水中乙醛、丙烯醛和丙烯腈3种测定方法的对比

对比研究了大体积直接进样填充柱气相色谱法、顶空-气相色谱法和吹扫捕集-气相色谱法等3种测定水中乙醛、丙烯醛和丙烯腈的方法.结果表明,大体积直接进样法设备简单,但手动进样耗力费时,且灵敏度低,精密度差,直接水样分析易影响色谱柱和检测器的使用寿命;顶空法稳定性好,线性范围宽,相关性和精密度好,适合较高浓度水样的分析;吹扫捕集法操作简便,峰形好,检出限低,回收率高,适合低浓度水样的分析.顶空法和吹扫捕集法自动化程度高,均适用于大批量样品分析.     

Acetaldehyde residue in polyethylene terephthalate (PET) bottles

A simple sample preparation technique was developed for rapid analysis of acetaldehyde residue in Polyethylene Terephthalate (PET) bottles. A laboratory-built heating system was used and coupled with gas chromatography-flame ionization detector (GC-FID) at optimized conditions. The results were a tremendous reduction of the sample preparation time from 24 hours, for the conventional method, to only one hour. The analysis took only 1.5 min with other good analytical performances i.e. a low detection limit, 0.3 ng mL^{? 1} and a wide linear dynamic range, 0.3 ng mL^{? 1} to 6.6 μ g mL^{? 1} with R² > 0.99.Acetaldehyde residue in freshly blown bottles were analyzed and found in the range of 0.4 to 1.1 ng mL^{? 1}. The results were good agreement with the conventional 24-hour airspace method (P < 0.01). The PET-bottle sampling technique was also developed to minimize the complication of sample transportation and pre-concentration. A purge and trap technique was found to be the most suitable. Then, it was implemented and compared, the results showed no significant difference (P < 0.01) with and without purge and trap.     

催化燃烧法处理聚酯工艺废气的实践

探索研究使用催化燃烧方法处理聚酯生产工艺废气的可行性，并在生产装置上进行了中试。试验结果证明，使用催化燃烧法处理效果好，不产生二次污染，处理后的废气可达标排放。     

仪化废水中乙醛污染的调查

通过对中国石化仪征化纤股份有限公司（以下简称仪化公司）排放废水中乙醛污染的调查，表明仪化公司排放的含乙醛废水主要产生于聚酯生产过程中的工艺废水，喷淋废水，冲洗地面和其他跑、冒、滴、漏的废水（“清下水”）。1996年－2000年污水处理场日排放含乙醛废水约5.66万t，日排放含乙醛的“清下水”约3万t。排放的乙醛在长江仪征段未检出，在沿山河和胥浦河水中有不同程度的检出和超标，超标率分别为50％和9.1%，最大超标倍数分别为8.88倍和0.14倍。对长江仪征段乙醛污染的影响预测结果为：污水处理场在非正常处理情况下（即直排），其排放的废水将在排污口周围形成长1250m，宽200m的污染带，污染面积为25万m^2。     

Carbonyls in the metropolitan area of Mexico City: calculation of the total photolytic rate constants Kp(s(-1)) and photolytic lifetime (tau) of ambient formaldehyde and acetaldehyde

A great number of studies on the ambient levels of formaldehyde and other carbonyls in the urban rural and maritime atmospheres have been published because of their chemical and toxicological characteristics, and adverse health effects. Due to their toxicological effects, it was considered necessary to measure these compounds at different sites in the metropolitan area of Mexico City, and to calculate the total rate of photolytic constants and the photolytic lifetime of formaldehyde and acetaldehyde. Four sites were chosen. Sampling was carried out at different seasons and atmospheric conditions. The results indicated that formaldehyde was the most abundant carbonyl, followed by acetone and acetaldehyde. Data sets obtained from the 4 sites were chosen to calculate the total rate of photolysis and the photolytic lifetime for formaldehyde and acetaldehyde. Maximum photolytic rate values were obtained at the maximum actinic fluxes, as was to be expected.     

大气乙醛碳同位素分析方法的研究

利用气相色谱/燃烧/同位素比值质谱(GC/C/IRMS)分析技术,采用NaHSO3与半胱胺衍生化方法,测定了气态乙醛在衍生化反应过程中的碳同位素效应,探讨了采用该方法测定大气乙醛碳同位素组成的可行性。试验测定了乙醛、衍生剂半胱胺及相应衍生物的碳同位素比值,结果表明,乙醛衍生物的δ13C测量值与理论值的偏差范围为0.11‰～0.35‰,在仪器精密度范围内(<0.50‰),即在衍生化过程中基本不会发生碳同位素分馏。采用该方法初步测定了大气中乙醛的碳同位素组成,实测数据显示,广州地化所和肇庆鼎湖山大气乙醛δ13C平均值分别为(-34.21±0.27)‰和(-31.23±0.16)‰,相同采样点的大气乙醛碳同位素组成基本不变,可见该方法可作为研究大气乙醛不同排放源的一种有效方法。     

顶空气相色谱法测定地表水中的乙醛

建立了顶空气相色谱法测定地表水中乙醛的方法,并对顶空进样条件进行了优化。方法精密度为5％～8％．加标回收率为93％～102％,检测限为0．03mg／L。方法简便、可靠,适用于地表水中乙醛的测定。     

吹扫捕集-气相色谱法同时测定水中的乙醛、丙烯醛和甲醛

研究了吹扫捕集-气相色谱法同时测定水中乙醛、丙烯醛和甲醛的方法并优化了实验条件.实验结果表明,该方法操作简便,灵敏高效,目标化合物的检出限分别为0.037、0.012、0.0006mg/L,相对标准偏差在3.9％ ～15.8％之间,实际水样的加标回收率在73.0％ ～118％之间,能很好满足《地表水环境质量标准》中相关项目的要求.     

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%。     

Catalytic liquid-phase oxidation of acetaldehyde to acetic acid over a Pt/CeO2–ZrO2–SnO2/γ-alumina catalyst

Pt/CeO₂–ZrO₂–SnO₂/γ-Al₂O₃ catalysts were prepared by co-precipitation and wet impregnation methods for catalytic oxidation of acetaldehyde to acetic acid in water. In the present catalysts, Pt and CeO₂–ZrO₂–SnO₂ were successfully dispersed on the γ-Al₂O₃ support. Dependences of platinum content and reaction time on the selective oxidation of acetaldehyde to acetic acid were investigated to optimize the reaction conditions for obtaining both high acetaldehyde conversion and highest selectivity to acetic acid. Among the catalysts, a Pt(6.4 wt.%)/Ce_0.68Zr_0.17Sn_0.15O_2.0(16 wt.%)/γ-Al₂O₃ catalyst showed the highest acetaldehyde oxidation activity. On this catalyst, acetaldehyde was completely oxidized after the reaction at 0°C for 8 hr, and the selectivity to acetic acid reached to 95% and higher after the reaction for 4 hr and longer.