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

An empirical model for COD removal in a biological aerated filter （BAF） in the presence of 2,4,6-trinitrophenol （TNP） was developed, which related effluent COD to influent COD or hydraulic loading rate along the bed height. The overall reaction rate for substrate biodegradation could be described as pseudo first order. The experimental data of COD removal against reactor height were used to calculate the parameters in the empirical model. The COD concentration at different reactor height was expressed as a function of influent COD concentration and hydraulic loading rate, ln（C0/C）=0.124H/QC0^0.77 and ln（C/C0）=-5.63H/L^0.94, respectively, under the experimental condition. The models may be used to predict the COD removal profiles along the reactor height at different hydraulic loading rates and influent COD concentration for design, selection and sizing of BAF.

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.

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.

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.

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.

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 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.

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。

甲午战争中日海军舰炮弹药技术优劣研究

在事关中日国运的甲午战争黄海大东沟海域遭遇战中,北洋海军的舰炮架退炮偏多,速射炮偏少,且弹药技术落后,使用黑火药填充、使用黑火药钝化成的栗色药发射。日本海军大量装备英国阿摩斯壮式速射炮,并使用威力更大的混装爆裂药和黑火药的炮弹,舰炮主弹为填装苦味酸爆裂药、带有引信的穿甲弹,使用无烟药发射。海军装备技术决定国运的兴衰,中日海军舰炮弹药技术代差明显,日本海军装备胜出一筹并在海战中起到制胜作用。黄海海战结束后,北洋舰队屡战屡败而最终覆灭,晚清也失去了制海权。

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。

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。

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%。

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。

超高效亲水作用色谱-串联质谱法检测水中的苦味酸及苦氨酸

建立了一种超高效亲水作用色谱-串联质谱检测水中苦味酸及其降解产物苦氨酸的方法。采用 Acquity UP-LC BEH HILIC亲水作用色谱柱（100 mm＆#215;2.1 mm，1.7μm，Waters）分离，用电喷雾电离串联质谱检测。地表水样品经过0.2μm滤膜过滤之后即可直接进样，加标回收率达89％~107％；废水样品通过固相萃取（ SPE）净化后进样分析，加标回收率达72％~101％。方法重复性的相对标准偏差为4.9％~14.7％。本方法对苦味酸和苦氨酸的检出限分别为0.1μg/L和0.3μg/L。此方法快速、准确，特异性强，灵敏度高，样品前处理方法简便易行，适用于地表水、废水样品的检测。

6种基于血肌酐的肾小球滤过率估算公式在健康人群中的应用评估

目的评价基于酶法和苦味酸速率法的血清肌酐的6种估算的肾小球滤过率（eGFR）公式在表观健康人群中的适用性。方法从健康体检人群中筛选出694名表观健康人，分别用酶学方法和碱性苦味酸速率法检测血清肌酐，通过6种eGFR公式[Cockcroft—Gault（C—G）公式、简化肾脏病膳食改善（MDRD）公式、MDRD-中国人公式、同位素稀释质谱法（IDMS）-MDRD公式、慢性肾脏病流行病合作组（CKD-EPI）公式和EPI-亚洲人（EPI-Asian）公式]分别计算其eGFR并进行比较。结果694名表观健康人群的血肌酐检测结果分别为酶法（65．8±13．3）μmolfL（范围为36～117μmol／L），苦味酸速率法（83．0±12．7）μmol／L（范围为57～131μmol／L）。以eGFR值男性85—125mL／min、女性75—115mL／min作为参考区间，基于酶法检测肌酐的eGFR值在表观健康人群中的适用性依次为CKD—EPI公式（72．3％）〉IDMS—MDRD公式（69．9％）〉简化MDRD公式（61．3％）〉EPI—Asian公式（60．7％）〉C—G公式（54．8％）〉MDRD一中国人公式（27．3％）（P〈0．05），IDMS—MDRD公式在男、女性之间的适用性差异最小（仅相差1．6％）；基于苦味酸速率法检测肌酐的eGFR值在表观健康人群中的适用性依次为MDRD一中国人公式（80．0％）〉EPI—Asian公式（70．1％）〉CKD—EPI公式（63．8％％）〉简化MDRD公式（59．1％）〉C—G公式（52．4％）〉IDMS—MDRD公式（40．7％）（P〈0．05），MDRD-中国人公式在男、女性之间的适用性差异最小（仅相差1％）。结论以上6种eGFR公式计算结果有明显差异。如果用溯源至IDMS的酶法检测血清肌酐，可选用CKD—EPI公式、IDMS—MDRD公式来评价中国北方健康人群的eGFR；如果用苦味酸速率法检测血清肌酐，可选用MDRD-中国人公式来评价中国北方健康人群的eGFR。