阴离子表面活性剂LAS在碳纳米管上的吸附及其应用
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摘要
目前碳纳米管(CNTs)作为吸附剂已经应用于有机和无机污染物的去除,并且可作为固相萃取(sPE)填料用于预富集中,将CNTs作为SPE吸附剂用作富集环境样品中痕量有机污染物和金属离子的研究较多。经过氧化处理后的CNTs表面被引入氧化官能团,同时其自身的比表面积和吸附能力会显著增加。氧化改性的羧基化多壁碳纳米管(CMMWCNTs)具有一定的亲水性,而且表面带负电荷,已用于预富集痕量金属离子。但尚无有关CMMWCNTs作为吸附剂富集烷基苯磺酸盐(LAS)的研究,为此,本研究主要开展了以下三方面的工作:
1、探讨用CMMWCNTs作为SPE吸附剂结合液相色谱分离用于水相样品中LAS的预富集方法;
2、探讨用离子对试剂对目标物进行改性,用CNTs做SPE吸附剂,建立离子对同相萃取液相色谱联用方法分析水中LAS的方法;
3、探讨了CNTs吸附LAS的特性及溶液水化学特性对CNTs吸附LAS的影响。
通过实验研究,得到以下主要结果:
1、用CMMWCNTs作为固相萃取吸附剂,实验分别考察并优化了固相萃取中洗脱液种类和体积、样品溶液的pH值、流速、超声时间和离子强度以及样品溶液的体积等因素,结果表明,该方法测定LAS同系物的检测限为0.02-0.03μg·L~(-1),标准偏差(RSD,n=6)在2.04-10.03%之间;LAS同系物在实际加标水样中的回收率为84.8-106.1%,同时实验对比了羧基化碳纳米管固相萃取柱和商品化C_8和C_(18)的固相萃取柱对LAS的富集效率,结果显示碳纳米管对目标物的保留能力要强于C_8和C_(18)。将本法应刚于水样中LAS同系物的分析,获得满意结果。
2、建立了以多壁碳纳米管(MWCNTs)为吸附剂的离子对固相萃取法与液相色谱联用测定水样中烷基苯磺酸盐的分析新方法,并探讨了离子对试剂的种类和浓度、样品溶液的超声时间、样品溶液的pH值、洗脱剂种类和体积、样品溶液的流速、样品体积对样品回收率的影响,获得了最佳的离子对试剂固相萃取条件:四丁基氢氧化铵(TBAH)作离子对试剂、TBAH与LAS摩尔比为1000、样品溶液超声处理3 min、pH为5、样品溶液流速在6 mL·min~(-1)、6mL甲醇洗脱样品。结果显示对于LAS同系物,该方法的标准偏差(RSD,n=6)为1.55-2.54%,检出限为0.033-0.126μg·L~(-1)。
3、研究了CMMWCNTs吸附LAS的动力学和吸附等温线。实验结果发现25℃的等温线与表面活性剂自组装体系中五区域等温线相似,而60℃的吸附等温线更像四区域吸附等温线。研究了溶液水化学对吸附的影响,包括不同阳离子(氯化钠、氯化钙和氯化镁)及无机阴离子、腐殖酸等;此外,还研究了超声时间对碳纳米管吸附效果的影响,结果表明,阴阳离子对吸附的影响与离子电荷相关,温度对吸附效果的影响较大,样品超声时间的影响相对较小。腐殖酸对吸附的影响受其浓度及来源的控制。
Carbon nanotubes(CNTs) as adsorbents have been used for removal of inorganic and organic pollutants,and also used as solid phase adsorbents for preconcentration of target analytes.Recently, CNTs as SPE(solid-phase extraction) adsorbents were used for enrichment of organic compounds and metal ions at trace levels.After oxidation process,CNTs can be introduced oxygen-containing functional groups on their surface.The surface area and sorption capacities are also remarkably increased and the modified CNTs have been used for preconcentration of metal ions at trace levels due to hydrophilic and negatively charged surface.However,there is no report on the application of oxidized CNTs as adsorbent to extract LAS from environmental waters.Thus,the present study will focus on the following three aspects:
1.Expoloring the possibility of using the CMMWCNTs as adsorbents combined with HPLC for LAS;,
2.Expoloring the possibility of using MWCNT as the adsorbent for LAS based on the ion-pair solid phase extraction system combined with high performance liquid chromatography(HPLC);
3.Expoloring the adsorption characteristics of LAS on CNTs and solution chemistry effects on LAS adsorption on CNTs.
The majr conclusions were as follows:
1,The effect of eluent and its volume,sample pH and flow rate,sample volume and the ultrasonic time of sample,the content of the electrolyte(NaCl) were investigated and optimized in detail.The detection limits of LAS homologues were 0.02-0.03μg L-1 with RSD(n=6) ranging from 2.04 to 10.03%.The recoveries of LAS homologues in the spiked environmental water samples ranged from 84.8 to 106.1%.Also,enrichment capability and recoveries of LAS in different water samples were also compared with commercial C8 and C18 SPE cartridge.The results indicated that CMMWCNTs cartridge showed stronger retention ability than C8 and C 18. The proposed method has been applied successfully to the analysis of LAS in aqueous environmental samples,which demonstrates that CMMWCNTs based solid-phase extraction is a precision and conveniently enrichmental method.
2,A new method was developed for the determination of LAS in water samples by using MWCNT as the adsorbent of the ion-pair solid phase extraction system combined with high performance liquid chromatography(HPLC).The factors affecting enrichment efficiency such as the kind and concentration of the ion-pair reagent,the sonication time of sample,the sample pH, the kind and volume of the eluent,the flow rate of sample,and the volume of sample were investigated.And the optimal SPE conditions were shown as follows:the molar ratio of TBAH/LAS was 1000,sonication time was 3 min,sample pH value was 5,the flow rate was 6 ml/min,and eluent was 6 ml methanol.It indicated from the experimental results that relative standard deviation(RSD) for four LAS homologues were 1.55-2.54,the detection limit was 0.033-0.126μg·L~(-1),respectively.The propose method was applied to determine LAS in tap water and Jialingjiang River water.
3,The 25℃-adsorption isotherm displayed a five-region mode,and the 60℃-adsorption isotherm is similar to four-region adsorption isotherm.The effect of solution chemistry including different cations,anionics and humic acid,on LAS adsorption on CNTs were studied,also effect of ultrasonic treatment time was considered.The results show that effect of ions was related to their charges.Temperature plays an important role,whereas the ultrasonic treatment time shows minor effect.The effect of humic acid is determined by its concentration and its source.
1、探讨用CMMWCNTs作为SPE吸附剂结合液相色谱分离用于水相样品中LAS的预富集方法;
2、探讨用离子对试剂对目标物进行改性,用CNTs做SPE吸附剂,建立离子对同相萃取液相色谱联用方法分析水中LAS的方法;
3、探讨了CNTs吸附LAS的特性及溶液水化学特性对CNTs吸附LAS的影响。
通过实验研究,得到以下主要结果:
1、用CMMWCNTs作为固相萃取吸附剂,实验分别考察并优化了固相萃取中洗脱液种类和体积、样品溶液的pH值、流速、超声时间和离子强度以及样品溶液的体积等因素,结果表明,该方法测定LAS同系物的检测限为0.02-0.03μg·L~(-1),标准偏差(RSD,n=6)在2.04-10.03%之间;LAS同系物在实际加标水样中的回收率为84.8-106.1%,同时实验对比了羧基化碳纳米管固相萃取柱和商品化C_8和C_(18)的固相萃取柱对LAS的富集效率,结果显示碳纳米管对目标物的保留能力要强于C_8和C_(18)。将本法应刚于水样中LAS同系物的分析,获得满意结果。
2、建立了以多壁碳纳米管(MWCNTs)为吸附剂的离子对固相萃取法与液相色谱联用测定水样中烷基苯磺酸盐的分析新方法,并探讨了离子对试剂的种类和浓度、样品溶液的超声时间、样品溶液的pH值、洗脱剂种类和体积、样品溶液的流速、样品体积对样品回收率的影响,获得了最佳的离子对试剂固相萃取条件:四丁基氢氧化铵(TBAH)作离子对试剂、TBAH与LAS摩尔比为1000、样品溶液超声处理3 min、pH为5、样品溶液流速在6 mL·min~(-1)、6mL甲醇洗脱样品。结果显示对于LAS同系物,该方法的标准偏差(RSD,n=6)为1.55-2.54%,检出限为0.033-0.126μg·L~(-1)。
3、研究了CMMWCNTs吸附LAS的动力学和吸附等温线。实验结果发现25℃的等温线与表面活性剂自组装体系中五区域等温线相似,而60℃的吸附等温线更像四区域吸附等温线。研究了溶液水化学对吸附的影响,包括不同阳离子(氯化钠、氯化钙和氯化镁)及无机阴离子、腐殖酸等;此外,还研究了超声时间对碳纳米管吸附效果的影响,结果表明,阴阳离子对吸附的影响与离子电荷相关,温度对吸附效果的影响较大,样品超声时间的影响相对较小。腐殖酸对吸附的影响受其浓度及来源的控制。
Carbon nanotubes(CNTs) as adsorbents have been used for removal of inorganic and organic pollutants,and also used as solid phase adsorbents for preconcentration of target analytes.Recently, CNTs as SPE(solid-phase extraction) adsorbents were used for enrichment of organic compounds and metal ions at trace levels.After oxidation process,CNTs can be introduced oxygen-containing functional groups on their surface.The surface area and sorption capacities are also remarkably increased and the modified CNTs have been used for preconcentration of metal ions at trace levels due to hydrophilic and negatively charged surface.However,there is no report on the application of oxidized CNTs as adsorbent to extract LAS from environmental waters.Thus,the present study will focus on the following three aspects:
1.Expoloring the possibility of using the CMMWCNTs as adsorbents combined with HPLC for LAS;,
2.Expoloring the possibility of using MWCNT as the adsorbent for LAS based on the ion-pair solid phase extraction system combined with high performance liquid chromatography(HPLC);
3.Expoloring the adsorption characteristics of LAS on CNTs and solution chemistry effects on LAS adsorption on CNTs.
The majr conclusions were as follows:
1,The effect of eluent and its volume,sample pH and flow rate,sample volume and the ultrasonic time of sample,the content of the electrolyte(NaCl) were investigated and optimized in detail.The detection limits of LAS homologues were 0.02-0.03μg L-1 with RSD(n=6) ranging from 2.04 to 10.03%.The recoveries of LAS homologues in the spiked environmental water samples ranged from 84.8 to 106.1%.Also,enrichment capability and recoveries of LAS in different water samples were also compared with commercial C8 and C18 SPE cartridge.The results indicated that CMMWCNTs cartridge showed stronger retention ability than C8 and C 18. The proposed method has been applied successfully to the analysis of LAS in aqueous environmental samples,which demonstrates that CMMWCNTs based solid-phase extraction is a precision and conveniently enrichmental method.
2,A new method was developed for the determination of LAS in water samples by using MWCNT as the adsorbent of the ion-pair solid phase extraction system combined with high performance liquid chromatography(HPLC).The factors affecting enrichment efficiency such as the kind and concentration of the ion-pair reagent,the sonication time of sample,the sample pH, the kind and volume of the eluent,the flow rate of sample,and the volume of sample were investigated.And the optimal SPE conditions were shown as follows:the molar ratio of TBAH/LAS was 1000,sonication time was 3 min,sample pH value was 5,the flow rate was 6 ml/min,and eluent was 6 ml methanol.It indicated from the experimental results that relative standard deviation(RSD) for four LAS homologues were 1.55-2.54,the detection limit was 0.033-0.126μg·L~(-1),respectively.The propose method was applied to determine LAS in tap water and Jialingjiang River water.
3,The 25℃-adsorption isotherm displayed a five-region mode,and the 60℃-adsorption isotherm is similar to four-region adsorption isotherm.The effect of solution chemistry including different cations,anionics and humic acid,on LAS adsorption on CNTs were studied,also effect of ultrasonic treatment time was considered.The results show that effect of ions was related to their charges.Temperature plays an important role,whereas the ultrasonic treatment time shows minor effect.The effect of humic acid is determined by its concentration and its source.
引文
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