Carbonized cotton fibers via a facile method for highly sensitive solid‐phase microextraction of polycyclic aromatic hydrocarbons

Cotton fiber is an environmentally friendly and natural material with a certain extraction capacity, while its enrichment ability is poor. In order to improve the extraction efficiency of cotton fibers, it was carbonized to form a layer of amorphous carbon as the sorbent by a simple carbonization method. Carbonized cotton fibers were filled into a polyetheretherketone tube for in‐tube solid‐phase microextraction. The carbonization time was investigated to obtain high extraction efficiency. Coupled to high‐performance liquid chromatography, the extraction tube was evaluated with polycyclic aromatic hydrocarbons, estrogens and phthalates, and it exhibited best extraction efficiency for polycyclic aromatic hydrocarbons. Under the optimum conditions, an online analysis method for several polycyclic aromatic hydrocarbons was established with large linear ranges (0.016–0.20 μg/L), low limits of detection (0.005–0.020 μg/L), and high enrichment factors (948–2874). Analysis method was successfully applied to the detection of targets in the real samples and shown satisfactory durability and chemical stability. Moreover, the relative recoveries ranged from 82 to 119.2%, which demonstrated the applicability of carbonized cotton fibers in sample preparation. Compared with other reported methods, the proposed method provided shorter extraction time, higher enrichment factors, comparable limits of detection, and recoveries.     

Nano‐MoO3 for highly selective enrichment of polycyclic aromatic hydrocarbons in in‐tube solid‐phase microextraction

Nano‐molybdenum trioxide was prepared from nano‐molybdenum disulfide by simple firing in muffle furnace. Nano‐molybdenum trioxide was used as the extraction coating on the stainless steel wire. Four wires were filled in a polyetheretherketone tube to get an extraction tube. The tube was connected to the six‐port valve of a high performance liquid chromatograph, and the online analysis system was constructed. Extraction selectivity of the tube for different types of compounds, including polycyclic aromatic hydrocarbons, plasticizers, estrogens, anilines and neonicotinoids, was studied. Good enrichment ability for polycyclic aromatic hydrocarbons, but the extraction efficiency of others was not satisfactory. Using eight polycyclic aromatic hydrocarbons as the targets, an analytical method was established after optimizing main factors such as sampling volume, sampling rate, methanol content, and desorption time. The established method exhibited wide linear range to 0.016–20.00 μg/L and low limits of detection to 0.005 μg/L, and the enrichment factors can be up to 2443. The method was applied to the detection of trace polycyclic aromatic hydrocarbons in tap water and river water, and a good recovery was obtained. The tube showed good durability and chemical stability, and it still remained good extraction effect after more than 140 run.     

稀土奥贝蠕铁制取工艺及其性能的研究

稀土奥贝蠕铁可用含稀土的蠕化剂及等温淬火工艺稳定地制取,藉助高温扫描电子显微镜,观察并研究了稀土蠕铁奥氏体化过程及稀土奥贝蠕铁随温度升高时组织的变化。用带有加热装置的万能材料试验等土奥贝蠕铁的各种性能进行了系统测定了如抗拉强度、延伸率、冲吉韧性、热膨胀系数及伸长百分率,结果表明,稀土奥贝蠕铁在室温和高温下均有良好的性能。     

在线中和富集及标准加入离子色谱法测定大气吸收液中的痕量阴离子

建立了大体积进样后的在线中和富集及在线标准加入离子色谱法,实现了对大气碱性吸收液中痕量氯离子、亚硝酸根、硝酸根、硫酸根的直接测定。比较了不同阀切换时间窗及在线中和柱的选择,确定了最佳的实验条件。利用戴安公司“谱睿”在线中和技术,通过Inguard H在线中和柱和CRD 200在线二氧化碳去除装置的共同作用,有效地去除了碱性吸收液中的OH~和CO2~3,使测定干扰降低到最小;通过大体积进样和在线富集,改进了样品的检出限,Cl~, NO~2, NO~3和SO2~4的检出限分别为17.5、171、34.7和42.4 ng/L;在线标准加入解决了痕量阴离子标准溶液的配制难题及NO~2低回收率对检测结果的影响。本方法实现了自动化分析,结果准确,重复性好,检测效率高,可用于常规离子色谱条件下无法测定的强碱性基体样品中痕量阴离子的准确测定。     

在线富集/高效液相色谱与电感耦合等离子体质谱联用测定玩具中超痕量可迁移六价铬

采用在线富集/高效液相色谱(HPLC)与电感耦合等离子体质谱(ICP-MS)联用技术,建立了玩具中超痕量可迁移六价铬的测定方法。以10 mmol/L硝酸铵为流动相,样品在Agilent BIO WAX NP5阴离子交换柱(4.6 mm×50 mm,5μm)中富集,再通过阀切换,以75 mmol/L硝酸铵将六价铬洗脱至Dionex AG7阴离子柱(4.0 mm×50 mm,10μm)中分离,最后经ICP-MS进行分析。优化得到在线富集时间为4 min,进样量为900μL,富集流速为0.4 mL/min,洗脱流速为0.6 mL/min。结果显示,六价铬在2～20 ng/L范围内线性良好,检出限为1.93 ng/L,相对标准偏差(RSD)为3.9%。与直接进样相比,浓缩因子约为8.1倍,富集效率约为90%。对欧盟玩具安全指令2009/48/EC规定的3类玩具材料在5、10 ng/L的浓度水平下进行加标回收,回收率为93.4%～111%。     

Liquid crystalline guanidinium phenylalkoxybenzoates: towards room temperature liquid crystals via bending of the mesogenic core and the use of triflate counter ions

A series of guanidinium salts 1(C _n ) _m –4(C _n ) _m ?X bearing phenyl alkoxybenzoate cores have been synthesised and their mesomorphic properties have been investigated by polarising optical microscopy (POM), differential scanning calorimetry (DSC) and powder X-ray diffraction experiments (small-angle X-ray scattering and wide-angle X-ray scattering). While compounds 1(C₁₂)₁?X and 3(C₁₂)₁?X with one alkoxy chain showed smectic A (SmA) phases irrespective of the counter ion, compounds 1(C₁₂)₂?OTf and 3(C₁₂)₂?OTf with two alkoxy chains displayed SmA phases and the corresponding chlorides 1(C₁₂)₂?Cl and 3(C₁₂)₂?Cl displayed Col_h. Guanidinium salts 1(C _n )₃–4(C _n )₃?X with three alkoxy chains showed Col_h phases. Whereas the use of cyclic guanidinium head groups rather than acyclic ones had only a minor influence on the mesophase properties, melting points were significantly decreased by bent core units instead of linear core units. Replacement of chloride counterions by triflate lead to a further depression of the clearing points and shifted the mesophase towards room temperature.     

Microwave‐Assisted Synthesis and Characterization of CuO Nanocrystals

CuO feather‐like and flower‐like crystals have been synthesized by a fast microwave‐assisted solution approach using Cu(NO₃)₂ and NaOH. The morphology transformation of CuO could be achieved by ionic liquid 1‐n‐butyl‐3‐methyl imidazolium tetrafluoroborate ([BMIM]BF₄). With [BMIM]BF₄, flower‐like CuO were obtained, whereas without [BMIM]BF₄, feather‐like CuO were obtained. The possible formation mechanism of flower‐like CuO was discussed on the basis of experimental results. The products were characterized by XRD, FESEM/EDS, and TEM/SAED. In addition, the adsorption of [BMIM]BF₄ on flower‐like CuO was confirmed by FTIR and TG/DSC, and the band gap energies of the flower‐like CuO was estimated by UV‐vis spectra.     

电感耦合等离子体质谱（ICP-MS）法测定黄精中15种稀土元素及其指纹图谱绘制

为了准确测定黄精中稀土元素的含量,采用电感耦合等离子体质谱（ICP-MS）法同时测定黄精中15种稀土元素（La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu）的含量,进而绘制稀土元素指纹图谱,以稀土元素含量的平均值构建黄精稀土元素标准指纹图谱,作为鉴定黄精中药材的参考依据。黄精样品采用微波消解法处理后,通过在线引入内标溶液,采用ICP-MS法测定15种稀土元素的含量,采用OriginPro 2021绘制稀土元素指纹图谱和进行主成分分析,采用SPSS 26.0进行聚类分析。15种稀土元素的线性关系、重复性、精密度良好,平均加标回收率在97.0%~103.3%,相对标准偏差小于等于1.74%。黄精中Ce、La、Nd含量相对较高,Ce含量为53.02～2004.58 μg/kg,位居第一。聚类分析和主成分分析结果表明,样品聚为2类,同一产地的样品能够较好地聚在一起。黄精药材中15种稀土元素的指纹图谱具有相似的分布形态,具有较强的特征性和一致性,相似度均大于0.950。该方法操作简单,准确可靠,能满足实验分析要求,可为黄精的质量控制和药理研究提供参考;建立的指纹图谱可用于黄精的鉴别。