Kinetics of COD Removal in a Biological Aerated Filter in the Presence of 2,4,6-Trinitrophenol （Picric Acid）

为在一个生物充气过滤器(BAF ) 的货到付款移动的一个实验模型面对 2,4,6-trinitrophenol (TNP ) 被开发，它沿着床高度联系了自河货到付款到流入的货到付款或水力的装载率。为底层简历降级的全面反应率能首先被描述为假顺序。对反应堆高度的货到付款移动的试验性的数据被用来在实验模型计算参数。在不同反应堆高度的货到付款集中被表示为流入的货到付款集中和水力的装载率的功能， ln (C 0/C)= 0.124H/Q 0.770 和 ln (C/0)=−； 5.63H/L 0.94}, 分别地，在试验性的条件下面。模型可以被用来为设计以不同的水力的装载率和流入的货到付款集中沿着反应堆高度预言 COD 移动侧面，选择并且 BAF 缩放。

An AIPE-active fluorinated cationic Pt(Ⅱ)complex for efficient detection of picric acid in aqueous media

A novel cationic Pt(Ⅱ)complex 2 with 2-(2,4-difluorophenyl)pyridine as the cyclometalating ligand and 1,10-phenanthroline as the auxiliary ligand has been synthesized and fully characterized.This complex exhibits much higher aggregation-induced phosphorescent emission activity than that of a nonfluorinated complex 1 in CH_(3)CN/H_(2)O.The complex 2 demonstrates efficient detection on picric acid(PA)in CH_(3)CN/H_(2)O,providing a high quenching constant(K_(SV)=2.3×10^(4) L/mol)and a low limit of detection(LOD=0.26μmol/L).In addition,complex 2 shows high selectivity for detection of PA in real water samples.Density functional theory calculations and proton nuclear magnetic resonance spectra suggest that the detection mechanism is attributed to the photo-induced electron transfer.

A fluorescent Eu(Ⅲ) MOF for highly selective and sensitive sensing of picric acid

A metal-organic framework [Eu_3L_3(CH_3COO)_2(H_2O)_2(μ_3-OH)]·3 DMF,(EuL, H_2L=9H-carbazole-2,7-dicarboxylic acid,DMF=N,N-dimethylformamide) has been synthesized under solvothermal conditions and structurally characterized. In EuL,Eu_6O_8 clusters are four-bridged by carboxylates to form parallel-aligned Eu–O–C chains, which are further linked by the carbazole moieties of L^(2-) ligands to form the three-dimensional framework with rhombic channels. The EuL material with characteristic emission of Eu^(3+) ion exhibits significant luminescence quenching response for picric acid(PA) and the linear Stern-Volmer plot was observed in the concentration range of 0.05–0.15 mM with K_(sv) of 98074 M^(-1). As far as we know, this Ksv is among the highest values for COFs and MOFs in detection of PA. The excellent anti-interference ability and repeatability were also verified by experiments. Lastly, we investigated the luminescence quenching mechanism in the EuL sensing system.

Detection of Picric Acid by Terpy-Based Metallo- Supramolecular Fluorescent Coordination Polymers in Aqueous Media

The synthesis of two linear terpy-based metallo-supramolecular fluorescent coordination polymers through 1 ： 1 complexation of Zn^2＋ and Cd^2＋ ions with ditopic terpyridine ligand was reported. The dispersibility of P1 and P2 was significantly improved in organic solvent and water through the introduction of hydrophilic oligo-ethyoxy side chain. Two polymers displayed yellow light emission both in solution and the solid state due to the intra-ligand charge transfer （ILCT） between the d^10 metal ions and the conjugated spacer unit. These coordination polymers were explored as fluorescent chemosensors for detecting picric acid in aqueous media, displaying high sensitivity and good selectivity. In addition, test strips were prepared from these polymers and exhibited the practical potential of detecting the NACs pollutants in the outdoor water for public safety and security.

苦味酸检测进展:基于Citespace的可视化分析

以中国知网数据库2008年至2023年间与“苦味酸检测”主题相关的123篇文献为数据来源,通过CiteSpace软件进行数据处理和可视化呈现,探讨了苦味酸检测近年来的发展趋势,介绍了一些关于苦味酸检测的新方法,重点分析了荧光探针法检测苦味酸。

A highly stable terbium metal-organic framework for efficient detection of picric acid in water

A highly stable fluorescent terbium MOF(Tb_(4)(paip)_(6)·1.2 H_(2) O,paip = 5-(1 H-pyrazole-4-yl)isophthalate)showing a sharp green emission(545 nm) and a quantum yield of 21.0% was successfully synthesized.This compound is shown to be a recyclable sensor for detecting picric acid in aqueous solution with both high sensitivity and selectivity,attributed to the electron transfer quenching mechanism.

Visual sensing of picric acid in 100% aqueous media based on supramolecular polythiophene assemblies with colorimetric and fluorescent dual response

A colorimetric and fluorometric dual probe based on a water-soluble polythiophene derivative(PMTPBA)was designed and synthesized.It can be applied to determination of picric acid(PA) in 100% aqueous solution.The approach relies on the formation of supramolecular polythiophene assemblies in the presence of PA through electrostatic,charge transfer and π-π stacking interactions.This probe could be utilized for the rapid and visual detection of PA both in aqueous solution and solid support with high specificity and sensitivity.The detection limit of this sensor is as low as 5.0 × 10^-8 mol/L.

Pyrenoviologen-based fluorescent sensor for detection of picric acid in aqueous solution

Two highly emissive pyrenoviologen derivatives were synthesized and used to fabricate fluorescent sensors for detection of picric acid(PA)with good sensitivity and selectivity.The sensitivity of the sensor was attributed to the specific electrostatic association effect of the cationic pyrenoviologens to the picrate anions,which also gave the sensor special selectivity among other compounds with similar structure.The electron transfer between them was attributed to the fluorescence response.Fluorescence lifetime measurements revealed that the quenching is static in nature.The novel and efficient pyrenoviologen derivatives-based sensors offered a strategy to fabricate real-life PA sensor.

A Water-stable Tetranuclear Cd(Ⅱ)Bicyclic Complex Used for the Picric Acid Detection

By solvothermal reaction of Cd(II)with organic ligand N,N’-bis(3,5-dicarboxylphenyl)-thiophene-2,5-dicarboxamide(H_(4)L),a water-stable complex[Cd_(4)(H_(2)L)_(4)(H_(2)O)_(10)]·2CH_(3)OH·8H_(2)O·4DMF(1,C_(102)H_(120)Cd_(4)N_(12)O_(64)S_(4))has been successfully synthetized(DMF=N,N-dimethylformamide).1 crystallizes in the triclinic space group of P1 with a=11.815(7),b=16.209(9),c=16.742(9)Å,α=82.224(13)°,β=76.741(13)°,γ=70.313(12)°,V=2932(3)Å^(3),M_(r)=3115.93,Z=1,F(000)=1584,D_(c)=1.765 Mg/cm^(3),μ=0.901 mm^(-1),GOOF=1.101,the final R=0.0391 and wR=0.1297 for 9007 observed reflections(I>2σ(I)).1 is a tetranuclear Cd(II)bicyclic complex with strong ligand-based blue emission and can stably exist in aqueous solutions over the pH range of 2~11.1exhibits high sensitivity,selectivity and anti-interference capability for picric acid(PA)detection in aqueous solution by luminescent quenching.The value of quenching constant(K_(sv))is 3.2×10^(4)M^(-1) within the PAconcentration range of 0~40μM and the detection limit is 6.89×10^(-7) M.Lastly,we went into depth on possible mechanism of the luminescent quenching.

碳量子点荧光探针的制备及其在苦味酸检测中的应用

以银杏叶为原料,采用水热法制备得到新型荧光碳量子点(CQDs)。该碳量子点的平均粒径为5.5 nm,最大激发波长为335 nm,最大发射波长为418 nm。基于碳量子点荧光光谱与苦味酸(PA)吸收光谱存在部分重叠而发生荧光共振能量转移(FRET),建立了以碳量子点作为荧光探针用于苦味酸检测的新方法。在最佳实验条件下,加入苦味酸前、后的荧光强度比值(I0/I)与苦味酸浓度(c)在0.2~800μmol/L范围内呈良好的线性关系,相关系数(r)为0.999 5,检出限(LOD)为32 nmol/L。在5、40、80μmol/L加标水平下,实际水样中苦味酸的回收率为98.0%~104%,相对标准偏差(RSD)为1.0%~3.2%。该方法可用于实际样品中苦味酸的灵敏、快速和高效检测。

衍生化-液液萃取气相色谱法测定环境水体中苦味酸

建立衍生化-液液萃取气相色谱法测定环境水体中的苦味酸。环境水体中的苦味酸经次氯酸钠氯化衍生后,用正己烷提取后进行气相色谱分析。对萃取溶剂、衍生化反应温度和时间、衍生试剂(次氯酸钠)的加入量、色谱柱的选择以及色谱分析条件进行了优化,采取正己烷作为萃取试剂,加入次氯酸钠溶液2.0 mL,选择衍生化反应温度为35℃,反应时间为50 min,DB-5细管柱(30 m×0.32 mm,0.25μm)作为分离柱,当取样体积为10 mL时,方法检出限为0.2μg/L。用该方法对实验用水做了高、中、低质量浓度水平的加标回收试验,回收率为85.5%~105.6%,相对标准偏差为2.93%~4.49%(n=6)。

微波辅助快速合成卵清蛋白金纳米簇检测苦味酸

本文采用微波加热法快速合成了卵清蛋白金纳米簇荧光探针(OVA-Au NCs)并应用于检测苦味酸(PA)。该探针在350 nm波长激发下,能发射红色荧光,最大发射荧光峰为680 nm,Stokes位移高达330 nm,可有效消除共振散射光的干扰。该合成方法与水热法相比,步骤简单快速,仅用50 s即可完成。由于PA的吸收光谱与OVA-Au NCs的激发光谱有较大范围的重叠,基于内滤效应(IFE) PA可选择性猝灭OVA-Au NCs的荧光,据此建立了检测苦味酸的新方法。在最佳实验条件下,在20~240μmol/L范围内,检测体系的荧光猝灭效率ΔF/F0与PA的浓度具有良好的线性关系,r为0.9985,检测限为6.4μmol/L。该方法简便、快速、准确,易于实现实时监测。

IC-MS和UHPLC-MS/MS方法测定地表水中丁基黄原酸和苦味酸

建立了直接进样离子色谱-质谱(IC-MS)和超高效液相色谱-串联质谱(UHPLC-MS/MS)测定地表水中丁基黄原酸和苦味酸的方法,2种方法简便易行,且灵敏度高。比较了2种方法测定丁基黄原酸和苦味酸的检出限、准确度和精密度,并用这2种方法同时分析了22份实际水样品中丁基黄原酸和苦味酸的质量浓度,结果均未检出。2种方法均能满足检测的要求,通过试验结果发现UHPLC-MS/MS法的检出限低于IC-MS法,但不能同时检测丁基黄原酸和苦味酸,而IC-MS法在符合方法要求的同时,可一次性检测这2种物质。因此,在要求同时检定水样中丁基黄原酸和苦味酸2种有机物时,推荐优先使用IC-MS法。

气相色谱法测定水中的苦味酸

建立了毛细管柱气相色谱-微池电子捕获检测器测定水中苦味酸的方法。水样中的苦味酸经次氯酸钠氯化衍生后,经正己烷提取后进行气相色谱分析。考察了萃取溶剂和次氯酸钠加入量对萃取的影响。在优化萃取条件下,苦味酸在25-500μg/L范围内有良好的线性关系。在低、中、高三个添加水平,苦味酸的回收率为83.0%-91.74%,相对标准偏差为1.79%-3.82%。

超高效液相色谱-串联质谱法快速测定地表水中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯

建立了一种经简单过滤即可直接进样的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法,可快速测定地表水中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯5种有机物的残留。样品经0.2μm针式滤头过滤除去颗粒性杂质后,进行UPLC-MS/MS分析,采用UPLC HSS T3色谱柱,2 mmol/L乙酸铵甲醇溶液和2 mmol/L乙酸铵水溶液作为流动相进行梯度洗脱,电喷雾离子源电离,正、负离子切换多反应监测模式进行定性和定量分析。5种目标化合物分别在0.10~10.0μg/L或1.00~100μg/L范围内线性关系良好,相关系数为0.996~0.999,方法的检出限为0.01~0.22μg/L;高、中、低3个添加水平的回收率为81.4%~113%,相对标准偏差为0.84%~14.0%。利用该方法对杭州市部分河流和水库的地表水样品进行分析,其中阿特拉津和溴氰菊酯在部分水样中有阳性检出。结果表明,该方法简便快捷、灵敏准确,适用于地表水样品中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯的快速测定。

4,4′-联吡啶锌(Ⅱ)配合物的合成及其晶体结构

苦味酸锌与44′联吡啶反应得到一种新型配合物Zn44′bpy2H2O2pic2·2H2O44′bpy44′联吡啶pic-苦味酸根并用元素分析、红外光谱等进行表征。X射线单晶衍射结果表明晶体属单斜晶系空间群Cc晶胞参数a=1.43902b=1.14181c=2.29083nmβ=95.081°V=3.7491nm3Z=4该配合物由44′联吡啶与金属配位形成多孔的二维网二维网再由未配位的水分子及苦味酸根离子通过氢键作用沿a轴方向堆积得三维网状结构且未配位的水分子、苦味酸根离子被包合在网络之中展示出一定的包合现象。

荧光熄灭的苦味酸光化学传感器

苦味酸对固定于聚氯乙烯 (PVC)膜中的N ,N′ 二苄基 3 ,3′,5 ,5′ 四甲基联苯二胺 (TMBD)有可逆荧光猝灭作用 ,据此研制成测定苦味酸浓度的荧光化学传感器。该传感器敏感膜最佳组成为 :5 0mgPVC、1 0 0mg癸二酸二异辛脂 (DOS)和 6.0mgTMBD。在 0 .1 2mol LH2 SO4底液中测定苦味酸 ,其线性响应范围为 2 .1 0×1 0 - 7～ 4 .0 0× 1 0 - 4 mol L ,检出限为 7.8× 1 0 - 8mol L ,其响应时间小于 4 0s。该传感器具有良好的重现性、可逆性和选择性 ,其它常见阴离子和阳离子不干扰测定。本方法用来直接测定合成水样中的苦味酸及间接测定药物辛可宁的含量 。

树脂相分光光度法测定水中痕量苦味酸

建立了树脂相分光光度法测定水中痕量苦味酸的新方法。该法灵敏度高,表观摩尔吸光系数为1.08×105L/(mol·cm);精密度理想(测定苦味酸质量浓度为5μg/mL的实验5次,相对标准偏差为1.0%);线性范围为0～7.0μg/mL;以3σ衡量,检出限为0.14μg/mL;加标回收率为97%～103%。采用该法直接测定水样中的苦味酸、间接测定烟草中的烟碱,结果令人满意。

苦味酸晶体及分子结构的研究

采用蒸发法制备苦味酸的单晶。用X射线衍射、元素分析、红外光谱对其进行了结构表征。苦味酸晶体属正交晶系 ,Pca2 (1)空间群。晶体参数为 :a =0 .92 6 84(16 )nm ,b =1.913 9(4)nm ,c =0 .9716 (2 )nm ,V =1.72 3 6 (6 )nm3,Z =4,Dc=1.76 6g·cm-3 ,μ =1.6 6cm-1,F(0 0 0 ) =92 8。最终偏离因子R =0 .0 45 4,Rw=0 .0 979。

4-氨基-1,2,4-三唑苦味酸盐的合成与性能

以4-氨基-1,2,4-三唑和苦味酸为原料合成了含能化合物4-氨基-1,2,4-三唑苦味酸盐(4-ATPA),其结构经元素分析、FTIR、MS和1HNMR表征。在甲醇和乙醇溶液中获得了两种不同显微形貌的4-ATPA晶体,SEM分析表明,它们分别为长柱形和椭球形,XRD及DSC分析表明它们的晶型相同。X射线单晶衍射计算得到晶体密度为1.720g/cm3。经测定,4-ATPA的部分热性能及机械感度为:熔点195.26℃,400℃下不分解,真空安定性实验(VST)0.16mL.g-1(120℃,48h),失重(TG)0.14%(120℃,48h);撞击感度为4%、摩擦感度为0%(90°)、特性落高H50=87.4cm(5kg落锤),均优于TNT,静电火花感度V50=3.909kV,E50=0.233J,与环三亚甲基三硝胺(RDX)相当,5s爆发点360℃,1000s临界温度251℃。结果表明:4-ATPA有良好的综合热稳定性和较低的机械感度,是一种综合性能优良的炸药。