Determination Of Deleterious Compounds In Adhesive By Chromatography

The propylene fiber adhesive is generated by vinyl acetate, acrylic esters, acrylic monomers copolymer or homopolymer, then added certain additives. As for the problem of raw materials and operation technics, monomer conversion is difficult to achieve100%. Therefore, the acrylic acid, methacrylic acid and their esters would be introduced into adhesive in the process of production. The acrylic acid, methacrylic acid and their esters can injure human respiratory, skin, eyes etc.. It also can poison liver organ, immune system and nervous system after long-term high concentration exposure, and some are identified as suspected carcinogens by IARC. Meanwhile, the nitrite is a toxic substance in the solvent of industrial water. Excess nitrite can cause methemoglobinemia and esophageal cancer. Therefor accurate and rapid analysis of them is very important. This paper studied the detection methods of these kinds of harmful substances, and the main jobs are in the following three aspects:1. A method for the determination of six kinds of acrylates and methyl acrylates residual monomers in adhesives by static headspace-gas chromatography-mass spectrometry was developed. Analytical conditions were established as follows by optimizing chromatographic and headspace conditions:The DB-WAX column was selected with a inlet temperature of250℃and split ratio of20:1. The temperature programe was designed as follows:initial column temperature of40℃and maintained for5min,40℃to200℃at the rate of25℃/min, holding for15min. Helium was carrier gas. Flow rate was1.0ml/min. Headspace equilibrium temperature was100℃, and kept for30min. The established method showed good separation and high sensitivity with a detection limit of0.0069～0.0096μg/mL and quantification limit of0.23～0.32mg/kg. The recovery rate was96.0%～104.6%. Good repeatability has been achived with a relative standard deviation below4.2%. Thus, this simple method can be applied to analyze the acrylates and methyl acrylates in adhesives rapidly and accurately.2. A method for the determination of nitrite in adhesives by ion chromatography was developed. The extraction was performed under the condition of Dionex IonPac AS11-HC and IonPac AG11-HC column at a temperature of30℃. The gradient elution program were conducted at a flow rate of1.0ml/min, using KOH-H2O as mobile phase. ASRS anion suppressor current was75mA. Under this optimum conditions, the established method showed good separation and high sensitivity with a detection limit of0.05mg/kg and quantification limit of0.16mg/kg. The recovery rates were in the range of92.0%to104.5%. The relative standard deviation was below3.6%. The method can be applied to rapidly analyze nitrite in adhesives.3. A method for the determination of acrylic acid and methacrylic acid in adhesives by high-performance liquid chromatography was developed. The extraction was performed under the condition of ZORBAX Eclipse XDB-C18column at a temperature of30℃. The gradient elution program were conducted at a flow rate of1.2ml/min, using CH3CN-H2O as mobile phase. Ultraviolet detector wavelength was210nm. Under this optimum conditions, the established method showed good separation and high sensitivity with a detection limit of0.1mg/kg and quantification limit of0.3mg/kg. The recovery rates were in the range of91.1%to102.9%. The relative standard deviation was below1.61%. The method can be applied to rapid analyze acrylic acid and methacrylic acid in adhesives.