本文選題：改性納米二氧化硅 + 吸附性能��； 參考：《湘潭大學(xué)》2015年碩士論文

【摘要】：由于納米二氧化硅的化學(xué)活性好、表面積大、吸附容量高,在化學(xué)、力學(xué)和生物學(xué)等方面顯示出很高的活性而被廣泛關(guān)注,在分析檢測(cè)中常被用作固相萃取劑。但是,在酸性條件下,納米二氧化硅容易凝聚成團(tuán)和失去活性。為了克服這個(gè)問(wèn)題,本實(shí)驗(yàn)用3-氨丙基三乙氧基硅烷對(duì)納米二氧化硅進(jìn)行化學(xué)修飾,用改性后的納米二氧化硅作為分離富集材料,以原子吸收光譜法為檢測(cè)手段,對(duì)藥品酒石酸唑吡坦和環(huán)境水樣中的鈀進(jìn)行預(yù)富集與測(cè)定,由此建立了簡(jiǎn)便、高效、選擇性好、靈敏度高、結(jié)果準(zhǔn)確的檢測(cè)痕量鈀的新方法。本文的主要研究?jī)?nèi)容如下:1.全面綜述了測(cè)定痕量金屬元素的意義及方法,對(duì)常用的分離富集方法、吸附材料做了簡(jiǎn)要介紹,重點(diǎn)對(duì)納米二氧化硅的特性、應(yīng)用以及制備方法進(jìn)行了較為詳細(xì)的敘述。2.采用溶膠—凝膠法制備了納米二氧化硅,再用3-氨丙基三乙氧基硅烷對(duì)納米二氧化硅進(jìn)行化學(xué)修飾,并運(yùn)用掃描電鏡,紅外光譜,X-射線衍射對(duì)其修飾前后進(jìn)行表征。以火焰原子吸收光譜法為檢測(cè)手段,系統(tǒng)研究了在靜態(tài)條件下改性納米SiO2對(duì)痕量鈀的吸附性能,探討了鈀在改性納米SiO2上的最佳吸附條件和飽和吸附容量。該法應(yīng)用于地質(zhì)標(biāo)準(zhǔn)參考物質(zhì)(批號(hào)為GBW07291)中鈀的測(cè)定,實(shí)驗(yàn)證明此方法具有準(zhǔn)確,靈敏,簡(jiǎn)便的特點(diǎn)。3.研究了改性納米二氧化硅在動(dòng)態(tài)條件下對(duì)痕量鈀的吸附性能,并結(jié)合石墨爐原子吸收光譜法測(cè)定酒石酸唑吡坦中痕量鈀。實(shí)驗(yàn)優(yōu)化了具體檢測(cè)條件,并對(duì)方法進(jìn)行了方法學(xué)驗(yàn)證。該方法測(cè)定痕量鈀的線性范圍為0.00~400.0 ng/mL,相關(guān)系數(shù)為0.9992,方法的檢出限為1.48 ng/mL,方法回收率在96.4%~101.4%之間,鈀對(duì)照品溶液(100 ng/mL)的RSD為2.6%(n=7)。該方法操作簡(jiǎn)便、迅速,具有良好的精密度和準(zhǔn)確度,可用于酒石酸唑吡坦中痕量鈀的測(cè)定。4.自制PTFE微柱,將改性納米二氧化硅作為固定相填充在其中,接入到在線流動(dòng)注射的程序中,將流動(dòng)注射技術(shù)與原子吸收光譜儀聯(lián)用,系統(tǒng)研究了在線條件下改性納米二氧化硅對(duì)痕量鈀的吸附性能。方法的線性范圍為5~500μg/L;相關(guān)系數(shù)為0.9987;檢測(cè)限是0.248μg/L;采樣體積為7.5 mL/次;測(cè)定100μg/L Pd(II)溶液RSD(n=7)為1.8%;流動(dòng)注射分析的富集因子為45,采樣頻率(f)為12/h。該方法應(yīng)用于不同環(huán)境水樣中痕量鈀的測(cè)定,結(jié)果滿意。
[Abstract]:Because of its good chemical activity, large surface area and high adsorption capacity, nano-silica has been widely concerned because of its high activity in chemistry, mechanics and biology, and is often used as solid phase extraction agent in analysis and detection. However, under acidic conditions, nano silica is easy to agglomerate and lose activity. In order to overcome this problem, 3-aminopropyl triethoxy silane was used to chemically modify the nano-silica. The modified nano-silica was used as the separation and enrichment material, and the atomic absorption spectrometry was used as the detection method. A new method for the determination of trace palladium in zolpidem tartrate and environmental water was established. The method is simple, efficient, selective, sensitive and accurate. The main contents of this paper are as follows: 1. The significance and method of determination of trace metal elements are summarized in this paper. The common separation and enrichment methods and adsorption materials are briefly introduced. The characteristics, applications and preparation methods of nano-silica are described in detail. Nano-silica was prepared by sol-gel method and then chemically modified with 3-aminopropyl triethoxysilane. It was characterized by scanning electron microscope (SEM) and X-ray diffraction (IR). The adsorption of trace palladium (PD) by modified nano SiO2 under static condition was studied by flame atomic absorption spectrometry (FAS). The optimum adsorption conditions and saturated adsorption capacity of PD on modified nano SiO2 were discussed. The method has been applied to the determination of palladium in the geological standard reference material (batch number GBW07291). The experimental results show that the method is accurate, sensitive and simple. The adsorption properties of modified nano-silica for trace palladium under dynamic conditions were studied and the trace palladium in zolpidem tartrate was determined by graphite furnace atomic absorption spectrometry. The test conditions were optimized and the method was validated. The linear range of the method for the determination of trace palladium is 0.004 400.0 ng / mL, the correlation coefficient is 0.9992, the detection limit of the method is 1.48 ng / mL, the recovery of the method is between 96.4% and 101.4%, and the RSD of the palladium reference solution is 2.6 ng / mL. The method is simple, rapid, with good precision and accuracy, and can be used for the determination of trace palladium in zolpidem tartrate. A self-made PTFE microcolumn filled with modified nano-silica as a stationary phase was inserted into the on-line flow injection program, and the flow injection technology was combined with atomic absorption spectrometer (AAS). The adsorption of trace palladium on-line modified nano silica was studied systematically. The linear range of the method is 5 渭 g / L; the correlation coefficient is 0.9987; the detection limit is 0.248 渭 g / L; the sampling volume is 7.5 mL/; the determination of 100 渭 g / L PD II solution is 1.8%; the enrichment factor of flow injection analysis is 45, the sampling frequency is 12% h. The method has been applied to the determination of trace palladium in different environmental water samples with satisfactory results.
【學(xué)位授予單位】：湘潭大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ127.2;TB383.1

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本文編號(hào)：1957216