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The increasing use of metal-based nanoparticle products has raised concerns in particular for the aquatic environment and thus the quantification of such nanomaterials released from products should be determined to assess their environmental risks. In this study, a simple, rapid and sensitive method for the determination of size and mass concentration of gold nanoparticles (AuNPs) in aqueous suspension was established by direct coupling of thin layer chromatography (TLC) with catalyzed luminol-H 2 O 2  chemiluminescence (CL) detection. For this purpose, a moving stage was constructed to scan the chemiluminescence signal from TLC separated AuNPs. The proposed TLC-CL method allows the quantification of differently sized AuNPs (13 nm, 41 nm and 100 nm) contained in a mixture. Various experimental parameters affecting the characterization of AuNPs, such as the concentration of H 2 O 2 , the concentration and pH of the luminol solution, and the size of the spectrometer aperture were investigated. Under optimal conditions, the detection limits for AuNP size fractions of 13 nm, 41 nm and 100 nm were 38.4 μg L −1 , 35.9 μg L −1  and 39.6 μg L −1 , with repeatabilities (RSD, n = 7) of 7.3%, 6.9% and 8.1% respectively for 10 mg L −1  samples. The proposed method was successfully applied to the characterization of AuNP size and concentration in aqueous test samples.

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Simultaneous Determination of Size and Quantification of Gold Nanoparticles by Direct Coupling Thin layer Chromatography with Catalyzed Luminol Chemiluminescence