液-液萃取-气相色谱法同时测定水中吡啶、松节油和苯胺

研究建立了气相色谱法同时测定水中吡啶、松节油和苯胺的方法.采用二氯甲烷萃取,萃取后直接进行色谱分离分析,3种物质能够有效分离.吡啶、松节油和苯胺的水中最低检测浓度分别为0.009、0.009、0.004mg/L,样品添加平均回收率为89％～114％,平行6次精密度实验,相对标准偏差小于6.5.实验结果表明,气相色谱法简单、快速、准确,适用于水中吡啶、松节油和苯胺的测定.     

Insights into simultaneous anammox and denitrification system with short-term pyridine exposure: Process capability,inhibition kinetics and metabolic pathways

• Short-term effect of the pyridine exposure on the SAD process was investigated. • The SAA at 150 mg/L pyridine reduced by 56.7% of the maximum value. • Inhibition kinetics models and inhibitory parameters were indicated. • Collaboration of AnAOB, HDB and PDB promoted the SAD. • Possible metabolic pathways of nitrogen and pyridine were proposed. In-depth knowledge on the role of pyridine as a bottleneck restricting the successful application of anammox-based process treating refractory coking wastewater remains unknown. In this study, the effect of short-term pyridine addition on a simultaneous anammox and denitrification (SAD) system fed with 25–150 mg/L pyridine was explored. The short-term operation showed that the highest total nitrogen (TN) removal efficiency was achieved at 25–50 mg/L of pyridine. As the pyridine addition increased, the contribution of the anammox pathway in nitrogen removal decreased from 99.3% to 79.1%, while the denitrification capability gradually improved. The specific anammox activity (SAA) at 150 mg/L pyridine decreased by 56.7% of the maximum SAA. The modified non-competitive inhibition model indicated that the 50% inhibitory concentration (IC₅₀) of pyridine on anammox was 84.18 mg/L and the substrate inhibition constant (K_i) of pyridine for self-degradation was 135.19 mg/L according to the Haldane model. Moreover, high-throughput sequencing confirmed the abundance of Candidatus Kuenenia as the amount of anammox species decreased, while the amounts of denitrifiers and pyridine degraders significantly increased as the pyridine stress increased. Finally, the possible pathways of nitrogen bioconversion and pyridine biodegradation in the SAD system were elucidated through metagenomic analysis and gas chromatography/mass spectrometry results. The findings of this study enlarge the understanding of the removal mechanisms of complex nitrogenous pyridine-containing wastewater treated by the SAD process.     

气相色谱法测定环境空气中吡啶

建立了用气相色谱法测定环境空气中吡啶的方法。环境空气中吡啶活性炭吸附,二硫化碳解吸,DB-200毛细管柱分离,直接进样分析,氢火焰离子化检测器检测,时间定性,峰面积定量,吡啶回收率为91．5％～103．1％,当采样体积为20L,吡啶最低检出质量浓度分别为0．006mg/m 3。本方法前处理简便,分离度好,分析灵敏度高,满足环境分析要求。     

污泥驯化和共代谢对吡啶和苯降解特性的研究

利用瓦氏呼吸仪测定微生物耗氧量的方法,研究了焦化废水及其中难降解有机污染物吡啶、苯的降解特性,并对吡啶和苯分别与苯酚共基质条件下的可生化性进行了研究。结果表明,pH值为7.2时,焦化废水降解率最高;当浓度小于40mg/L时,吡啶和苯可以部分被降解,浓度大于60mg/L时微生物呼吸作用明显地被抑制;污泥驯化有利于有机污染物降解速率的提高。初步分析了共代谢降解焦化废水中难降解有机污染物的生理生化特性。     

固相微萃取技术测定水中的吡啶与静态顶空方法的比较

用固相微萃取技术(SPME)及静态顶空(SHS)分别与气相色谱联用来分析水中的吡啶。通过试验确定了固相微萃取的分析参数:纤维萃取头、吸附时间、解吸时间、无机盐浓度,并与静态顶空方法作了比较。以同一浓度的标准溶液来分析两种方法的检出限、线性及重复性。结果表明,两种方法都具有很好的重复性和线性,固相微萃取的RSD在0.9%～3.1%之间,静态顶空的RSD在0.7%～3.6%之间。两种发方法的标准曲线相关系数也都在0.999以上。但是固相微萃取技术的检出限比静态顶空法低很多。固相微萃取方法测定水中吡啶的检出限是0.001mg/L,而静态顶空法的检出限只有0.03 mg/L。因此,测定水中的吡啶,使用固相微萃取技术优于静态顶空法。     

GDX 502管吸附-二氯甲烷解吸-气相色谱法测定气中的吡啶

建立了GDX 502管吸附-二氯甲烷解吸-气相色谱测定气中吡啶的方法,考察吸附管类型、解吸溶剂、解吸溶剂体积、采样时间和采样流量对测定结果的影响。结果表明,气中吡啶用GDX 502吸附管以0. 5 L/min的流量采样20 min,二氯甲烷解吸至1 m L,DB-1 (30 m×250μm×0. 25μm)柱分离,空白样品低、中、高3种加标量回收率为90. 8%～108%(n=6),相对标准偏差为2. 9%～4. 4%,方法在0～19. 6 mg/L线性范围内响应良好,相关系数(r)=0. 999 9。当采样体积为10 L时,检出限为0. 01 mg/m~3。该方法重复性好、回收率高、干扰较小,能够满足空气和废气中吡啶分析的要求。     

吹扫捕集-气相色谱/质谱法测定水中的乙醛、丙烯醛、丙烯腈和吡啶

水中的乙醛、丙烯醛、丙烯腈和吡啶经吹扫捕集、解吸后,用HP-VOC毛细管色谱柱进行GC分离,用GC-MS法选择离子模式(SIM)下进行检测,外标法定量。结果表明,选择取样量25 m L,吹扫流量为40 m L/min,吹扫温度为40℃,吹扫时间为15 min,解吸时间为2 min,解吸温度为200℃,烘焙时间20 min,乙醛和吡啶质量浓度在0.025~0.60 mg/L之间,丙烯醛和丙烯腈质量浓度在0.002 5~0.10 mg/L之间时,校准曲线呈线性关系,相关系数r0.995,乙醛、丙烯醛、丙烯腈和吡啶的方法检出限分别为0.001 6,0.001 3,0.000 5和0.002 1 mg/L。对3个不同浓度样品进行空白加标实验,测量的回收率为87.8%~114.3%,相对标准偏差(n=6)为2.51%~10.4%。对3批实际水样进行分析,其中一个废水水样加标回收率为79.2%~103.8%,相对标准偏差(n=6)为3.04%~6.39%。     

去除水中全氟辛基磺酸的纳米吸附剂的制备及性能表征

实验研究了去除水中全氟辛基磺酸(PFOS)的纳米吸附剂的制备方法,并对其性能进行表征.研究结果表明:单体(4-乙烯基吡啶)含量对吸附剂去除PFOS的效果影响显著;而聚合状态、聚合液含水率、有机溶剂和交联剂的种类仅对吸附剂形态和比表面积有一定影响,但对吸附剂去除PFOS的效果影响不大.红外光谱揭示了单体和交联剂的有效聚合,ζ电位的测定则证实了单体和PFOS是由于静电作用而结合.     

Peroxymonosulfate activation by Fe-N-S co-doped tremella-like carbocatalyst for degradation of bisphenol A: Synergistic effect of pyridine N, Fe-Nx, thiophene S

Bisphenol A (BPA) has received increasing attention due to its long-term industrial application and persistence in environmental pollution. Iron-based carbon catalyst activation of peroxymonosulfate (PMS) shows a good prospect for effective elimination of recalcitrant contaminants in water. Herein, considering the problem about the leaching of iron ions and the optimization of heteroatoms doping, the iron, nitrogen and sulfur co-doped tremella-like carbon catalyst (Fe-NS@C) was rationally designed using very little iron, S-C₃N₄ and low-cost chitosan (CS) via the impregnation-calcination method. The as-prepared Fe-NS@C exhibited excellent performance for complete removal of BPA (20 mg/L) by activating PMS with the high kinetic constant (1.492 min⁻¹) in 15 min. Besides, the Fe-NS@C/PMS system not only possessed wide pH adaptation and high resistance to environmental interference, but also maintained an excellent degradation efficiency on different pollutants. Impressively, increased S-C₃N₄ doping amount modulated the contents of different N species in Fe-NS@C, and the catalytic activity of Fe-NS@C-1-x was visibly enhanced with increasing S-C₃N₄ contents, verifying pyridine N and Fe-N_x as main active sites in the system. Meanwhile, thiophene sulfur (C-S-C) as active sites played an auxiliary role. Furthermore, quenching experiment, EPR analysis and electrochemical test proved that surface-bound radicals (^·OH and SO₄^⋅−) and non-radical pathways worked in the BPA degradation (the former played a dominant role). Finally, possible BPA degradation route were proposed. This work provided a promising way to synthesize the novel Fe, N and S co-doping carbon catalyst for degrading organic pollutants with low metal leaching and high catalytic ability.     

Simultaneous pyridine biodegradation and nitrogen removal in an aerobic granular system

Simultaneous pyridine biodegradation and nitrogen removal were successfully achieved in a sequencing batch reactor(SBR) based on aerobic granules. In a typical SBR cycle, nitritation occurred obviously after the majority of pyridine was removed, while denitrification occurred at early stage of the cycle when oxygen consumption was aggravated. The effect of several key operation parameters, i.e., air flow rate, influent NH_4~+-N concentration,influent p H and pyridine concentration, on nitritation, pyridine degradation and total nitrogen(TN) removal, was systematically investigated. The results indicated that high air flow rate had a positive effect on both pyridine degradation and nitritation but a negative impact of overhigh air flow rate. With the increase of NH_4~+ dosage, both nitritation and TN removal could be severely inhibited. Slightly alkaline condition, i.e., pH 7.0–8.0, was beneficial for both pyridine degradation and nitritation. High pyridine dosage often resulted in the delay of both pyridine degradation and nitritation. Besides, extracellular polymeric substances production was affected by air flow rate, NH_4~+ dosage, pyridine dosage and p H.In addition, high-throughput sequencing analysis demonstrated that Bdellovibrio and Paracoccus were the dominant species in the aerobic granulation system. Coexistence of pyridine degrader, nitrification related species, denitrification related species, polymeric substances producer and self-aggregation related species was also confirmed by highthroughput sequencing.