本文選題：流動注射分析 + 分光光度法　； 參考：《西南科技大學(xué)》2015年碩士論文

【摘要】：痕量元素分析在諸多領(lǐng)域如環(huán)境監(jiān)測、食品科學(xué)、現(xiàn)代醫(yī)藥學(xué)、生命科學(xué)、材料科學(xué)、地質(zhì)、化工等領(lǐng)域都有重要意義。元素銅、碘和鈷均為人體的必需微量元素,在人體內(nèi)起著至關(guān)重要的作用,關(guān)于其痕量級測定方法的研究也引起人們越來越高的重視。流動注射技術(shù)(FIA)這種新型的溶液連續(xù)處理技術(shù)始建于1975年。分光光度法是FIA最為經(jīng)典的聯(lián)用檢測手段。將兩者聯(lián)和后組成流動注射-分光光度法,利用此聯(lián)用技術(shù)進(jìn)行元素分析,既可避免了分光光度分析中繁瑣的手工操作,使其靈敏度提高的同時又可實現(xiàn)自動連續(xù)分析和現(xiàn)場監(jiān)測分析,且此方法對儀器要求較低、試劑也經(jīng)濟(jì)易得,適于推廣普及,非常適合我國國情,因此研究發(fā)展迅速。本研究中建立了3個元素的流動注射-分光光度法分析測定體系,并對其應(yīng)用進(jìn)行了探索。(1)流動注射-分光光度法檢測痕量銅在酸性介質(zhì)中,銅與1-(2-吡啶偶氮)-2-萘酚(PAN)在表面活性劑溴化十六烷基吡啶(CPB)的存在下迅速發(fā)生高靈敏顯色反應(yīng),據(jù)此建立了流動注射-分光光度法測定痕量銅的新方法。最佳分析條件經(jīng)優(yōu)化后確立為:顯色體系中PAN濃度為0.20 g·L-1,CPB濃度為5.6 g·L-1,加入醋酸-醋酸鈉緩沖溶液體積為8 m L/25 m L;主蠕動泵進(jìn)樣速度為8 m L·min-1,副蠕動泵進(jìn)樣速度為8m L·min-1,多通道采樣閥進(jìn)樣時間為20 s,反應(yīng)盤管長度為2.5 m。方法在Cu2+濃度10~180μg·L-1范圍內(nèi)與峰高呈線性關(guān)系(r=0.999),方法檢出限為1.05μg·L-1,精密度RSD=1.03%(n=11)。應(yīng)用于實際水樣中痕量銅的檢測,加標(biāo)回收率為97.8%~104.5%,呈現(xiàn)良好的重現(xiàn)性和準(zhǔn)確性,結(jié)果令人滿意。(2)流動注射-分光光度法檢測痕量碘在硫酸溶液介質(zhì)中,十六烷基三甲基溴化胺(CTMAB)存在與KI過量條件下,利用IO3-與過量I-生成I3-,染料乙基紫與I3-反應(yīng)生成藍(lán)綠色締合物。據(jù)此,以流動注射-分光光度法為檢測技術(shù),建立了測定痕量碘的新方法。最佳分析條件確定為:顯色體系中乙基紫濃度為8.0×10-5 mol·L-1,KI溶液濃度為10 g·L-1,CTMAB濃度為1.0×10-4mol·L-1,硫酸溶液濃度為0.10 mol·L-1;主蠕動泵進(jìn)樣速度為6 m L·min-1,副蠕動泵進(jìn)樣速度為8 m L·min-1,多通道采樣閥進(jìn)樣時間為15 s,反應(yīng)盤管長度為2.5 m。方法在IO3-濃度20~250μg·L-1范圍內(nèi)與峰高呈現(xiàn)的線性關(guān)系良好,線性方程為A=0.0024c+0.1441(r=0.9991)。方法檢出限為0.4μg·L-1,精密度為0.77%(n=11),經(jīng)抗干擾能力檢定,該方法具有較好的選擇性和重現(xiàn)性。將方法應(yīng)用于市場上幾類食鹽中的碘含量的測定,得加標(biāo)回收率為97.1%~102.4%,效果可觀。(3)流動注射-膠束增溶分光光度法檢測痕量鈷在硼砂緩沖溶液介質(zhì)及在表面活性劑溴化十六烷基吡啶(CPB)作用下,Co(Ⅱ)可與水楊基熒光酮(SAF)迅速發(fā)生絡(luò)合反應(yīng),據(jù)此將流動注射與膠束增溶分光光度法聯(lián)用建立了測定痕量Co(Ⅱ)的新方法。最佳分析條件選定為:顯色體系中SAF濃度為1.6×10-4 mol·L-1,CPB濃度為3.6 g·L-1,硼砂緩沖溶液體積為3 m L/25 m L;主蠕動泵進(jìn)樣速度為7 m L·min-1,副蠕動泵進(jìn)樣速度為1 m L·min-1,多通道采樣閥進(jìn)樣時間為15 s,反應(yīng)盤管長度為2 m。方法在Co2+濃度3~40μg·L-1范圍內(nèi)峰高與濃度成線性關(guān)系,線性方程A=0.006c+0.3693,相關(guān)系數(shù)r=0.9995,方法檢出限D(zhuǎn)L=0.1μg·L-1,精密度為0.95%(n=11)。應(yīng)用于檢測實際水樣中的痕量鈷,加標(biāo)回收率在97.0%~102.3%之間。
[Abstract]:Trace element analysis is of great significance in many fields, such as environmental monitoring, food science, modern medicine, life science, material science, geology, chemical industry and other fields. Element copper, iodine and cobalt are essential trace elements in human body, and play a vital role in human body. Higher attention. The flow injection technique (FIA), a new continuous solution treatment technology, was built in 1975. Spectrophotometric method is the most classical method for the detection of FIA. In order to improve the sensitivity and realize the automatic continuous analysis and field monitoring and analysis at the same time, this method has a low requirement for the instrument, and the reagent is also economical. It is suitable for popularization and popularization. It is very suitable for the national conditions of our country. Therefore, the research and development is rapid. In this study, 3 elements are established by flow injection spectrophotometry analysis and determination system. The application has been explored. (1) flow injection spectrophotometry is used to detect trace copper in acid medium, copper and 1- (2- pyridazo) -2- naphthol (PAN) are rapidly sensitive to color reaction in the presence of surfactant brominated sixteen alkyl pyridine (CPB). According to this, a new method for the determination of trace copper by flow injection spectrophotometry is established. The analysis conditions were optimized as follows: the concentration of PAN was 0.20 G. L-1, the concentration of CPB was 5.6 G. L-1, the volume of acetic acid sodium acetate buffer solution was 8 m L/25 m L, the injection speed of the main peristaltic pump was 8 m L. The method has a linear relationship with peak height in the range of Cu2+ concentration of 10~180 g / L-1. The detection limit is 1.05 mu g L-1 and precision RSD=1.03% (n=11). The detection of Trace Copper in actual water samples is applied to the detection of Trace Copper in actual water samples. The recovery rate is 97.8%~104.5%, and the results are satisfactory. (2) flow injection spectrophotometric detection marks In the medium of sulphuric acid solution, the presence of sixteen alkyl three methyl bromide (CTMAB) and the excess of KI, using IO3- and excess I- to produce I3-, and the reaction of dye ethyl violet and I3- to produce blue-green Association. In the color system, the concentration of ethyl violet is 8 * 10-5 mol. L-1, KI solution concentration is 10 g. L-1, CTMAB concentration is 1 x 10-4mol L-1, and the concentration of sulphuric acid solution is 0.10 mol L-1; the injection speed of the main peristaltic pump is 6 m L. The sampling speed of the auxiliary peristaltic pump is 8, and the sampling time of the multi-channel sampling valve is 15, and the reaction coil length is 2.5. The linear relationship between the peak height and the peak height in the range of IO3- concentration 20~250 g / L-1 is good, the linear equation is A=0.0024c+0.1441 (r=0.9991). The detection limit is 0.4 mu g. L-1 and the precision is 0.77% (n=11). The method has good selectivity and reproducibility. The method is applied to the iodine content of several kinds of salt in the market. The rate of recovery was 97.1%~102.4% and the result was significant. (3) flow injection micellar solubilization spectrophotometry was used to detect trace cobalt in borax buffer solution medium and surface active agent brominated sixteen alkyl pyridine (CPB), Co (II) could react with salicylfluorone (SAF) rapidly, according to which the flow injection and micelle solubilization was added. A new method for the determination of trace Co (II) was established by photometric method. The optimum analysis conditions are as follows: the concentration of SAF in the color system is 1.6 * 10-4 mol. L-1, CPB concentration is 3.6 g L-1, the volume of borax buffer solution is 3 m L/25 m L; the inlet velocity of the main peristaltic pump is 7 m. The inlet velocity of the auxiliary peristaltic pump is 1 The sample time was 15 s, and the reaction coil length of 2 M. was linear with the peak height and concentration in the Co2+ concentration of 3~40 mu g. L-1. The linear equation A=0.006c+0.3693, the correlation coefficient r=0.9995, the detection limit DL=0.1 micron G. L-1, the precision of 0.95% (n=11).
【學(xué)位授予單位】：西南科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：O657.3;X832

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 陳亞紅,樊靜,葉存玲,馮素玲;廢水中痕量酚的流動注射停流-催化光度法測定[J];分析化學(xué);2001年03期

2 張大倫,馬燕,余有平*;負(fù)催化動力學(xué)光度法測定微量碘的研究[J];分析科學(xué)學(xué)報;2001年02期

3 白林山,黎偉利;靛藍(lán)胭脂紅-溴酸鉀體系催化光度法測定微量碘[J];分析試驗室;2001年03期

4 季劍波;;微波消解-水楊基熒光酮光度法測定中草藥中痕量鍺[J];分析試驗室;2007年10期

5 譚愛民，周馳;流動注射分析[J];分析試驗室;1995年06期

6 劉華忠,陳小云,羅萍;微量元素銅的研究進(jìn)展[J];國外畜牧學(xué)(豬與禽);2000年01期

7 李昌厚;;略論流動注射分析及其發(fā)展[J];光學(xué)儀器;1990年01期

8 尚德;杜文勇;羅建民;;流動注射-分光光度法測定環(huán)境水樣中的硫化物[J];光譜實驗室;2013年01期

9 馮立明;雙波長分光光度法測定焦磷酸鹽仿金鍍液中的銅、鋅含量[J];化學(xué)分析計量;2001年05期

10 黃典文,葉雪芬;酸性絡(luò)藍(lán)K褪色光度法測定食鹽中微量碘[J];理化檢驗(化學(xué)分冊);2001年04期

，

本文編號：1910684