Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry

An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0 mL/min, and dicyandiamide was eluted with 20 mL of a methanol/acetonitrile mixture (V/V = 2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography–ultraviolet spectroscopy (HPLC–UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC^®-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50 mm × 2.1 mm, 3.5 μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R² > 0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n = 3) were below 6.1% with a detection limit of 5.0 ng/mL for stream water samples.     

Promoting effect of vanadium on catalytic activity of Pt/Ce–Zr–O diesel oxidation catalysts

A series of Pt–V/Ce–Zr–O diesel oxidation catalysts was prepared using the impregnation method. The catalytic activity and sulfur resistance of Pt–V/Ce–Zr–O were investigated in the presence of simulated diesel exhaust. The effect of vanadium on the structure and redox properties of the catalysts was also investigated using the Brunauer–Emmett–Teller method,X-ray diffraction, H2temperature-programmed reduction, CO temperature-programmed desorption, X-ray photoelectron spectroscopy, and Energy Dispersive Spectroscopy. Results showed that the Pt particles were well dispersed on the Ce–Zr–O carrier through the vanadium isolation effect, which significantly improved the oxidation activity toward CO and hydrocarbons. An electron-withdrawing phenomenon occurred from V to Pt, resulting in an increase in the metallic nature of platinum, which was beneficial to hydrocarbon molecular activation.     

Activated carbon coated palygorskite as adsorbent by activation and its adsorption for methylene blue

An activation process for developing the surface and porous structure of palygorskite/carbon(PG/C) nanocomposite using ZnC l2 as activating agent was investigated. The obtained activated PG/C was characterized by X-ray diffraction(XRD), Fourier transform infrared spectroscopy(FTIR), field-emission scanning electron microscopy(SEM), and Brunauer–Emmett–Teller analysis(BET) techniques. The effects of activation conditions were examined,including activation temperature and impregnation ratio. With increased temperature and impregnation ratio, the collapse of the palygorskite crystal structure was found to accelerate and the carbon coated on the surface underwent further carbonization. XRD and SEM data confirmed that the palygorskite structure was destroyed and the carbon structure was developed during activation. The presence of the characteristic absorption peaks of C_C and C–H vibrations in the FTIR spectra suggested the occurrence of aromatization. The BET surface area improved by more than 11-fold(1201 m2/g for activated PG/C vs. 106 m2/g for PG/C) after activation, and the material appeared to be mainly microporous. The maximum adsorption capacity of methylene blue onto the activated PG/C reached 351 mg/g. The activated PG/C demonstrated better compressive strength than activated carbon without palygorskite clay.     

Determination of 27 pharmaceuticals and personal care products (PPCPs) in water: The benefit of isotope dilution

• Isotope dilution method was developed for the determination of 27 PPCPs in water. • The established method was successfully applied to different types of water samples. • The correction effect of corresponding 27 ILSs over 70 d was investigated. • Benefit of isotopic dilution method was illustrated for three examples. Pharmaceuticals and personal care products (PPCPs) are a unique group of emerging and non-persistent contaminants. In this study, 27 PPCPs in various water samples were extracted by solid phase extraction (SPE), and determined by isotope dilution method using liquid chromatography coupled to tandem triple quadruple mass spectrometer (LC-MS/MS). A total of 27 isotopically labeled standards (ILSs) were applied to correct the concentration of PPCPs in spiked ultrapure water, drinking water, river, effluent and influent sewage. The corrected recoveries were 73%–122% with the relative standard deviation (RSD)<16%, except for acetaminophen. The matrix effect for all kinds of water samples was<22% and the method quantitation limits (MQLs) were 0.45–8.6 ng/L. The developed method was successfully applied on environmental water samples. The SPE extracts of spiked ultrapure water, drinking water, river and wastewater effluent were stored for 70 days, and the ILSs-corrected recoveries of 27 PPCPs were obtained to evaluate the correction ability of ILSs in the presence of variety interferences. The recoveries of 27 PPCPs over 70 days were within the scope of 72%–140% with the recovery variation<37% in all cases. The isotope dilution method seems to be of benefit when the extract has to be stored for long time before the instrument analysis.     

固相萃取-超高效液相色谱/三重四极杆质谱法同时测定地表水中8种亚硝胺类化合物

建立了固相萃取（SPE）-超高效液相色谱/三重四极杆串联质谱（UPLC-MS/MS）同时测定地表水中8种亚硝胺类化合物的方法。水样中目标物经椰壳活性炭固相萃取小柱吸附富集，小柱经氮气吹干后采用二氯甲烷洗脱。待测样品采用Atlantis T₃柱，以水-甲醇作为流动相进行梯度洗脱，大气压力化学电离源（APCI）正离子模式多反应监测方式（MRM）进行检测，内标法定量分析。8种目标物在相关线性范围内线性良好(r≥0.9950)，地表水加标回收率为55.4%~90.4%，相对标准偏差为3.1%~14.3%，方法检出限为1.1 ~1.8 ng/L。本方法准确度和灵敏度高，适用于快速测定地表水中8种亚硝胺类化合物含量。     

液氮泡沫发生器内流动特性研究

低温液氮与泡沫混合液直接接触产生氮气泡沫是一种新型的掺混形式,利用液氮高汽化比的特点,搭建液氮泡沫可视化实验装置,进行氮气-水两相流及液氮泡沫流动特性的研究。结果表明,液氮相变产生大量氮气,其与泡沫液混合产生泡沫,温度有所回升,最终趋于泡沫混合液温度;管路沿程压降较小;液氮射流破碎及流动过程可分为6个区域:低温液氮区、向上循环翻滚区、滞留区、泡沫与泡沫混合液混合区、致密泡沫区、泡沫混合液区。流体向下游流动过程中持续发泡;为防止管路结冰,需合理控制泡沫混合液与液氮流量。     

Enhanced triallyl isocyanurate (TAIC) degradation through application of an O3/UV process: Performance optimization and degradation pathways

• UV/O₃ process had higher TAIC mineralization rate than O₃ process. • Four possible degradation pathways were proposed during TAIC degradation. • pH impacted oxidation processes with pH of 9 achieving maximum efficiency. • CO₃^2– negatively impacted TAIC degradation while HCO₃^– not. • Cl^– can be radicals scavenger only at high concentration (over 500 mg/L Cl^–). Triallyl isocyanurate (TAIC, C₁₂H₁₅N₃O₃) has featured in wastewater treatment as a refractory organic compound due to the significant production capability and negative environmental impact. TAIC degradation was enhanced when an ozone(O₃)/ultraviolet(UV) process was applied compared with the application of an independent O₃ process. Although 99% of TAIC could be degraded in 5 min during both processes, the O₃/UV process had a 70%mineralization rate that was much higher than that of the independent O₃ process (9%) in 30 min. Four possible degradation pathways were proposed based on the organic compounds of intermediate products identified during TAIC degradation through the application of independent O₃ and O₃/UV processes. pH impacted both the direct and indirect oxidation processes. Acidic and alkaline conditions preferred direct and indirect reactions respectively, with a pH of 9 achieving maximum Total Organic Carbon (TOC) removal. Both CO₃^2– and HCO₃^– decreased TOC removal, however only CO₃^2– negatively impacted TAIC degradation. Effects of Cl^– as a radical scavenger became more marked only at high concentrations (over 500 mg/L Cl^–). Particulate and suspended matter could hinder the transmission of ultraviolet light and reduce the production of HO· accordingly.     

高效液相色谱串联质谱法测定某市污水处理厂进出水中的全氟化合物

通过建立直接进样-高效液相色谱串联质谱（HPLC-MS/MS）测定污水处理厂进出水中的10种全氟化合物的方法，了解污水厂进出水中全氟化合物污染情况。10种目标分析物在10~500 ng/L范围内具有良好的线性关系，方法检出限为2.3~8.3 ng/L，精密度为2.1%~7.1%，加标回收率为60.6%~91.7%。应用该方法测定某市典型污水厂进出水中的全氟化合物，进水中全氟化合物质量浓度为90.9~206 ng/L，主要污染物是PFOA、PFHxS和PFBS；出水中全氟化合物的质量浓度为67.4~158 ng/L，环境排放量为6.7~22.9 g/d，主要污染物是PFOA和PFHxS。结果表明，该方法能很好地适用于复杂基质中10种全氟化合物的检测。     

基于RFPA2D复合局部挠曲岩体数值模拟

为研究复合局部挠曲岩体强度特征以及破坏规律，采用岩石真实破裂软件RFPA^2D，对水平层面挠曲30°，45°，60°，75°的复合岩体进行单轴压缩试验模拟。模拟结果表明:挠曲角为30°，45°，60°，75°的复合岩体破坏面几乎与挠曲段夹层重合，其挠曲端部均产生了垂直于挠曲段夹层的裂纹；复合单斜岩体与复合挠曲岩体破坏面的形成因素大致相同，夹层强度是2种岩体失稳的主要因素；复合挠曲岩体单轴抗压强度随挠曲角增大同样呈“U”型变化，与单斜岩体变化趋势一致；当水平层状岩体发生挠曲后，其单轴抗压强度减小，当挠曲角为60°时，强度降低25.19%，当挠曲角为75°时，强度降低0.17%。；随着均质系数m的增大，复合挠曲岩体单轴抗压强度以及轴向应变均出现逐渐递增的趋势，且不同m值，其岩体裂隙扩展方式具有明显差别。     

高效液相色谱-三重四级杆/复合线性离子阱质谱法测定饮用水中22种邻苯二甲酸酯

建立了一种同时测定饮用水中22种邻苯二甲酸酯(PAEs)的高效液相色谱-三重四级杆/复合线性离子阱质谱方法:饮用水样品经针头过滤器过滤,选用Biphenyl液相色谱柱进行分离,以含0.1%甲酸的水溶液和含0.1%甲酸的甲醇溶液为流动相,电离模式为电喷雾正离子,选用多反应监测触发增强子离子扫描模式进行检测。结果表明,22种PAEs的灵敏度良好,定量限为0.001～0.1 μg/L。配制浓度为0.1～100.0 μg/L的混标溶液进行进样分析,分析结果显示,22种PAEs在该范围内的线性关系良好,相关系数均大于0.995,方法的平均回收率为82.9%～108.9%,相对标准偏差为0.9%～11.2%。同时,使用增强子离子扫描谱图进行搜库匹配,定性准确性高。该方法适用于饮用水中PAEs的检测。