广州市大气典型羰基化合物碳同位素组成初探

采用气相色谱/燃烧/同位素比值质谱(GC/C/IRMS)技术,通过2,4-二硝基苯肼(DNPH)衍生化方法,初步测定了广州市城区交通主干线大气中甲醛、乙醛和丙酮的碳同位素组成.结果表明,甲醛的δ13C值变化范围为-42.06‰--33.52‰,乙醛的δ13C值变化范围为-35.84‰--32.20‰,丙酮的δ13C值变化范围为-30.85‰--29.50‰;而且,白天相对于夜晚而言,甲醛、乙醛和丙酮的最大碳同位素分馏分别为6.65‰,3.27‰和0.75‰,碳同位素分馏上的差异表明它们在环境大气中不同化学活性上的差异.     

A Method for Measuring Degradation of Individual Components in Multicomponent Biodegradable Plastics by Fourier Transform Infrared Spectrometry

A new chemometric method based on Beer's law was derived that uses peak ratios from Fourier transform infrared spectra of neat polymers and their composite plastics to quantify degradation of the individual polymers after biodegradation. The method affords direct measurement of polymer concentrations and weight losses without prior calibration against known composites. Unlike traditional chemometric methods, this method does not require sampling of as many or more different composites as the number of polymers in the composite being analyzed. When the neat polymer spectra are known, only two measurements, one before and one after biodegradation, are needed. A potentially major advance is that the method allows automation of analytical infrared wavelength selection by computer from all possible wavelength combinations. In this paper, the theoretical basis and derivation of the mathematical model for multicomponent systems is presented. The validity of the model was proved initially by applying the method to simulated two-polymer and three-polymer composites and finally by comparing test results with known samples of biodegradable composites prepared in the laboratory. Potential future development of the method for more challenging multicomponent plastics is discussed.     

TOA-MIBK萃取火焰原子吸收法同时测定土壤及蔬菜中铅镉

用氢氟酸、硝酸、高氯酸消化土壤样品,干灰化法消解蔬菜样品,用相对TOA-MIBK系统萃取,火焰原子吸收光谱法在同一条件下测定土壤、蔬菜中的铅、镉。在选定条件下,测得土壤铅、镉的相对标准偏差分别为2．3％～4．4％和3．0％～4.3％,蔬菜铅、镉的相对标准偏差分别为2．9％～4．5％和2．6％～4．5％;土壤铅、镉的回收率分别为96％～104％和95％～101％,蔬菜铅、镉的回收率分别为93％～102％92％104％。由测定结果得出离公路越近,蔬菜、土壤铅、镉含量越高。     

洞庭湖及入湖河流中209种多氯联苯同类物分布特征与风险评估

为全面了解洞庭湖水域多氯联苯(PCBs)的污染情况,采用同位素稀释-高分辨质谱法对洞庭湖及入湖河流共21处表层水进行了 209种PCB同类物测定分析结果表明,共检出50种PCB同类物,ρ(∑ PCBs)在0.077～10 ng·L-1之间,平均值为2.7ng·L-1,中值为1.9 ng·L-1,污染浓度为:入湖河流＞湖...     

固相萃取-超高压液相色谱-串联质谱法测定海水中16种磺胺类抗生素残留

利用固相萃取前处理方法,净化和富集海水中的16种磺胺类抗生素,采用超高压液相色谱-串联质谱法进行定性和定量检测,建立了完整的海水中磺胺类抗生素的检测方法,并对质谱条件、液相条件和固相萃取条件进行了优化。实验结果表明,16种磺胺类抗生素在0.1～100μg/L质量浓度范围内线性良好,相关系数均可以达到0.996以上,方法检出限为0.3~1.1 ng/L。对水样进行高、中、低3个质量浓度的加标回收实验,回收率分别为82.3%~125.7%,73.3%~125.1%和75.2%~119.2%,相对标准偏差为2.4%~12.0%。该方法具有操作简便、重现性好、灵敏度高的优点,可用于海水中磺胺类抗生素的监测分析。     

Application of ultrasonic to speciation analysis of heavy metals in soil

In order to reduce the operation time and improve the extraction efficiency, ultrasonic energy by means of ultrasonic bath was used to the modified Tessier sequential extraction for speciation analysis of heavy metals in soil. Extractable contents of Cu, Fe, Mn, Ni,Pb and Zn were measured by atomic absorption spectroscopy(hAS). The merit of the ultrasonic extraction (UE) applied to the modified Tessier method is not only that the operation time for the first 4 fractions was reduced from ca. 18 h to 8 h, comparing with conventional extraction(CE), but also the extraction efficiency was higher. The results for both of UE and CE were consistent. The extractable Cu, Ni and Zn in the sample No. 1 were mainly associated with the third fraction (Fe-Mn oxides fraction), and fourth fraction (organic matter fraction) in the sample No.2. The extractable Fe and Mn were all mainly associated with the third fraction, and Pb the fourth fraction in both of the samples. The effects of concentration of hydroxylamine chloride on the capability for the extraction of studied metals were also studied.     

Absorption cross-sections of atmospheric constituents: NO2, O2, and H2O

Absorption spectroscopy, which is widely used for concentration measurements of tropospheric and stratospheric compounds, requires precise values of the absorption cross-sections of the measured species. NO₂, O₂ and its collision-induced absorption spectrum, and H₂O absorption cross-sections have been measured at temperature and pressure conditions prevailing in the Earth’s atmosphere. Corrections to the generally accepted analysis procedures used to resolve the convolution problem are also proposed.     

一种新的真空冷原子吸收法测定汞

本文建立了真空冷原子吸收光谱技术测定汞的一种方法。在负压下用ＮａＢＨ４将酸性溶液中Ｈｇ（Ⅱ）离子还原成为金属汞。在室温下使用真空泵将基态汞原子直接吸入到真空石英炉内。本法给出了改善的灵敏度,检出限（３σ）是０．０６ｎｇ。重复１０次测定０．５ｎｇ汞,方法的相对标准偏差是３．０％,将本法应用到测定水系沉积物标准样品中汞的含量,分析结果是令人满意的。     

萃取－同步荧光光谱法测定大气飘尘中苯并(a)芘

提出用浓Ｈ２ＳＯ４从大气飘尘样品的环己烷提取液中一次萃取后,用同步荧光光谱测定苯并（ａ）芘的方法,选用△λ为２０ｎｍ时可获最佳效果,用浓硫酸萃取的时间仅１ｍｉｎ,苯并（ａ）芘在浓硫酸相中１ｈ内稳定,样品加标的回收率为８５％,其它多环芳烃化合物在５３０－６００ｎｍ的测定波长范围不干扰苯并（ａ）芘的测定,用乙酰化滤纸层析－荧光分光光度的统一方法作为对比对实际样品进行了测定,结果与后者的偏差在±１５％以     

引滦水中天然有机化合物的形态及紫外吸收特征

用改进的Leenheer法将引滦水中的天然有机化合物分离为悬浮态和溶解态两大类,后者又分离成憎水有机物、腐殖酸类、强阴离子化合物和其它亲水化合物4种。溶解态有机物含量在4—5mgC/L之间,其中半数左右为腐殖酸类,其紫外吸收强度远在其它形态之上。非极性憎水有机物在5％以下。