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  • A novel miniaturized extraction capillary for determining gaseous formaldehyde by high-performance liquid chromatography.

A novel miniaturized extraction capillary for determining gaseous formaldehyde by high-performance liquid chromatography.

Analytical and bioanalytical chemistry (2014-09-10)
Ikuo Ueta, Suguru Mochizuki, Susumu Kawakubo, Tetsuo Kuwabara, Kiyokatsu Jinno, Yoshihiro Saito
ABSTRACT

A novel miniaturized sample extraction capillary was developed to provide a simple and sensitive method for analyzing gaseous formaldehyde (FA) using conventional high-performance liquid chromatography (HPLC). The extraction capillary was prepared by packing silica gel particles in a stainless steel capillary with a 1.6-mm o.d. Before the gaseous samples were collected, the silica gel particles were impregnated with a derivatizing reagent 2,4-dinitrophenylhydrazine (DNPH) by passing a solution of DNPH through the extraction capillary. FA was derivatized to form the corresponding hydrazone during the active sampling of a gaseous sample, and the derivative was sorbed by the silica gel. The capillary was then directly connected to a six-port valve, and desorption from the capillary and injection into the HPLC were achieved simultaneously by passing a solvent through the capillary. The run-to-run and device-to-device variabilities, as relative standard deviations, were both less than 6.9%. The limit of detection for FA was 2.5 ng/L using a sampling volume of 100 mL, and a sample collection time of 2 min. Acetaldehyde and acetone in a gaseous sample could also be simultaneously extracted and determined using this method. The applicability of the developed method for determining FA in real indoor air samples was confirmed by comparing the results obtained using the proposed method and a conventional sample preparation method. The developed method enables the rapid and simple sample preparation of gaseous FA and gives a good level of sensitivity.

MATERIALS
Product Number
Brand
Product Description

USP
Acetone, United States Pharmacopeia (USP) Reference Standard
Supelco
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Sigma-Aldrich
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Acetone, puriss., meets analytical specification of Ph. Eur., BP, NF, ≥99% (GC)
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Acetone, ACS reagent, ≥99.5%
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Acetone, suitable for HPLC, ≥99.9%
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Acetone, histological grade, ≥99.5%
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Hydrochloric acid, meets analytical specification of Ph. Eur., BP, NF, fuming, 36.5-38%
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Acetone, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%
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Acetone, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.5% (GC)
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Acetone, analytical standard
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Acetone, ≥99%, meets FCC analytical specifications
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Acetone, natural, ≥97%
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Formaldehyde-2,4-DNPH Solution, certified reference material, TraceCERT®, 100 μg/mL in acetonitrile (as aldehyde), ampule of 5 × 1 mL
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Formaldehyde-DNPH solution, certified reference material, TraceCERT®, 100 μg/mL in acetonitrile (as aldehyde), ampule of 1 mL
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Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
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Acetonitrile, suitable for HPLC-GC, ≥99.8% (GC)
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Acetonitrile, for HPLC, for UV, ≥99.9% (GC)
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USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
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Formaldehyde-2,4-DNPH, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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Hydrochloric acid solution, 32 wt. % in H2O, FCC
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