聚苯乙烯—甲基丙烯醛缩氨基硫脲固相萃取填料的制备及其对重金属离子吸附性能的研究
发布时间：2018-07-25 08:26
【摘要】：本文以苯乙烯和甲基丙烯醛为原料,聚乙烯吡咯烷酮为分散剂,偶氮二异丁腈为引发剂,采用悬浮聚合法合成聚合物,再将氨基硫脲接枝到聚合物上,制备聚苯乙烯-甲基丙烯醛缩氨基硫脲固相萃取填料。采用红外光谱、扫描电子显微镜、X光电子能谱和有机元素分析等仪器对其结构、形貌及元素组成进行分析。以该固相萃取填料制成固相萃取小柱,与原子吸收光谱联用,对水中Ag+、Pb2+、Mn2+、Cu2+、Cd2+、Fe2+、Hg2+、Ni2+、Co2+、Cr3+10种金属离子进行吸附实验,吸附容量分别为12.21 mg/g、11.42 mg/g、7.20 mg/g、12.42 mg/g、10.07 mg/g、9.28 mg/g、11.78 mg/g、7.34 mg/g、9.64 mg/g和10.42 mg/g。考察了洗脱液种类,过柱流速和溶液pH值对萃取回收率的影响。当洗脱液为10 mL 5 mol/L HNO3和0.25 mL三乙醇胺混合液,过柱流速为0.5 mL/min,溶液pH值为5时,自制固相萃取小柱对Ag+、Pb2+、Mn2+、Cu2+、Cd2+、Fe2+、Hg2+、Ni2+、Co2+、Cr3+的回收率分别为98.94%、97.80%、92.17%、99.80%、96.36%、94.59%、98.24%、93.23%、95.35%、96.98%。通过实验测得小柱的穿透体积为120 mL。在0.1 mg/L-20.0mg/L范围内,Ag+、Pb2+、Mn2+、Cu2+、Cd2+、Fe2+、Hg2+、Ni2+、Co2+、Cr3+的原子吸收吸光度与浓度呈现良好的线性关系,相关系数分别为0.9993、0.9997、0.9965、0.9982、0.9990、0.9994、0.9987、0.9999、0.9995和0.9987。原子吸收法测定水中Ag+、Pb2+、Mn2+、Cu2+、Cd2+、Fe2+、Hg2+、Ni2+、Co2+、Cr3+的最低检出限分别为1.080μg/L、3.341μg/L、2.543μg/L、1.152μg/L、3.052μg/L、3.235μg/L、4.256μg/L、2.481μg/L、2.324μg/L和3.168μg/L,相对标准偏差(n=20)分别为6.42%、6.87%、9.64%、7.52%、10.08%、8.67%、6.53%、8.91%、7.23%和10.04%。
[Abstract]:The polymer was synthesized by suspension polymerization with styrene and methacrolein as raw materials, polyvinylpyrrolidone as dispersant and azodiisobutyronitrile as initiator, and then the thiosemicarbazone was grafted onto the polymer. Polystyrene-methacrolein thiosemicarbazone solid-phase extraction filler was prepared. The structure, morphology and composition of organic elements were analyzed by means of infrared spectroscopy, scanning electron microscope and X-ray photoelectron spectroscopy. The solid phase extraction (SPE) column was prepared with this solid phase extraction filler. The adsorption experiments were carried out on 10 kinds of metal ions in water by AAS. The adsorption capacity was 12.21 mg / g ~ (11.42) mg / g ~ (12.42) mg / g ~ (12) mg / g ~ (9.28) mg / g ~ (11.78) mg / g ~ (7.34) mg / r ~ (9.64) mg/g and 10.42 mg / g ~ (-1 / g) respectively. The effects of eluent type, flow rate and pH value on extraction recovery were investigated. When the eluent was mixed with 10 mL 5 mol/L HNO3 and 0.25 mL triethanolamine, the flow rate was 0.5 mL / min and the pH value of the solution was 5 mL, the recoveries of self-made solid phase extraction column were 98.9497.80 / 92.1799.80 ~ (99.80) ~ 94.5998.2493.23 ~ 95.23 ~ 95.35 ~ (th) and 95.9896.9896.9896.98 respectively for Ag ~ (2 +) Pb _ (2) O _ (2) C _ (2) C _ (2) C _ (2) C _ (2) C _ (2) H _ (2) H _ (2) H _ (2) C _ (2) C _ (2) C _ (2) C _ (2) C _ (3) C _ (3), respectively. The experimental results show that the penetrating volume of the column is 120 mL. In the range of 0.1 mg/L-20.0mg/L, there is a good linear relationship between the atomic absorption absorbance and the concentration of Ag, Pb, Pb2, Mn2, Cu2, CD2, Fe2, Hg2, Ni2, Co2, Cr3. The correlation coefficients are 0.9993, 0.99975, 0.9982n 0.99990, 0.99944, 0.9987U, 0.99995, and 0.99877.The correlation coefficients are 0.9993, 0.99975 and 0.9987, respectively. 鍘熷瓙鍚告敹娉曟祴瀹氭按涓瑼g ,Pb2 ,Mn2 ,Cu2 ,Cd2 ,Fe2 ,Hg2 ,Ni2 ,Co2 ,Cr3 鐨勬渶浣庢鍑洪檺鍒嗗埆涓，
本文编号：2143218
[Abstract]:The polymer was synthesized by suspension polymerization with styrene and methacrolein as raw materials, polyvinylpyrrolidone as dispersant and azodiisobutyronitrile as initiator, and then the thiosemicarbazone was grafted onto the polymer. Polystyrene-methacrolein thiosemicarbazone solid-phase extraction filler was prepared. The structure, morphology and composition of organic elements were analyzed by means of infrared spectroscopy, scanning electron microscope and X-ray photoelectron spectroscopy. The solid phase extraction (SPE) column was prepared with this solid phase extraction filler. The adsorption experiments were carried out on 10 kinds of metal ions in water by AAS. The adsorption capacity was 12.21 mg / g ~ (11.42) mg / g ~ (12.42) mg / g ~ (12) mg / g ~ (9.28) mg / g ~ (11.78) mg / g ~ (7.34) mg / r ~ (9.64) mg/g and 10.42 mg / g ~ (-1 / g) respectively. The effects of eluent type, flow rate and pH value on extraction recovery were investigated. When the eluent was mixed with 10 mL 5 mol/L HNO3 and 0.25 mL triethanolamine, the flow rate was 0.5 mL / min and the pH value of the solution was 5 mL, the recoveries of self-made solid phase extraction column were 98.9497.80 / 92.1799.80 ~ (99.80) ~ 94.5998.2493.23 ~ 95.23 ~ 95.35 ~ (th) and 95.9896.9896.9896.98 respectively for Ag ~ (2 +) Pb _ (2) O _ (2) C _ (2) C _ (2) C _ (2) C _ (2) C _ (2) H _ (2) H _ (2) H _ (2) C _ (2) C _ (2) C _ (2) C _ (2) C _ (3) C _ (3), respectively. The experimental results show that the penetrating volume of the column is 120 mL. In the range of 0.1 mg/L-20.0mg/L, there is a good linear relationship between the atomic absorption absorbance and the concentration of Ag, Pb, Pb2, Mn2, Cu2, CD2, Fe2, Hg2, Ni2, Co2, Cr3. The correlation coefficients are 0.9993, 0.99975, 0.9982n 0.99990, 0.99944, 0.9987U, 0.99995, and 0.99877.The correlation coefficients are 0.9993, 0.99975 and 0.9987, respectively. 鍘熷瓙鍚告敹娉曟祴瀹氭按涓瑼g ,Pb2 ,Mn2 ,Cu2 ,Cd2 ,Fe2 ,Hg2 ,Ni2 ,Co2 ,Cr3 鐨勬渶浣庢鍑洪檺鍒嗗埆涓，
本文编号：2143218
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