ZIF-8吸附材料对雪菊中木犀草苷的富集及在微型近红外光谱分析中的应用EI北大核心CSCD

制备了SiO;@ZIF-8吸附剂并用于吸附雪菊中微量的木犀草苷,建立了基于特征变量筛选的微型近红外光谱分析方法。以木犀草苷为对象,研究了吸附剂的质量、pH、振荡时间对吸附效果的影响;在最佳条件下对富集了木犀草苷的吸附剂直接进行检测,探讨分别采用竞争自适应加权采样算法(CARS)、蒙特卡罗-无信息变量消除法(MC-UVE)和随机青蛙算法(RT)进行变量筛选,并用偏最小二乘法建立定量校正模型。研究发现,当吸附剂质量为0.20 g, pH 7时振荡20 min,木犀草苷吸附率可达到92%;经3种变量筛选后最优模型为CARS,CWT方法光谱预处理后,木犀草苷校正模型参考浓度和预测浓度两者之间的相关系数达到最佳的0.9700,预测回收率在85%~120%。SiO_(2)@ZIF-8吸附剂可以有效的富集雪菊中的木犀草苷,在CARS变量筛选下,通过微型近红外光谱可以实现雪菊中微量木犀草苷的测定。     

聚多巴胺包覆氨基硅球用于木犀草素的富集及检测

采用聚多巴胺包覆氨基硅球材料,作为吸附剂对木犀草素进行吸附与检测,建立了一种快速测定稀溶液中木犀草素的近红外光谱分析方法。在进行吸附试验的过程中,考察了质量、pH值和吸附时间对木犀草素吸附率的影响;不需要脱附,富集了木犀草素的吸附剂经近红外漫反射光谱直接检测,并以偏最小二乘回归法建立定量木犀草素校正模型进行含量的预测。研究显示,在中性条件下,常温吸附10 min,吸附剂质量为0.2 g,木犀草素的吸附率可达到93.8%;近红外光谱经过SNV+CWT处理后,木犀草素校正模型的参考浓度和预测浓度之间的相关系数为0.9811,在0.3-15.0 mg L~(-1)的较低浓度范围内,预测集的回收率可以达到86.6-118.8%。结果表明,可通过近红外漫反射光谱技术和吸附预富集相结合的方式对稀溶液中微量的木犀草素进行富集与灵敏检测。     

雪菊中木犀草苷的富集及近红外光谱分析方法

采用温和的方法制备了苯硼酸吸附剂,将其用于雪菊中微量木犀草苷的富集,并以此为基础建立了快速、选择性地测定雪菊中木犀草苷含量的近红外光谱分析方法。富集了木犀草苷的吸附剂无需脱附,即可用近红外漫反射光谱直接检测,通过偏最小二乘回归法建立了定量分析木犀草苷的校正模型,并成功实现了木犀草苷含量的测定。采用此苯硼酸吸附剂0.2 g,常温振荡吸附20 min后,吸附效率可达85.5%。结果表明,经连续小波变换处理近红外光谱分析数据,木犀草苷预测模型的预测浓度和参考浓度之间的相关系数为0.9765,且木犀草苷在0.15～19.5 mg/L浓度范围内具有较好的预测结果,预测回收率为84.7%～113.2%。本研究建立了苯硼酸吸附剂吸附预富集方法,与近红外漫反射光谱结合,实现了雪菊溶液中微量木犀草苷的选择性测定,为近红外光谱与吸附富集分析药食用植物中的其它有效成分的研究提供了参考。     

一种通过水光谱探究木犀草素浓度测定的新方法

采集了一定含水量、不同浓度的木犀草素溶液的近红外光谱,借助于多元分析方法研究了其谱峰变化,建立了一种基于不同浓度木犀草素对水光谱的扰动情况进行木犀草素检测的模型。通过比较不同光谱预处理方法,最终确定采用标准正态变换（SNV）法进行光谱预处理,并以偏最小二乘（PLS）法建立木犀草素的定量预测模型。结果显示,经Kennard-Stone(KS)筛选的模型相关系数R为0.994 7,交叉验证均方根误差（RMSECV）为1.947 8,预测残差（RPD）为4.292 7,说明模型稳健,误差小;预测集样品的预测均方根误差（RMSEP）为2.077 7,回收率为98.0%～105%。结果表明,基于木犀草素对水的近红外光谱的扰动可以进行木犀草素浓度测定。该方法简便、快速,结果准确,为生物活性成分的测定提供了一种新的方法。     

酸酐改性巴旦木壳在罗丹明B分析中的应用

采用邻苯二甲酸酐改性的巴旦木壳,作为吸附剂对稀溶液中罗丹明B进行富集与近红外光谱分析方法研究。首先考察了pH值和吸附时间对罗丹明B吸附率的影响;其次,富集了罗丹明B的吸附剂经近红外漫反射光谱可直接检测,最后以偏最小二乘回归法建立其定量校正模型进行含量预测。结果表明,在中性或偏碱性条件下,常温吸附10 min,罗丹明B的吸附率达到90%;光谱经标准正态变化处理后,罗丹明B校正模型的参考浓度和预测浓度之间的相关系数为0.9643,在0.8～20.0 mg·L~(-1)的较低浓度范围内,剔除奇异样本,预测集的回收率可以达到92.8～110.4%。基于以上结果,邻苯二甲酸酐改性的巴旦木壳可用于稀溶液中微量的罗丹明B的富集与近红外光谱灵敏检测。     

可见-近红外光谱结合CARS优化模型预测棕榈油碘值

采用可见-近红外透射光谱结合CARS变量优选方法优化模型,对棕榈油碘值进行近红外定量分析。通过将使用不同预处理方法产生的建模效果进行比较,找到了理想的预处理方法,通过CARS变量选择方法优选出与棕榈油碘值相关的有效波点共60个,利用60个有效波点建立棕榈油碘值优化模型。根据优化模型的建模集相关系数(R_c=0.9814)和预测集相关系数(R_p=0.9806),得到的建模均方根误差(RM SEC=0.0398)和预测均方根误差(RM SEP=0.0406)优于采用全波段建立的模型得到的系数误差。利用可见近红外透射光谱结合CARS变量优选方法,简化了棕榈油碘值模型,并能够保证碘值预测的准确度。     

生物吸附剂菹草干粉对Cr(Ⅵ)的吸附性能

开发了高效去除重金属Cr(Ⅵ)污染的生物吸附剂,菹草(Potamogeton crispus)干粉吸附剂,通过单因素分析考察了吸附时间、吸附剂颗粒大小、溶液初始pH值、吸附剂用量、Cr(Ⅵ)初始浓度以及离子强度等对重金属离子Cr(Ⅵ)的吸附性能。 结果表明,对吸附效果影响显著的因素有Cr(Ⅵ)初始浓度、吸附剂颗粒大小、溶液初始pH值和离子强度;其吸附行为符合准二级动力学方程,相关系数为0.9998;菹草对Cr(Ⅵ)的吸附等温线符合Langmuir方程。     

基于近红外光谱的食用植物油中反式脂肪酸含量快速定量检测及模型优化研究

利用近红外光谱技术对食用植物油中反式脂肪酸(Trans fatty acids,TFA)含量进行快速定量检测,并通过波段选择、预处理方法、变量筛选及建模方法对TFA含量预测模型进行优化.采用AntarisⅡ傅里叶变换近红外光谱仪在4000~10000 cm-1光谱范围采集98个食用植物油样本的近红外透射光谱,然后采用气相色谱法测定TFA的真实含量.首先,对样本原始光谱进行波段、预处理方法优选;在此基础上,采用竞争自适应重加权法(Competitive adaptive reweighted sampling,CARS)筛选TFA相关的重要变量,最后应用主成分回归、偏最小二乘和最小二乘支持向量机方法分别建立食用植物油中TFA含量的预测模型.研究结果表明,近红外光谱技术检测食用植物油中的TFA含量是可行的,优化后的最佳预测模型的校正集和预测集R2分别为0.992和0.989,RMSEC和RMSEP分别为0.071%和0.075%.最佳预测模型所用的变量仅26个,占全波段变量的0.854%.此外,与全波段偏最小二乘预测模型相比,其预测集R2由0.904上升为0.989,RMSEP由0.230%下降为0.075%.由此表明,模型优化非常必要,CARS能有效筛选TFA相关的重要变量,极大减少建模变量数,从而简化预测模型,并较大提高预测模型的精度和稳定性.     

新型磁性复合生物吸附剂吸附铀的实验研究

为了提升含铀废水的净化效果,制备一种新型磁性复合生物吸附剂,用于铀离子的吸附实验研究,运用BET吸附理论、红外光谱(IR)、X射线衍射光谱(XRD)、扫描电子显微镜(SEM)等对吸附剂进行表征,对吸附动力学进行研究.实验结果表明,Fe3 O4和啤酒酵母粉质量比为1:2,溶液pH值为5、吸附剂用量为0.05 g、初始浓度...     

超富集植物蜈蚣草对水中As(Ⅲ)吸附行为的研究

采用流动注射-氢化物发生-电热石英管原子吸收光谱法研究了超富集植物蜈蚣草对水中As(Ⅲ)的吸附行为。探讨了蜈蚣草的前处理方法、溶液pH值、吸附时间、吸附剂用量、As(Ⅲ)浓度和溶液体积等因素对蜈蚣草吸附As(Ⅲ)的吸附率的影响。结果表明,以50 mg经2 mol.L-1HCl洗脱处理后的蜈蚣草粉末为吸附剂,在pH为2.0、As(Ⅲ)浓度为20 ng.mL-1、溶液体积50 mL、吸附时间15 min条件下,蜈蚣草对As(Ⅲ)的吸附率可达86.1%,水中残余As(Ⅲ)仅为2.8 ng.mL-1。本法成本低廉、操作简便,可望直接用于地下水中As(Ⅲ)的去除。     

Diethylenetriamine-grafted poly(glycidyl methacrylate) adsorbent for effective copper ion adsorption

Amine-functionalized adsorbents have attracted increasing interest in recent years for heavy metal removal. In this study, diethylenetriamine (DETA) was successfully grafted (through a relatively simple solution reaction) onto poly(glycidyl methacrylate) (PGMA) microgranules to obtain an adsorbent (PGMA-DETA) with a very high content of amine groups and the PGMA-DETA adsorbent was examined for copper ion removal in a series of batch adsorption experiments. It was found that the PGMA-DETA adsorbent achieved excellent adsorption performance in copper ion removal and the adsorption was most effective at pH>3 in the pH range of 1-5 examined. X-ray photoelectron spectroscopy (XPS) revealed that there were different types of amine sites on the surfaces of the PGMA-DETA adsorbent but copper ion adsorption was mainly through forming surface complexes with the neutral amine groups on the adsorbent, resulting in better adsorption performance at a higher solution pH value. The adsorption isotherm data best obeyed the Langmuir-Freundlich model and the adsorption capacity reached 1.5 mmol/g in the case of pH 5 studied. The adsorption process was fast (with adsorption equilibrium time less than 1-4 h) and closely followed the pseudo-second-order kinetic model. Desorption of copper ions from the PGMA-DETA adsorbent was most effectively achieved in a 0.1 M dilute nitric acid solution, with 80% of the desorption being completed within the first 1 min. Consecutive adsorption-desorption experiments showed that the PGMA-DETA adsorbent can be reused almost without any loss in the adsorption capacity.     

浮石负载壳聚糖吸附去除水中丙溴磷

通过浮石负载壳聚糖制备了吸附剂壳聚糖/浮石复合物,采用扫描电子显微镜(SEM)、热重分析(TGA)、元素分析、傅里叶红外光谱(FT-IR)、X射线衍射(XRD)和X射线荧光光谱(XRF)等技术手段表征了吸附剂性质,考察了吸附剂量、吸附时间、溶液pH值、离子强度和温度对该吸附剂吸附去除水中丙溴磷的影响,研究了再生吸附剂的吸附性能。结果表明,负载在浮石上的壳聚糖占吸附剂总量的8.69%;在p H值3.0~7.0内,壳聚糖/浮石对丙溴磷的吸附率大于90%;这种吸附剂对丙溴磷的吸附受溶液离子强度影响较小,随温度升高而稍微减小。在溶液温度25℃、pH=7.0、丙溴磷浓度40 mg/L、壳聚糖/浮石剂量为0.7 g/L和吸附平衡时间为90 min条件下,此吸附剂对丙溴磷最大吸附率为93.3%(最大吸附量为53.4 mg/g)。壳聚糖/浮石连续经过3次吸附/再生循环,每次循环对丙溴磷的吸附率下降约12%。可见壳聚糖/浮石通过吸附可有效地去除水中的农药丙溴磷。     

Thiocyanate removal from aqueous solution by a synthetic hydrotalcite sol

The use of a chloride-containing synthetic hydrotalcite sol (LDHC) as adsorbent to remove thiocyanate from aqueous solution was investigated. LDHC was prepared by coprecipitation and was characterized by HRTEM, particle size, XRD, and FTIR. The experiments showed that LDHC was particularly effective in removing thiocyanate due to its small particle size and high zeta potential. The adsorption of thiocyanate on LDHC was favored when the initial solution pH was in the range 3-10, though the most effective pH range was between 4.0 and 8.0. The adsorption reached equilibrium within 150 min. The interaction between the surface sites of LDHC and thiocyanate ions may be a combination of both anion exchange and surface complexation. The pseudo-second-order model best described the adsorption kinetics of thiocyanate onto LDHC. The equilibrium isotherm showed that the adsorption of thiocyanate on LDHC was consistent with the Langmuir equation and the saturated adsorption capacity of LDHC for thiocyanate was 98.3 mg/g at 20°C. The regenerated LDHC in FeCl(3) solution can be used repeatedly in adsorption-regeneration cycles. The results showed that LDHC can be used as a new adsorbent for thiocyanate removal from aqueous solution because of its high adsorption capacity and rapid adsorption rate.     

Removal of Rhodamine B,a Cationic Dye From Aqueous Solution Using Poly(cyclotriphosphazene-co-4,4′-sulfonyldiphenol) Nanotubes

Poly(cyclotriphosphazene-co-4,4′-sulfonyldiphenol) (PZS) nanotubes were evaluated as an efficient adsorbent for the removal of Rhodamine B (RhB), a cationic dye from aqueous solution. The as-synthesized adsorbent (PZS nanotubes) were characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FTIR) and N₂ adsorption/desorption isotherms. The factors influencing the adsorption efficiency and capacity had been systematically studied. Results showed that the adsorption was highly dependent on temperature, initial RhB concentration and adsorbent dose. Effects of initial solution pH indicate that the adsorption can proceed in both basic and acidic environment. The equilibrium absorption capacity at 25°C can reach up to 35.58 mg/g within 60 min implying the adsorption procedure was highly rapid. The kinetic data was better described by the pseudo-second-order model with the correlation coefficient (R² = 0.9981), and the adsorption process followed Weber's intraparticle model, indicating the adsorption process could be divided into two stages. Results also showed that the adsorption equilibrium obeyed the Langmuir isotherm, and the value of equilibrium parameter R_L suggested that the PZS nanotubes were an efficient adsorbent for the removal of RhB from aqueous solution.     

Synthesis, characterization, thermodynamic and kinetic investigations on uranium (VI) adsorption using organic-inorganic composites: Zirconyl-molybdopyrophosphate-tributyl phosphate

Zirconyl-molybdopyrophosphate-tributyl phosphate (ZMPP-TBP) was a novel organic-inorganic composite adsorbent prepared by co-precipitation method and used in the adsorption of uranium from aqueous solution in batch adsorption experiments. The as-obtained product was characterized using SEM, energy dispersive X-ray spectroscopy (EDX), XRD and BET-N₂ adsorption measurements. The study had been conducted to investigate the effects of solution pH, temperature, contact time, initial concentration and coexisting ions. A maximum removal of 99.31% was observed for an initial concentration 5 mg/L, at pH 6.0 and an adsorbent dose of 1.0 g/L. The isothermal data were fitted with both Langmuir and Freundlich equations, but the data fitted the former better than the latter. According to the evaluation using the Langmuir equation, the maximum adsorption capacity of uranium (VI) was 196.08 mg/g at 293 K and pH 6.0. The pseudo-first-order kinetic model and pseudo-second-order kinetic model were used to describe the kinetic data, and the pseudo-second-order kinetic model was better. The thermodynamic parameter ΔG was calculated, the negative ΔG values of uranium (VI) at different temperature showed that the adsorption process was spontaneous. The good reusability of ZMPP-TBP also indicated that the ZMPP-TBP was a very promising adsorbent for uranium adsorption from aqueous solution.     

Surface-bound humic acid increased rhodamine B adsorption on nanosized hydroxyapatite

In this study, humic acid-bound nanosized hydroxyapatite (HA-nHAP) was developed as a novel adsorbent, and the potential of using HA-nHAP for the adsorption of rhodamine B (RhB) from aqueous solution as functions of pH, adsorbent dosage, contact time, ionic strength, and temperature was investigated. The results indicated that the HA binding significantly increased the adsorption of RhB due to the introduction of abundant negatively charged functional groups. The adsorption capacity of HA-nHAP for RhB was found to be pH-dependent, and the optimal pH value was found to be 6.0. The adsorption equilibrium data obeyed Sips and Freundlich isotherms and the kinetic data were well described by the Elovich kinetic model. According to the Sips equation, the maximum adsorption capacity for RhB was 24.12 mg/g. The temperature and ionic strength experiment showed that they both had an effect on the adsorption capacity of HA-nHAP. Thermodynamic study confirmed that the adsorption was a spontaneous, endothermic, and more random arrangement process. The present investigation showed that HA-nHAP is a promising adsorbent for the removal of RhB from aqueous solution.     

Enhanced adsorptive removal of toxic dyes using SiO2 nanofibers

Electrospinning method was used to synthesize porous SiO₂ nanofibers. The adsorption of Methyl Orange and Safranin O by porous SiO₂ nanofibers was carried out by varying the parameters such as pH, contact time, adsorbent dose, dye concentration, and temperature. Equilibrium adsorption data followed Langmuir isotherms. Kinetic adsorption followed second-order rate kinetics model. The maximum adsorption capacity for Methyl Orange and Safranin O was found to be 730.9 mg/g and 960.4 mg/g, respectively. Acidic pH was favorable for the adsorption of Methyl Orange while basic pH was favorable for the adsorptions of Safranin O. Modeling study suggested the major mode of adsorption, while thermodynamic study showed the endothermic reactions. This effort has pronounced impact on environmental applications of SiO₂ nanofibers as auspicious adsorbent nanofibers for organic material from aqueous solution.     

Enhanced Removal of Cu(II) Ions from Aqueous Solution by Poorly Crystalline Hydroxyapatite Nanoparticles

Poorly crystalline and well-dispersed hydroxyapatite (HAP) nanoparticles were synthesized and used as novel adsorbents for the removal of Cu(II) from aqueous solution. Various factors affecting the adsorption such as adsorbent crystallinity, pH, adsorbent dosage, contact time, temperature, competing cations, and the presence of humic acid were investigated in detail. Results showed that the HAP calcined at lower temperature was poorly crystalline and had better adsorption capacity for Cu(II) than those calcined at higher temperature. Cu(II) removal was increased with increases of pH, adsorbent dosage, temperature, and the presence of humic acid, but decreased as the existence of competing divalent cations. Kinetic studies showed that pseudo-second-order kinetic model better described the adsorption process. Equilibrium data were best described by Langmuir model, and the estimated maximum adsorption capacity of poorly crystalline HAP was 41.80 mg/g at 313 K, displaying higher efficiency for Cu(II) removal than many previously reported adsorbents. Thermodynamics studied revealed that the adsorption of Cu(II) by poorly crystalline HAP was spontaneous, endothermic, and entropy-increasing in nature. This study showed that poorly crystalline HAP could be used as an efficient adsorbent material for the removal of Cu(II) from aqueous solution.     

Facial Synthesis of Adsorbent from Hemicelluloses for Cr(VI) Adsorption

It is challenging work to develop a low-cost, efficient, and environmentally friendly Cr(VI) adsorbent for waste water treatment. In this paper, we used hemicelluloses from chemical fiber factory waste as the raw material, and prepared two kinds of carbon materials by the green hydrothermal method as adsorbent for Cr(VI). The results showed that hemicelluloses hydrothermally treated with citric acid (HTC) presented spherical shapes, and hemicelluloses hydrothermally treated with ammonia solution (HTC-NH₂) provided spongy structures. The adsorption capacity of the samples can be obtained by the Langmuir model, and the adsorption kinetics could be described by the pseudo-second-order model at pH 1.0. The maximum adsorption capacity of HTC-NH₂ in the Langmuir model is 74.60 mg/g, much higher than that of HTC (61.25 mg/g). The green hydrothermal treatment of biomass with ammonia solution will provide a simple and feasible way to prepare adsorbent for Cr(VI) in waste water treatment.