【摘要】：本文以苯乙烯和甲基丙烯醛為原料,聚乙烯吡咯烷酮為分散劑,偶氮二異丁腈為引發(fā)劑,采用懸浮聚合法合成聚合物,再將氨基硫脲接枝到聚合物上,制備聚苯乙烯-甲基丙烯醛縮氨基硫脲固相萃取填料。采用紅外光譜、掃描電子顯微鏡、X光電子能譜和有機(jī)元素分析等儀器對(duì)其結(jié)構(gòu)、形貌及元素組成進(jìn)行分析。以該固相萃取填料制成固相萃取小柱,與原子吸收光譜聯(lián)用,對(duì)水中Ag+、Pb2+、Mn2+、Cu2+、Cd2+、Fe2+、Hg2+、Ni2+、Co2+、Cr3+10種金屬離子進(jìn)行吸附實(shí)驗(yàn),吸附容量分別為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�？疾炝讼疵撘悍N類,過柱流速和溶液pH值對(duì)萃取回收率的影響。當(dāng)洗脫液為10 mL 5 mol/L HNO3和0.25 mL三乙醇胺混合液,過柱流速為0.5 mL/min,溶液pH值為5時(shí),自制固相萃取小柱對(duì)Ag+、Pb2+、Mn2+、Cu2+、Cd2+、Fe2+、Hg2+、Ni2+、Co2+、Cr3+的回收率分別為98.94%、97.80%、92.17%、99.80%、96.36%、94.59%、98.24%、93.23%、95.35%、96.98%。通過實(shí)驗(yàn)測(cè)得小柱的穿透體積為120 mL。在0.1 mg/L-20.0mg/L范圍內(nèi),Ag+、Pb2+、Mn2+、Cu2+、Cd2+、Fe2+、Hg2+、Ni2+、Co2+、Cr3+的原子吸收吸光度與濃度呈現(xiàn)良好的線性關(guān)系,相關(guān)系數(shù)分別為0.9993、0.9997、0.9965、0.9982、0.9990、0.9994、0.9987、0.9999、0.9995和0.9987。原子吸收法測(cè)定水中Ag+、Pb2+、Mn2+、Cu2+、Cd2+、Fe2+、Hg2+、Ni2+、Co2+、Cr3+的最低檢出限分別為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,相對(duì)標(biāo)準(zhǔn)偏差(n=20)分別為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，

本文編號(hào)：2143218