皮革中重金屬元素檢測方法研究
發(fā)布時間：2019-03-28 15:58
【摘要】：皮革是人們生活中必備品,皮鞋、皮衣帽、手套、箱包、機動車內(nèi)飾等都是皮革制品。我國是皮革生產(chǎn)、制造和消費大國,在面臨經(jīng)濟快速高效發(fā)展的同時,皮革工業(yè)也面臨著一些問題。皮革中甲醛、五氯苯酚、重金屬含量超標問題尤為突出。針對皮革中重金屬檢測,本文采用了基于質(zhì)譜技術(shù)對皮革中重金屬檢測進行了研究,工作內(nèi)容如下：1、建立了一種快速、簡單、高效測定皮革中7種重金屬元素的方法——ICP-MS內(nèi)標法。微波消解法具有消解過程樣品需求量小、污染引入少、樣品損失較少、消解效果好效率高的特點；能夠滿足目前國內(nèi)和國際上關(guān)于皮革及皮革制品中重金屬含量檢測的要求：內(nèi)標的使用,極大地減小了皮革中復雜的基體對含量測定的影響,提高了方法的準確度。2、以ICP-MS基體匹配法為基本方法,建立了皮革中7種重金屬的快速檢測方法。采用半定量方法確定皮革樣品中的基體元素的種類及排除含量極低的元素,再采用外標法測試皮革中基體元素的準確含量,然后確定標準曲線的基體元素添加方案。按照基體元素添加方案,在內(nèi)標法的基礎(chǔ)上,在標準曲線內(nèi)加入基體物質(zhì),進行皮革中7種重金屬元素含量的測定。結(jié)果與其它幾種方法有偏差,不適合對皮革中樣品進行檢測3、以ICP-MS標準加入法為基本方法,建立了皮革中7種重金屬的快速檢測方法。采用微波消解法,較好的消解了皮革樣品。將同源的樣品消解液分別取出添加對應濃度的混合標準物質(zhì),可以作為種皮革中重金屬含量檢測的方法。4、以IDMS為基本方法,建立了皮革中6種重金屬的檢測方法�；谕凰叵♂屬|(zhì)譜法的基本原理和實驗流程方法,以最佳稀釋比公式計算最合適的稀釋劑溶液濃度、皮革樣品和稀釋劑的取樣量,在樣品前處理之前添加稀釋劑,并設(shè)計流程空白實驗。實驗過程中一旦皮革樣品和稀釋劑經(jīng)過消解達到同位素交換平衡,在后續(xù)的消解液轉(zhuǎn)移、稀釋的過程中即使有轉(zhuǎn)移操作失誤如遺失待測樣品等,也不會影響實驗的測量結(jié)果。6種重金屬元素的同位素稀釋質(zhì)譜法分為3次進行,較大的節(jié)約了實驗時間。與ICP-MS內(nèi)標法、ICP-MS基體匹配法、ICP-MS標準加入法相比,同位素稀釋質(zhì)譜法有著更高的準確度。
[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.
【學位授予單位】：北京化工大學
【學位級別】：碩士
【學位授予年份】：2016
【分類號】：TS57;O657.63
本文編號：2449017
[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.
【學位授予單位】：北京化工大學
【學位級別】：碩士
【學位授予年份】：2016
【分類號】：TS57;O657.63
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