Aldehydes are a kind of substances with strong irritant odor. They are often used as solvents or resin raw materials in adhesives. They are carcinogenic, teratogenic, irritating to skin and respiratory tract, and seriously harmful to human health. When adhesive is used in some products, especially in close contact with human body, such as interior decoration materials, toys, automobile interior parts, etc., its volatile aldehydes will continue to be released, which has a serious impact on human health. The detection of aldehydes in adhesives is mainly based on the determination of free formaldehyde content and the total amount of other aldehydes by spectrophotometry. Therefore, it is very necessary to establish a scientific and accurate method to detect the release of aldehydes in adhesives, in order to more truly and accurately explain the harm of adhesives to the environment and human health, which is conducive to the introduction of relevant standards and regulations to control the release of harmful substances from adhesives.
Cheng Yuxiao, senior engineer of Shanghai Customs industrial products and raw materials testing technology center, established an environmental climate box HPLC method to detect the release of 13 volatile aldehydes after the adhesive construction. The adhesive was coated on the substrate and placed in a climate box with constant temperature and humidity. 2,4-dinitrophenylhydrazine (DNPH) adsorption tube was used to sample from the sampling port of the climate box. Aldehydes reacted with DNPH to form stable phenylhydrazone derivatives, which were eluted and desorbed with acetonitrile and analyzed by liquid chromatography after constant volume. The base material, coating amount, sampling rate and liquid chromatography detection conditions were optimized to obtain the best conditions: 120 g adhesive sample was evenly coated on 0.4 M2 toughened glass plate, placed in the climate box for 24 hours, and then sampled for detection. The sampling flow rate was 2.0 ml / min, and the sampling amount was 24 L; kromasil kr100-5 C18 column (250 mm × 4.6 mm, 5 μ m). Acetonitrile water was used as mobile phase for gradient elution at a flow rate of 1.0ml/min. The column temperature was 40 ℃, and the detection wavelength was 360 nm.
The results show that 13 aldehydes have a good linear relationship (R ≥ 0.9977). The detection limit is 3.84-49.9 μ g / L according to the three times signal-to-noise ratio. When the gas sampling volume is 24 L and the constant volume is 10 ml, the detection limit converted into a climate box is 1.6-20.8 μ g / m3. The standard samples of aldehydes were added directly to DNPH adsorption tube to investigate the recovery of the method. The recovery was calculated after elution, constant volume and 5 parallel determinations by HPLC. The recovery of the method was 86.3% - 115%, and the relative standard deviation (RSD) was 3.5% - 8.6%. This method has a good accuracy and precision, and provides a new method for the detection of the release of aldehydes after the adhesive construction.
The research was supported by the national key research and development project (2016yff0203704) and the science and technology project of AQSIQ (2015ik229), and the relevant contents were published in the Journal of analysis and testing, 3 issues, 2020, page 396-400.
doi：10.3969/j.issn.1004-4957.2020.03.016
[cited in this paper]: Cheng Yuxiao, Gu Zhongyi, Zhao Bo, Guo Zhengyun, Jin Yinghua. Study on Simulation of environmental climate chamber release of volatile aldehydes in adhesives and detection method of high performance liquid chromatography [J]. Journal of analysis and test, 2020, 39 (3): 396-400
【Cite this article】：CHENG Yu-xiao, GU Zhong-yi, Zhao Bo, GUO Zheng-yun, JIN Ying-hua. Determination of Emission Quantity of Volatile Aldehydes in Adhesive by High Performance Liquid Chromatography with Environmental Chamber[J]. Journal of Instrumental Analysis, 2020, 39(3)：396-400.
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