气袋采样法对还原硫化物测定的影响因素分析及机理研究

孟洁; 翟增秀; 刘英会; 张君; 韩萌

doi:10.15898/j.cnki.11-2131/td.201804010034

气袋采样法对还原硫化物测定的影响因素分析及机理研究

Influence Factors and Mechanism Study on Bag Sampling Method for Determination of Reduced Sulfide Compound by Gas Chromatography-Mass Spectrometry

摘要

摘要: 还原硫化物是一Z类典型的恶臭物质，其特点是活性高、不易储存，因此适宜的储存条件对还原硫化物的准确测定具有重要意义。本文使用气相色谱-质谱联用技术，从气袋材质、还原硫化物初始浓度、还原硫化物性质和储存时间四个因素探究袋采样法储存还原硫化物过程的损失情况。以Tedlar^®PVF和Teflon^®FEP为目标采样袋，使用5个初始浓度（0.001、0.010、0.100、1.000和10.000μg/mL）的混合还原硫化物，选择0、2、6、12、24、48以及72h的储存时间，以响应因子和相对回收率作为评价因子，并使用配对t检验法和吸附动力学，研究影响储存效果的主要因素、物质损失机理以及两种采样袋的储存能力。结果表明，储存时间越长、物质初始浓度越高，物质活性越强，损失情况越严重；在环境温度达到60℃时，Tedlar^®PVF的基质背景较Teflon^®FEP更复杂；相同条件下，还原硫化物在Teflon^®FEP储存过程中损失更严重。依据研究结果建议：①样品采集后避光保存；②低浓度含硫样品的测定在采样后8h内完成，高浓度含硫样品的测定在2h内完成；③若待测样品气体温度较高，优先选择Teflon^®FEP采样袋，气体温度较低条件下选择Tedlar^®PVF采样袋，可最大限度保持样品的原始状态。本研究成果有利于确保还原硫化物样品的储存稳定性，最大限度还原恶臭污染现场情况，为恶臭污染的分析测试以及后续的恶臭污染控制与治理提供技术支持。

Abstract:
BACKGROUNDReduced sulfide compound is a typical odorant characterized by high activity and is difficult to store. Therefore, suitable storage conditions are of great significance for the accurate determination of reduced sulfides.
OBJECTIVESTo understand the causes of loss and deterioration of highly active reduced sulfides, and to select the optimal storage conditions.
METHODSGas Chromatography-Mass Spectrometry was used to investigate the loss of the process of storing reduced sulfides by bag sampling from the following four factors, air bag material, initial concentration of reduced sulfide, reduced sulfide property, and storage time. Sample bags, Tedlar^®PVF and Teflon^®FEP, were used as object bags. Using 5 initial concentrations (0.001, 0.010, 0.100, 1.000 and 10.000μg/mL) of mixed reduced sulfides, 0, 2, 6, 12, 24, 48 and 72h as the storage time, using the response factor and relative recovery as the evaluation factor, and using the paired t-test and adsorption kinetics, the main factors affecting the storage effect, the mechanism of material loss and the comparison of the storage capacity of the two sampling bags were studied.
RESULTSThe results show that the longer the storage time, the higher the initial concentration of the substance, and the stronger the activity of the substance, the more serious the loss. When the ambient temperature reaches 60℃, the substrate background of Tedlar^®PVF is more complicated than that of Teflon^®FEP. Under the same conditions, the reduced sulfides are more severely damaged during Teflon^®FEP storage.
CONCLUSIONSIt was suggested that:(1) the reduced sulfide be stored in shad after sampling; (2) analysis should be finished within eight hours and two hours for low and high concentration, respectively; (3) Teflon^®FEP be used at high temperature and Tedlar^®PVF at low temperature. The research results were beneficial to ensure the storage stability of the reduced sulfide samples, minimize the situation of odor pollution, and provide technical support for the analysis of odor pollution and the subsequent control and treatment of odor pollution.

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