环境中臭氧的被动采样—仪器分析方法研究
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摘要
目前,对于环境中多种污染气体的采集和检测,已经有过很多研究报道,但是臭氧作为环境中存在但含量又相对较少的气体,相关的采集和检测研究还相对较少,尤其是在博物馆环境中。本文主要针对博物馆环境中的臭氧气体进行采样方法和检测方法的研究。以无动力扩散采样的方式,对样品的检测分别采用分光光度法与离子色谱法。
对于分光光度法,在原有国标GB/T18204.27-2000的基础上进行了适当的改进。对臭氧采用被动采样的方式,使用了溶解性更好的靛蓝二磺酸钾作为吸收液的主要成分。并且考察了空白的保存、采样重复性及不同材质滤网对采样结果的影响等因素。与国标的主动采样法进行对比,获得了“被动采样-分光光度”法对臭氧的吸收系数aIDS=0.219×10-3(m3/h)。使得被动采样法检测到的气体浓度可以转化成实际空气中臭氧的浓度,体现了该方法的应用价值。
对于离子色谱法,在前人已经建立的仪器条件的基础上,选择了Dionex-320加上RFC-30淋洗液自动发生器,IonPac AS18阴离子色谱柱,梯度淋洗的方式,能够较好地分离实验中存在的所有阴离子。使用被动采样法,创新地设计了一种新的配方,在吸收臭氧的同时也能采集空气中酸性气体——甲酸、乙酸。考察了标样及样品的重复性、12小时内的稳定性、采样的平行性、加标回收率和采样回收率等,确定了检测限与定量限(甲酸根、乙酸根和硝酸根的定量限均在7.0μg/L以下),绘制了采样时间与浓度曲线。与已经成熟的甲酸、乙酸常规检测方法进行对比,证明了使用新型吸收液检测到的酸性气体的含量与之基本吻合。对照国标中主动采样法得到“被动采样-离子色谱”法对臭氧的吸收系数aIC=0.705×10-3(m3/h),与传统臭氧检测方法相比,新开发的方法不仅适用于臭氧气体的检测,还可以同时检测环境中甲酸、乙酸的含量。与此同时对国标中靛蓝二磺酸盐与臭氧的传统反应方程式提出了质疑。
通过上述实验研究,最终确立了一整套检测环境中臭氧气体含量的方法。该方法简单易行,灵敏度高,检测限低,线性较好,具有很高的实际应用价值,为博物馆环境中的气体检测做出了重要的贡献。
Nowadays, there are many research literatures about the collection and detection of various environmental polluting gas, especially, the detection of environmental air quality in museum becomes much more attractive. Ozone, as environment atmosphere gas, although the concentration is relative less, it is important and its collection and detection studies are also little. Here, our investigation (article) mainly aims at the environmental sampling method and testing methods for determining the ozone in the museum air. by using spectrophotometry and ion chromatograpy.
For spectrophotometry, there are appropriate improvements that based on the original GB/T18204.27-2000. With passive sampling, using indigodisulfonate dipotassium salt as the main absorbing matter because of itsbetter stability we study the factors like blank preservation, sampling repeatability and different filter for samplingaffecting the results. Compared with active sampling method according to the national stardand, the passive sampling got the absorption coefficient is aIDS=0.219×10-3(m3/h). The gas concentration which is detected by passive sampling method can be converted into practical ozone concentration in atmosphere, enlarging the value of this method.
For ion chromatography(IC), according to the previous report, Dionex-320 with RFC-30, column IonPac AS 18 and different gradient elution methods were chosen as the instrument conditions, which can provide better anions separation of anions in research. Using passive sampling, our innovation is that the alkaline was added into absorbing liquid, designing an innovative method which can absorb atmosphere ozone and collect the airborne acidic gas (formic acid, acetic acid) at the same time. We investigated the repeatability of standard samples and text samples, respectively. The stability within 12 hours after sampling, the sampling parallel, recovery, sampling recovery etc, determining the limit detection(the limit detection of formic acid, acetic and nitrate all are below 7.0 g/L), getting the curve of sampling time and concentration. Compared with conventional detection methods which used to determin the formic acid and acetic acid, using new absorbing solution to detect acid gas was also feasible. Compared with active sampling method of the national stardand, we got the absorption coefficient of "passive samples-spectrophotometric" is aIC=0.705×10-3(m3/h). Compared with the traditional ozone detection methods, the new method not only suitable for detection of atmosphere ozone but also can monitor environment formic acid and acetic acid. Furthermore,questioned the chemical equation for indigodisulfonate salt and ozone.
Through the above study, a new method to detect the ozone in museum environment was established. The advantages of this method is simple, high sensitivity, low detection limit, good linear and has high practical value, making important contributions for the gas detection in museum environment.
对于分光光度法,在原有国标GB/T18204.27-2000的基础上进行了适当的改进。对臭氧采用被动采样的方式,使用了溶解性更好的靛蓝二磺酸钾作为吸收液的主要成分。并且考察了空白的保存、采样重复性及不同材质滤网对采样结果的影响等因素。与国标的主动采样法进行对比,获得了“被动采样-分光光度”法对臭氧的吸收系数aIDS=0.219×10-3(m3/h)。使得被动采样法检测到的气体浓度可以转化成实际空气中臭氧的浓度,体现了该方法的应用价值。
对于离子色谱法,在前人已经建立的仪器条件的基础上,选择了Dionex-320加上RFC-30淋洗液自动发生器,IonPac AS18阴离子色谱柱,梯度淋洗的方式,能够较好地分离实验中存在的所有阴离子。使用被动采样法,创新地设计了一种新的配方,在吸收臭氧的同时也能采集空气中酸性气体——甲酸、乙酸。考察了标样及样品的重复性、12小时内的稳定性、采样的平行性、加标回收率和采样回收率等,确定了检测限与定量限(甲酸根、乙酸根和硝酸根的定量限均在7.0μg/L以下),绘制了采样时间与浓度曲线。与已经成熟的甲酸、乙酸常规检测方法进行对比,证明了使用新型吸收液检测到的酸性气体的含量与之基本吻合。对照国标中主动采样法得到“被动采样-离子色谱”法对臭氧的吸收系数aIC=0.705×10-3(m3/h),与传统臭氧检测方法相比,新开发的方法不仅适用于臭氧气体的检测,还可以同时检测环境中甲酸、乙酸的含量。与此同时对国标中靛蓝二磺酸盐与臭氧的传统反应方程式提出了质疑。
通过上述实验研究,最终确立了一整套检测环境中臭氧气体含量的方法。该方法简单易行,灵敏度高,检测限低,线性较好,具有很高的实际应用价值,为博物馆环境中的气体检测做出了重要的贡献。
Nowadays, there are many research literatures about the collection and detection of various environmental polluting gas, especially, the detection of environmental air quality in museum becomes much more attractive. Ozone, as environment atmosphere gas, although the concentration is relative less, it is important and its collection and detection studies are also little. Here, our investigation (article) mainly aims at the environmental sampling method and testing methods for determining the ozone in the museum air. by using spectrophotometry and ion chromatograpy.
For spectrophotometry, there are appropriate improvements that based on the original GB/T18204.27-2000. With passive sampling, using indigodisulfonate dipotassium salt as the main absorbing matter because of itsbetter stability we study the factors like blank preservation, sampling repeatability and different filter for samplingaffecting the results. Compared with active sampling method according to the national stardand, the passive sampling got the absorption coefficient is aIDS=0.219×10-3(m3/h). The gas concentration which is detected by passive sampling method can be converted into practical ozone concentration in atmosphere, enlarging the value of this method.
For ion chromatography(IC), according to the previous report, Dionex-320 with RFC-30, column IonPac AS 18 and different gradient elution methods were chosen as the instrument conditions, which can provide better anions separation of anions in research. Using passive sampling, our innovation is that the alkaline was added into absorbing liquid, designing an innovative method which can absorb atmosphere ozone and collect the airborne acidic gas (formic acid, acetic acid) at the same time. We investigated the repeatability of standard samples and text samples, respectively. The stability within 12 hours after sampling, the sampling parallel, recovery, sampling recovery etc, determining the limit detection(the limit detection of formic acid, acetic and nitrate all are below 7.0 g/L), getting the curve of sampling time and concentration. Compared with conventional detection methods which used to determin the formic acid and acetic acid, using new absorbing solution to detect acid gas was also feasible. Compared with active sampling method of the national stardand, we got the absorption coefficient of "passive samples-spectrophotometric" is aIC=0.705×10-3(m3/h). Compared with the traditional ozone detection methods, the new method not only suitable for detection of atmosphere ozone but also can monitor environment formic acid and acetic acid. Furthermore,questioned the chemical equation for indigodisulfonate salt and ozone.
Through the above study, a new method to detect the ozone in museum environment was established. The advantages of this method is simple, high sensitivity, low detection limit, good linear and has high practical value, making important contributions for the gas detection in museum environment.
引文
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