O bond shows a characteristic band between 1710 and 1760 cm⁻¹, and the O–H bond exhibits a broad band between 2500 and 3300 cm⁻¹.
However, the stretching absorptions for the C=O bond vary depending on the structure of carboxylic acids. The C=O bond of the free carboxylic acids shows a higher stretching frequency, 1760 cm−1, while H-bonded carboxylic acids (dimers) exhibit stretching absorptions at a lower frequency, 1710 cm−1. The C=O bond of the...

In ¹H NMR spectroscopy, acidic protons (–COOH) of carboxylic acids are highly deshielded and absorb far downfield, at around 9–12 ppm. The chemical shift value depends on the concentration and solvent used.
While α protons of carboxylic acids absorb at 2–2.5 ppm, β protons absorb further upfield.
Carboxylic acids are easily identified by dissolving them in deuterium oxide, which results in a rapid exchange of the acidic protons with deuterium. This leads to the disappearance of the acidic...

Gas chromatography–mass spectrometry (GC–MS) is the combination of analytical techniques of gas chromatography and mass spectrometry in a single instrument for analyzing a mixture of compounds. The gas chromatograph separates the compounds in the mixture, and the mass spectrometer analyzes each compound separately to determine the molecular masses and molecular structures.
A gas chromatograph consists of a long, narrow capillary column with a polysiloxane coating on the inner wall. The coating...

Mass spectrometry is an important technique for the identification of pure compounds. However, it has some limitations for the analysis of complex mixtures, often due to excessive fragmentation making the spectrum too complicated to decipher. Mass spectrometry can be combined with suitable separation methods in sequence, forming hyphenated methods, which are useful in the analysis of complex mixtures.
GC–MS is a powerful hyphenated method commonly used in forensics and environmental...

In gravimetry, the precipitant is chosen carefully to obtain a pure solid that can be easily filtered. Common inorganic precipitants can be used to determine several cations and anions. In some cases, the formation of the same precipitate can be used to determine the cation and the anion. For example, the reaction of barium and chromate ions to give barium chromate is used to determine both barium and chromate. However, precipitates such as hydroxides, oxalates, and metal ammonium phosphates...

For AAS measurements, samples must be introduced as clear solutions, often requiring extensive preliminary treatment to dissolve materials like soils, animal tissues, and minerals. Common methods for sample preparation include treatment with hot mineral acids, wet ashing, combustion in closed containers, high-temperature ashing, or fusion with reagents.
 Solutions containing organic solvents, such as low-molecular-mass alcohols, esters, or ketones, enhance absorbances by increasing nebulizer...