CN103196855A - Method for measuring trace element lead in linden tree by flame atomic absorption spectrometry (FAAS) - Google Patents
Method for measuring trace element lead in linden tree by flame atomic absorption spectrometry (FAAS) Download PDFInfo
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Abstract
本发明公开了一种火焰原子吸收光谱测定椴树中铅含量的测定方法。样品的处理方法是:准确称取样品分次进行消化,消化液及洗涤液一并转移至50mL容量瓶中,用二次去离子水定容待测。按以下火焰原子吸收光谱条件测定样品吸光值:波长为270.0λ/nm;负高压389V;参比电流5mA;实际电流2.5mA;燃烧器高度8.6h/mm;光谱通带宽度0.5SBW/n;空气流量1.1L/min;乙炔流量1.1L/min。按回归曲线A=0.0286C+0.0034计算出样品的含量,本发明测定方法操作简单、快速、灵敏度高,同时也能测定一些其它中药材中微量元素铅的含量。The invention discloses a method for determining lead content in linden trees by flame atomic absorption spectrometry. The processing method of the sample is: accurately weigh the sample for digestion in stages, transfer the digestion solution and washing solution to a 50mL volumetric flask, and use secondary deionized water to make up the volume for testing. Determine the absorbance value of the sample according to the following flame atomic absorption spectrometry conditions: wavelength 270.0λ/nm; negative high voltage 389V; reference current 5mA; actual current 2.5mA; burner height 8.6h/mm; spectral passband width 0.5SBW/n; Air flow rate 1.1L/min; Acetylene flow rate 1.1L/min. The content of the sample is calculated according to the regression curve A=0.0286C+0.0034. The determination method of the present invention is simple, fast and sensitive, and can also determine the content of trace element lead in some other Chinese medicinal materials.
Description
技术领域 technical field
本发明涉及火焰原子吸收光谱测定椴树中微量元素铅含量的方法。 The invention relates to a method for determining the content of trace element lead in linden trees by flame atomic absorption spectrometry.
背景技术 Background technique
椴树蜜其性甘温,能增强体质改善情绪、降低中枢神经兴奋性、维护脑细胞功能。意气补胃、止疼解毒,有医治和减轻高血压、心脏病、便秘、失眠的多种疾病的功效。紫椴,又称籽椴、小叶椴、阿穆尔椴、椴树,为中国原产树种,在东北及华北地区山地均有野生分布。东北地区的长白山、小兴安岭等地的垂直分布可达海拔1100米以上。糠椴又叫大叶椴、辽椴、菩提树,大量分布在我国黑龙江和吉林两省林区。椴树蜜是蜜蜂从椴树花中采集的。呈白色、特浅琥珀色。气味芳香馥郁。味道甜润适口,较易结晶,结晶后为细腻洁白的油脂状,为一等蜜,群众称为特级蜜,深受国内外欢迎。它晶莹洁白、色纯味香,营养丰富,含葡萄糖和果酸70%以上,还有多种维生素和无机盐、有机酸酶,有促进人体生长和活力的生物素,能增进健康。它不仅是营养齐全的食品,还能治疗咳嗽、支气管炎,并作安眠镇静剂。 Linden honey is sweet and warm in nature, can enhance physical fitness, improve mood, reduce central nervous excitability, and maintain brain cell function. Qi nourishes the stomach, relieves pain and detoxifies, and has the effect of treating and alleviating various diseases such as high blood pressure, heart disease, constipation, and insomnia. Linden, also known as Tilia seed, Tilia small, Tilia Amur, Tilia, is a tree species native to China, and it is wildly distributed in the mountains of Northeast and North China. The vertical distribution of Changbai Mountain and Xiaoxing'an Mountains in Northeast China can reach an altitude of more than 1,100 meters. Tilia bran, also known as Tilia big-leaf, Tilia Liao, and Linden, are distributed in large numbers in the forest areas of Heilongjiang and Jilin provinces in my country. Linden honey is collected by bees from the flowers of the linden tree. White, very light amber. The smell is aromatic and fragrant. The taste is sweet and palatable, and it is easy to crystallize. After crystallization, it becomes fine and white oily, and it is a first-class honey. The masses call it super honey and is very popular at home and abroad. It is crystal clear and white, pure in color and fragrant, rich in nutrition, containing more than 70% of glucose and fruit acid, as well as multivitamins, inorganic salts, organic acid enzymes, biotin that promotes human growth and vitality, and can improve health. It is not only a nutritious food, but also can treat coughs, bronchitis, and act as a sleeping sedative.
微量元素与药理有关,微量元素是人体正常生活所必需物质,在机体组成及生理过程中有着十分重要的作用。如果人体微量元素含量异常将会引起多种疾病发生。本研究探索了测定椴树中元素钙的火焰原子吸收光谱法,为中药材中铅含量的测定提供一种方法。同时也为椴树和椴树蜜的进一步研究及开发利用提供科学依据。 Trace elements are related to pharmacology. Trace elements are essential substances for the normal life of the human body, and play a very important role in the composition of the body and physiological processes. If the content of trace elements in the human body is abnormal, it will cause a variety of diseases. This study explored the flame atomic absorption spectrometry for the determination of elemental calcium in linden tree, providing a method for the determination of lead content in traditional Chinese medicinal materials. At the same time, it also provides a scientific basis for the further research, development and utilization of linden and linden honey.
发明内容 Contents of the invention
本发明提供一种针对椴树中微量元素铅含量的测定方法,该方法主要过程为:1、样品处理;2、火焰原子吸收法最佳的工作条件;3、测定标准样品中铅的含量;4、绘出标准曲线并得出在一定浓度范围的标准曲线回归方程;5、测定样品;6、计算椴树样品中微量元素铅的含量。 The invention provides a method for determining the content of trace element lead in linden trees. The main process of the method is: 1. sample processing; 2. the best working conditions for flame atomic absorption method; 3. determining the content of lead in standard samples; 4. Draw the standard curve and draw the standard curve regression equation in a certain concentration range; 5. Measure the sample; 6. Calculate the content of the trace element lead in the linden tree sample.
本发明所述的椴树中微量元素铅的火焰原子吸收光谱方法,由以下步骤组成: The flame atomic absorption spectrometry method of trace element lead in lime tree of the present invention, is made up of following steps:
样品的处理: Sample handling:
准确称取样品,分次于小烧杯中,加入硝酸,浸泡过夜,次日在小烧杯上加上表面皿,加入硝酸,置于电热板上加热,使样品消化完全,加入一定量的高氯酸,消化至淡棕色气体冒尽,样液接近2mL左右,取下冷却,用二次去离子水冲洗小烧杯内壁和表面皿,样液及洗涤液一并转移至50mL容量瓶中,用二次去离子水定容,待测。 Accurately weigh the samples, divide them into small beakers, add nitric acid, soak overnight, add a watch glass to the small beaker the next day, add nitric acid, heat on an electric heating plate to completely digest the samples, add a certain amount of high chlorine acid, digest until the light brown gas exhausts, the sample liquid is close to about 2mL, remove and cool, rinse the inner wall of the small beaker and the watch glass with secondary deionized water, transfer the sample liquid and washing liquid to a 50mL volumetric flask, and use two Dilute to volume with deionized water, to be tested.
火焰原子吸收最佳的工作条件: The best working conditions for flame atomic absorption:
波长为270.0λ/nm;负高压389V;参比电流5mA;实际电流2.5mA;燃烧器高度8.6h/mm;空气流量1.1L/min;乙炔流量1.1L/min。 The wavelength is 270.0λ/nm; the negative high voltage is 389V; the reference current is 5mA; the actual current is 2.5mA; the burner height is 8.6h/mm; the air flow rate is 1.1L/min; the acetylene flow rate is 1.1L/min.
绘出标准曲线得出标准曲线回归方程: Draw the standard curve to get the standard curve regression equation:
将1000μg/mL的Pb标准贮备液稀释配制Pb质量浓度:0.0000、0.5000、1.0000、3.0000、5.0000、10.0000μg/mL,按原子吸收光谱测定条件,分别测定标准系列溶液的吸光值,根据测定结果绘出标准曲线并得出回归方程。微量元素铅含量C(μg/mL)的标准曲线回归方程A(吸光值)为A=0.0286C+0.0034,R2为0.9989铅含量的浓度线性范围为0.5000~10.0000μg/mL。 Dilute the 1000 μg/mL Pb standard stock solution to prepare the Pb mass concentration: 0.0000, 0.5000, 1.0000, 3.0000, 5.0000, 10.0000 μg/mL, measure the absorbance values of the standard series solutions respectively according to the measurement conditions of atomic absorption spectrometry, and draw Draw the standard curve and get the regression equation. The standard curve regression equation A (absorbance value) of trace element lead content C (μg/mL) is A=0.0286C+0.0034, and R2 is 0.9989. The concentration linear range of lead content is 0.5000~10.0000μg/mL.
样品的测定: Determination of samples:
按火焰原子吸收光谱测定条件测定出椴树样品的吸光值。 The absorbance value of the linden tree sample was determined according to the conditions of flame atomic absorption spectrometry.
计算椴树样品中微量元素铅含量: Calculation of trace element lead content in linden samples:
由测得的椴树样品的吸光值,根据回归曲线计算出样品椴树微量元素铅的含量。 From the measured absorbance value of the linden tree sample, the content of trace element lead in the sample linden tree was calculated according to the regression curve.
附图说明 Description of drawings
图1是吸光度(A)与铅含量(C)关系曲线。 Figure 1 is the relationship curve between absorbance (A) and lead content (C).
具体实施方式 Detailed ways
准确称取样品,分次于小烧杯中,加入硝酸,浸泡过夜,次日在小烧杯上加上表面皿,加入硝酸,置于电热板上加热,使样品消化完全,加入一定量的高氯酸,消化至淡棕色气体冒尽,样液接近2mL左右,取下冷却,用二次去离子水冲洗小烧杯内壁和表面皿,样液及洗涤液一并转移至50mL容量瓶中,用二次去离子水定容,待测。 Accurately weigh the samples, divide them into small beakers, add nitric acid, soak overnight, add a watch glass to the small beaker the next day, add nitric acid, heat on an electric heating plate to completely digest the samples, add a certain amount of high chlorine acid, digest until the light brown gas exhausts, the sample liquid is close to about 2mL, remove and cool, rinse the inner wall of the small beaker and the watch glass with secondary deionized water, transfer the sample liquid and washing liquid to a 50mL volumetric flask, and use two Dilute to volume with deionized water, to be tested.
火焰原子吸收最佳的工作条件: The best working conditions for flame atomic absorption:
波长为270.0λ/nm;负高压389V;参比电流5mA;实际电流2.5mA;燃烧器高度8.6h/mm;空气流量1.1L/min;乙炔流量1.1L/min。 The wavelength is 270.0λ/nm; the negative high voltage is 389V; the reference current is 5mA; the actual current is 2.5mA; the burner height is 8.6h/mm; the air flow rate is 1.1L/min; the acetylene flow rate is 1.1L/min.
标准曲线回归方程: Standard curve regression equation:
微量元素铅含量C(μg/mL)的标准曲线回归方程A(吸光值)为A=0.0286C+0.0034,R2为0.9989,铅含量的浓度线性范围为0.5000~10.0000μg/mL。 The standard curve regression equation A (absorbance value) of trace element lead content C (μg/mL) is A=0.0286C+0.0034, R2 is 0.9989, and the concentration linear range of lead content is 0.5000~10.0000 μg/mL.
样品的测定: Determination of samples:
按火焰原子吸收光谱测定条件测定出椴树样品的吸光值。 The absorbance value of the linden tree sample was determined according to the conditions of flame atomic absorption spectrometry.
计算椴树样品中微量元素铅含量: Calculation of trace element lead content in linden samples:
由测得的椴树样品吸光值,根据标准曲线回归方程计算出样品椴树微量元素铅的含量。 From the measured absorbance value of the linden tree sample, the content of trace element lead in the sample linden tree was calculated according to the standard curve regression equation.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103512854A (en) * | 2013-09-23 | 2014-01-15 | 桂林理工大学 | Flame atomic absorption spectrometry method for separating, enriching and detecting trace plumbum in water sample by utilizing thiobarbituric-acid-modified silica gel |
CN103528980A (en) * | 2013-09-23 | 2014-01-22 | 桂林理工大学 | Flame atomic absorption spectrum method for separating, enriching and determining trace lead and cadmium in water sample by using thiomalamic acid modified silica gel |
CN104713873A (en) * | 2013-12-11 | 2015-06-17 | 江南大学 | Trace lead spectrophotometric measuring method |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103512854A (en) * | 2013-09-23 | 2014-01-15 | 桂林理工大学 | Flame atomic absorption spectrometry method for separating, enriching and detecting trace plumbum in water sample by utilizing thiobarbituric-acid-modified silica gel |
CN103528980A (en) * | 2013-09-23 | 2014-01-22 | 桂林理工大学 | Flame atomic absorption spectrum method for separating, enriching and determining trace lead and cadmium in water sample by using thiomalamic acid modified silica gel |
CN103512854B (en) * | 2013-09-23 | 2015-06-17 | 桂林理工大学 | Flame atomic absorption spectrometry method for separating, enriching and detecting trace plumbum in water sample by utilizing thiobarbituric-acid-modified silica gel |
CN103528980B (en) * | 2013-09-23 | 2015-12-09 | 桂林理工大学 | Utilize the flame atomic absorption spectrometry method of trace lead, cadmium in thiomalic acid modified silica-gel separation and concentration-mensuration water sample |
CN104713873A (en) * | 2013-12-11 | 2015-06-17 | 江南大学 | Trace lead spectrophotometric measuring method |
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