CN110806400B - 一种减小土壤含水率对多环芳烃荧光工作曲线影响的校正方法 - Google Patents
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Abstract
本发明属于检测方法领域,涉及土壤内多环芳烃的检测,尤其是一种减小土壤含水率对多环芳烃荧光工作曲线影响的校正方法,包括如下步骤,步骤1:选取多个不同含水率的土壤样本,并针对土壤样本制备多个不同浓度多环芳烃的土壤样品;步骤2:建立相应多环芳烃浓度矩阵C;步骤3:扫描土壤样品制备荧光谱和近红外漫反射光谱;步骤4:选定定量荧光谱带M;步骤5:选定近红外漫反射光谱带N;步骤6:得到相应荧光强度矩阵F;步骤7:得到相应近红外漫反射强度矩阵S;步骤8:得到每个土壤样品的校正荧光强度矩阵Fc;步骤9:建立校正工作曲线。
Description
技术领域
本发明属于检测方法领域,涉及土壤中多环芳烃的检测,尤其是一种减小土壤含水率对多环芳烃荧光工作曲线影响的校正方法。
背景技术
众所周知,多环芳烃(PAHs)具有致癌性,而土壤作为一种重要的环境介质,多环芳烃污染问题尤为严重,严重影响了土壤的可持续发展,就需要修复和治理,但前提是需要明确土壤中多环芳烃的分布和浓度。目前对于土壤中PAHs,主要采用气相、液相、气质联用等方法,但这些方法多是将土壤样品经过复杂的前处理进行分离提纯,再进行分析,操作繁琐,且需要大量的有机试剂,费时费力,且不能保证将PAHs全部抽提出来,不能满足全面普查、动态监测土壤污染状况的需求。因此,开发一种便捷、快速土壤中PAHs的检测方法已成为环保和农业部门亟需解决的重大问题之一。
荧光光谱技术由于灵敏度高、选择性好,可实现快速、现场检测等优点,已经被广泛应用于土壤中多环芳烃的检测。中国发明专利申请公开号CN106442447 A公开了一种减小土壤粒径对多环芳烃工作曲线的影响,通过瑞利散射光强度实现土壤粒径对PAHs荧光强度影响的有效校正。本发明是针对土壤粒径对PAHs荧光的影响,提出并建立一种减小土粒径对PAHs荧光工作曲线的校正方法。
但除土壤粒径外,土壤含水率等因素也会对PAHs的荧光强度造成严重影响,这就制约了该技术在土壤PAHs污染物检测中的应用,为此应建立一种减小土壤含水率对多环芳烃工作曲线影响的校正方法。
发明内容
针对现有技术中存在的不足,本发明提供一种将荧光光谱技术和近红外漫反射光谱技术相结合,为现场检测土壤中多环芳烃提供理论和实验基础的减小土壤含水率对多环芳烃荧光工作曲线影响的校正方法。
本发明采取的技术方案是:
一种减小土壤含水率对多环芳烃荧光工作曲线影响的校正方法,其特征在于:包括如下步骤:
步骤1:选取多个不同含水率的土壤样品,并针对土壤样本制备多个不同浓度多环芳烃的土壤样品;
步骤2:根据步骤1中不同含水率多环芳烃的土壤样品,建立相应多环芳烃浓度矩阵C;
步骤3:扫描步骤1中制备的每个土壤样品制备相应的荧光谱和近红外漫反射光谱,得到每个土壤样品的荧光谱和近红外漫反射光谱;
步骤4:对于步骤3中的荧光谱,选定用于建立定量分析多环芳烃工作曲线的荧光谱带M;
步骤5:对于步骤3中的近红外漫反射光谱,选定用于校正工作曲线的近红外漫反射光谱带N;
步骤6:提取步骤4中定量荧光谱带M处的荧光强度,得到相应荧光强度矩阵F;
步骤7:提取步骤5中近红外漫反射谱带N的强度,得到相应近红外漫反射强度矩阵S;
步骤9:根据步骤7得到的校正荧光强度矩阵Fc和步骤2中建立的多环芳烃浓度矩阵C,建立校正工作曲线。
进一步的,所述土壤样品的含水率范围为0-35%。
本发明的优点和积极效果是:
附图说明
图1为不同的浓度菲的各土壤样品在333nm波长光激发下的荧光谱;
图2为不同的浓度菲的各土壤样品的近红外漫反射光谱;
图3为校正之后,土壤中菲荧光工作曲线;
图4为校正之前,土壤中菲荧光工作曲线。
具体实施方式
下面结合实施例,对本发明进一步说明,下述实施例是说明性的,不是限定性的,不能以下述实施例来限定本发明的保护范围。
多环芳烃是由两个或两个以上苯环连接而成的有机化合物,包括蒽、菲、荧蒽等150余种化合物,下面以菲为实施例,结合附图对本发明的校正方法进行详细说明。
1、一种减小土壤含水率对多环芳烃荧光工作曲线影响的校正方法,其特征在于:包括如下步骤:
步骤1:选取多个不同含水率的土壤样本,并针对土壤样本制备多个不同浓度多环芳烃的土壤样品;
本实施例中,所述步骤1中的土壤样本选取天津农学院校园土,经烘干、过筛、研磨操作,制得干土样品。
本实施例中,取一定量的菲粉末(分析纯,购置于天津希恩思生化科技有限公司)溶于二氯甲烷,摇匀制成溶液,再把该溶液用玻璃棒引流浇到干土样品中,并将其置于通风橱中,等二氯甲烷完全挥发之后,将风干的菲土壤样品进行研磨,保证菲均匀混合在土壤中混合菲土均匀,接着,根据国家标准GB7172-1987《土壤水分测定法》,称取一定量上述配置的含菲土壤样品,加入自来水使得完全淹没含菲的土壤,静置一会后放入烘干箱干燥,干燥后得到不同含水率的相应土壤样品。
步骤2:根据步骤1中不同浓度多环芳烃的土壤样品,建立相应多环芳烃浓度矩阵C;
本实施例中,配置10个不同含水率、不同浓度菲土壤样品:菲浓度C分别为1mg/g、2mg/g、3mg/g、4mg/g、5mg/g、6mg/g、7mg/g、8mg/g、9mg/g、10mg/g;其对应的含水率分别为:24.44%、29.28%、14.82%、19.79%、12.82%、22%、28%32%、7.08%和8.96%。
步骤3:扫描步骤1中制备的每个土壤样品的荧光谱和近红外漫反射光谱,得到每个土壤样品的荧光谱和近红外漫反射光谱;
本实施例中,采用美国珀金埃尔默公司生产的LS-55荧光分光光度计对制备的土壤样品进行荧光扫描,得到每一样品的荧光光谱。
仪器参数设置如下:激发光源波长为333nm,荧光谱的波长范围为370~500nm,激发和发射单色仪狭缝宽度分别为5nm和5nm,光电倍增管电压为700,扫描速率为1000nm/min。
如图1所示,不同含水率的土壤样品,不同浓度的菲在土壤中存在三个明显的特征荧光峰,其位置分别在384nm、407nm和430nm处根据荧光谱确定用于建立定量分析菲荧光工作曲线的特征谱带M为333nm。
与此同时,采用美国珀金埃尔默公司生产的傅里叶近红外光谱仪对制备的土壤样品进行近红外漫反射光谱扫描,得到每一样品的近红外漫反射光谱。
仪器参数设置设置如下:扫描范围12000-4000cm-1,分辨率为8cm-1,每个样品扫描64次,取平均光谱。
如图2所示,可见不同含水率、不同浓度菲土壤样品在12000-4000cm-1范围的漫反射光谱强度存在差异,根据近红外漫反射光谱确定用于校正菲荧光工作曲线的近红外漫反射谱带N为5148cm-1。
步骤4:对于步骤3中的荧光谱,选定用于建立菲工作曲线的定量荧光谱带384nm;
步骤5:对于步骤3中的近红外漫反射光谱,选定用于校正工作曲线的近红外漫反射光谱带5148cm-1;
步骤6:提取步骤4中的10个菲的土壤样本在384nm处的荧光强度,得到相应荧光强度矩阵F;
步骤7:提取步骤5中10个菲的土壤样本在5148cm-1处的强度,得到相应近红外漫反射强度矩阵S;
步骤9:根据步骤7得到的校正荧光强度矩阵Fc和步骤2中建立的多环芳烃浓度矩阵C,建立横纵坐标轴,以Fc为纵轴,C为横轴,建立校正工作曲线(如图3所示)。
Fc=24.67+68.90C (2)
为了比较,对不同含水率、不同浓度菲土壤样品在487nm处的未校正荧光强度矩阵F与土壤中菲浓度矩阵C建立工作曲线(如图4所示),其方程为:
F=117.69+57.54C (3)
比较校正前后的工作曲线发现:校正工作曲线的相关系数为0.994,标准偏差为24.16;未校正工作曲线的相关系数为0.763,标准偏差为156.54。从上述结果可以看出:该专利所申请的校正方法可以有效的减小土壤含水率对菲荧光工作曲线的影响。
经过实验证明,对于不同含水率(0-35%)土壤,对于土壤中任何一种多环芳烃,包括芘、蒽、荧蒽等,均可通过本申请所建立的校正方法减小土壤含水率对定量分析多环芳烃工作曲线影响。
Claims (2)
1.一种减小土壤含水率对多环芳烃荧光工作曲线影响的校正方法,其特征在于:包括如下步骤:
步骤1:选取多个不同含水率的土壤样品,并针对土壤样本制备多个不同浓度多环芳烃的土壤样品;
步骤2:根据步骤1中不同含水率多环芳烃的土壤样品,建立相应多环芳烃浓度矩阵C;
步骤3:扫描步骤1中制备的每个土壤样品制备相应的荧光谱和近红外漫反射光谱;得到每个土壤样品的荧光谱和近红外漫反射光谱;
步骤4:对于步骤3中的荧光谱,选定用于建立定量分析多环芳烃工作曲线的定量荧光谱带M;
步骤5:对于步骤3中的近红外漫反射光谱,选定用于校正工作曲线的近红外漫反射光谱带N;
步骤6:提取步骤4中定量荧光谱带M处的荧光强度,得到相应荧光强度矩阵F;
步骤7:提取步骤5中近红外漫反射谱带N的强度,得到相应近红外漫反射强度矩阵S;
步骤9:根据步骤8 得到的校正荧光强度矩阵Fc和步骤2中建立的多环芳烃浓度矩阵C,建立校正工作曲线。
2.根据权利要求1所述的一种减小土壤含水率对多环芳烃荧光工作曲线影响的校正方法,其特征在于:所述土壤样品的含水率范围为0-35%。
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