皮革中重金属元素检测方法研究

发布时间：2019-03-28 15:58

【摘要】：皮革是人们生活中必备品,皮鞋、皮衣帽、手套、箱包、机动车内饰等都是皮革制品。我国是皮革生产、制造和消费大国,在面临经济快速高效发展的同时,皮革工业也面临着一些问题。皮革中甲醛、五氯苯酚、重金属含量超标问题尤为突出。针对皮革中重金属检测,本文采用了基于质谱技术对皮革中重金属检测进行了研究,工作内容如下：1、建立了一种快速、简单、高效测定皮革中7种重金属元素的方法——ICP-MS内标法。微波消解法具有消解过程样品需求量小、污染引入少、样品损失较少、消解效果好效率高的特点；能够满足目前国内和国际上关于皮革及皮革制品中重金属含量检测的要求：内标的使用,极大地减小了皮革中复杂的基体对含量测定的影响,提高了方法的准确度。2、以ICP-MS基体匹配法为基本方法,建立了皮革中7种重金属的快速检测方法。采用半定量方法确定皮革样品中的基体元素的种类及排除含量极低的元素,再采用外标法测试皮革中基体元素的准确含量,然后确定标准曲线的基体元素添加方案。按照基体元素添加方案,在内标法的基础上,在标准曲线内加入基体物质,进行皮革中7种重金属元素含量的测定。结果与其它几种方法有偏差,不适合对皮革中样品进行检测3、以ICP-MS标准加入法为基本方法,建立了皮革中7种重金属的快速检测方法。采用微波消解法,较好的消解了皮革样品。将同源的样品消解液分别取出添加对应浓度的混合标准物质,可以作为种皮革中重金属含量检测的方法。4、以IDMS为基本方法,建立了皮革中6种重金属的检测方法。基于同位素稀释质谱法的基本原理和实验流程方法,以最佳稀释比公式计算最合适的稀释剂溶液浓度、皮革样品和稀释剂的取样量,在样品前处理之前添加稀释剂,并设计流程空白实验。实验过程中一旦皮革样品和稀释剂经过消解达到同位素交换平衡,在后续的消解液转移、稀释的过程中即使有转移操作失误如遗失待测样品等,也不会影响实验的测量结果。6种重金属元素的同位素稀释质谱法分为3次进行,较大的节约了实验时间。与ICP-MS内标法、ICP-MS基体匹配法、ICP-MS标准加入法相比,同位素稀释质谱法有着更高的准确度。
[Abstract]:Leather is necessary in people's life, leather shoes, leather clothes and hats, gloves, luggage, motor vehicle interior accessories are leather products. China is a big country in leather production, manufacture and consumption. With the rapid and efficient development of economy, leather industry also faces some problems. Formaldehyde, pentachlorophenol, heavy metal content in leather exceeded the standard problem is particularly prominent. For the detection of heavy metals in leather, this paper adopts mass spectrometry technology to study the detection of heavy metals in leather. The main contents are as follows: 1. A rapid and simple method has been established for the determination of heavy metals in leather. An efficient method for the determination of seven heavy metal elements in leather-ICP-MS internal standard method. Microwave digestion has the characteristics of small sample demand, less pollution introduction, less sample loss and better digestion effect and high efficiency. It can meet the current domestic and international requirements for the determination of heavy metals in leather and leather products: the use of internal standards greatly reduces the influence of complex matrix in leather on the determination of heavy metals, and improves the accuracy of the method. Based on ICP-MS matrix matching method, a rapid method for the determination of seven heavy metals in leather was established. A semi-quantitative method was used to determine the types of matrix elements in leather samples and to exclude the elements with very low content. Then the accurate content of matrix elements in leather was tested by external standard method and then the matrix element addition scheme of standard curve was determined. On the basis of internal standard method, the content of seven heavy metal elements in leather was determined by adding matrix substance to the standard curve according to the method of adding matrix elements. Results there was a deviation from other methods, which was not suitable for the detection of samples in leather. Based on the ICP-MS standard addition method, a rapid method for the determination of seven heavy metals in leather was established. The leather samples were digested by microwave digestion method. The sample digestion solution of the same origin was taken out with the corresponding concentration of mixed reference material, which can be used as a method for the determination of heavy metals in seed leather. 4. Taking IDMS as the basic method, the determination methods of six heavy metals in leather were established. Based on the basic principle of isotope dilution mass spectrometry and experimental flow method, the optimum dilution ratio formula was used to calculate the most suitable diluent concentration, sample volume of leather sample and diluent, and adding diluent before sample pretreatment. And design process blank experiment. During the experiment, once the leather sample and diluent reach isotope exchange equilibrium after digestion, even if there are transfer operation errors, such as loss of sample to be measured, etc., in the subsequent digestion solution transfer, dilution process, The isotope dilution mass spectrometry of six heavy metal elements is divided into three times, which saves the time of the experiment. Compared with ICP-MS internal standard method, ICP-MS matrix matching method and ICP-MS standard addition method, isotope dilution mass spectrometry has higher accuracy.
【学位授予单位】：北京化工大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：TS57;O657.63

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