张丽楠, 张淼, 任海燕, 蒲攀, 孔盼. Superfloc127用于电极法测定土壤硝态氮含量的可行性分析[J]. 农业工程学报, 2015, 31(z1): 196-204. DOI: 10.3969/j.issn.1002-6819.2015.z1.023
    引用本文: 张丽楠, 张淼, 任海燕, 蒲攀, 孔盼. Superfloc127用于电极法测定土壤硝态氮含量的可行性分析[J]. 农业工程学报, 2015, 31(z1): 196-204. DOI: 10.3969/j.issn.1002-6819.2015.z1.023
    Zhang Linan, Zhang Miao, Ren Haiyan, Pu Pan, Kong Pan. Feasibility of rapid detection of soil nitrate-nitrogen content using Superfloc127 in ion-selective electrode[J]. Transactions of the Chinese Society of Agricultural Engineering (Transactions of the CSAE), 2015, 31(z1): 196-204. DOI: 10.3969/j.issn.1002-6819.2015.z1.023
    Citation: Zhang Linan, Zhang Miao, Ren Haiyan, Pu Pan, Kong Pan. Feasibility of rapid detection of soil nitrate-nitrogen content using Superfloc127 in ion-selective electrode[J]. Transactions of the Chinese Society of Agricultural Engineering (Transactions of the CSAE), 2015, 31(z1): 196-204. DOI: 10.3969/j.issn.1002-6819.2015.z1.023

    Superfloc127用于电极法测定土壤硝态氮含量的可行性分析

    Feasibility of rapid detection of soil nitrate-nitrogen content using Superfloc127 in ion-selective electrode

    • 摘要: 样本前处理是影响离子选择电极测土时效性的关键环节。以缩短静置时间为目的,该文探讨了高分子絮凝剂Superfloc127用于土壤硝态氮浸提前处理操作的可行性。首先,基于相界电位模型对Superfloc127加入土样硝态氮浸提液后电极反应动力学过程进行建模分析,理论可行性验证后,开展测土试验,分析其对自制全固态电极(PPy-NSISE)及商用电极(PVC-NISE)电化学性能的影响。结果表明:使用Superfloc127后,样本制备时间由1.5 h缩短至10 s;PPy-NSISE及PVC-NISE响应斜率分别为-51.4和-52.1 mV/Decade,检测灵敏度无明显改变,测土结果与标准结果之间的决定系数分别为0.69和0.31;连续测定12 h后,PPy-NSISE和PVC-NISE的响应斜率分别降低至-35.1和-25.4 mV/Decade,性能不可恢复。通过理论解析及大量分析试验证明,絮凝剂Superfloc127无法应用在基于离子选择电极法的土壤硝态氮快速分析,提高土壤前处理效率的研究工作仍需深入开展。

       

      Abstract: Abstract:Sample pretreatment is one of the key steps for soil nutrient analysis. It greatly affects the detection efficiency of Ion-selective electrode (ISE) based soil nitrate-nitrogen (NO3--N) detection. Aiming at shortening the standing time, the polymer flocculant Superfloc127, one of conventional non-ionic polyacrylamide chemicals, was reported to be applied in sample pretreatment of soil detections based on the ultraviolet-visible spectrophotometry (UV-VIS). In this study, the feasibility of employing Surperfloc127 into the soil NO3--N rapid detection by using ISE was discussed. First, the theoretical analysis of the dynamic electrode process was conducted under the stationary-state conditions, which described the assumed electrochemical equilibrium of the ionic exchange, ionic flux and ionic co-extraction under zero current condition in artificial nitrate solution. A phase boundary potential model was built to prove the ignorable influences produced by Superfloc127 on the solvent polymeric ISE with the inner filling solution. The calculated results of the phase boundary potential model showed that less degradation of the linear detection ranges (LDR) was observed when Superfloc127 was added into the nitrate sample. Theoretically, Superfloc127 was demonstrated acceptable influences on the performance of nitrate ISE. And then, soil samples was prepared to further verify the applicability of Superfloc127. Soil testing was carried out by the self-developed PPy (NO3--N)-membrane nitrate solid-state ISE (PPy-NSISE) and the commercial PVC-membrane nitrate ISE (PVC-NISE). The previous developed soil macronutrient automatic detecting stand was integrated for the measurements throughout the whole study. The effects of Superfloc127 on the performances of PPy-NSISE and PVC-NISE were evaluated by comparing the response sensitivities in standard nitrate solutions. The concentrations of superfloc127 were artificially controlled to 0, 25, 50 and 75 mg/L. 10 soils covering 4 different types were selected. Each soil was divided into three sets. Soil set1 was measured with ultraviolet spectrophotometry. Soil set2 was pretreated without Superfloc127 and analyzed by the ISEs. Soil set3 was pretreated with Superfloc127 and analyzed with the ISEs. Results showed that the standing time, which represented the duration from the ending instant of the shaking process to the instant of obtaining transparent soil extracts, was enormously shortened from 1.5h to 10s by the addition of Superfloc127. The PPy-NSISE and the PVC-NISE produced good sensitivities with the response slopes of -51.4 and -52.1 mV/decade. Neglectable influence made by Superfloc127 was observed on the changes of sensitivities of PPy-NSISE and PVC-NISE. The determination coefficient (R2) of linear regression between ISEs based soil NO3--N measurements and the UV-VIS results were 0.69 and 0.31 for PPy-NSISE and PVC-NISE, respectively. After continuous determination of 12h, the absolute response slopes of the PPy-NSISE and the PVC-NISE were reduced to 35.1 and 25.4 mV/decade. Moreover, the ISE performance couldn’t be recovered even by the re-activation process. In summary, Superfloc127 could greatly improve the efficiency of soil pretreatment. But it will fasten the ISE deteriorating promptly. Therefore, it was not recommended to use Superfloc127 in ISE based soil NO3--N detection. Researches should be carried out to clarify the mechanism of Superfloc127. The attempts of enhance the pretreatment efficiency of ISE based soil detection were greatly encouraged.

       

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