CN112213178A - 一种浅河区域沉积物中微塑料的检测方法 - Google Patents
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Abstract
本发明公开了一种浅河区域沉积物中微塑料的检测方法,涉及沉积物微塑料检测技术领域,为解决现有微塑塑料的检测方法准确度不高,耗时较长,工作效率低下的问题。步骤一:将采集的浅河区域沉积物过筛后,称取沉积物干燥至恒重,称重,并记录沉积物的干重;步骤二:将烘干的浅河区域沉积物和1.5mol/L KOH混合后,置于磁力搅拌器上80℃下搅拌,消解2h;步骤三:将消解产物烘干;步骤四:向烘干的消解物产物中加入500mL超纯水,并置于电热炉上加热至70℃后,加入NaI物质浮选,期间不断进行搅拌,并确保最终NaI溶液密度达到2.5g/cm3后静置沉淀,整个浮选过程恒温70℃;步骤五:取碘化钠浮选液经过醋酸纤维滤膜进行抽滤。
Description
技术领域
本发明涉及沉积物微塑料检测技术领域,具体为一种浅河区域沉积物中微塑料的检测方法。
背景技术
环境中的塑料垃圾在物理磨损、化学降解和生物降解的共同作用下,可降解为粒径更小的塑料,即微塑料。一般将直径或长度小于5mm的塑料纤维、颗粒或碎片定义为微塑料。由于微塑料被证实可对生物体产生负面影响,联合国环境规划署于2014年将微塑料列为十大新兴重要污染物之一,其检测方法也成为当下环保领域的热点。为减少环境样品基底对微塑料测定的干扰,微塑料样品的分离涉及到消解,目前常用的消解有强酸消解、强碱消解、氧化消解、酶消解,强碱消解的应用还不是十分广泛。一些研究表明1mol/L左右的强碱有较佳的消解效果,但存在消解浓度不明确,消解时间长等问题。
另外,微塑塑料的检测方法中通常采用饱和NaCl溶液对样品进行浮选,但此方法筛选的微塑料种类不齐全,常常无法浮选高密度微塑料,不适合于微塑料的精确检测;因此,不满足现有的需求,对此我们提出了一种浅河区域沉积物中微塑料的检测方法。
发明内容
本发明的目的在于提供一种浅河区域沉积物中微塑料的检测方法,以解决上述背景技术中提出的现有微塑料的检测方法准确度不高,耗时较长,工作效率低下的问题。
为实现上述目的,本发明提供如下技术方案:一种浅河区域沉积物中微塑料的检测方法,包括如下步骤:
步骤一:将采集的浅河区域沉积物过筛后,称取沉积物干燥至恒重,称重,并记录沉积物的干重;
步骤二:将烘干的浅河区域沉积物和1.5mol/L KOH混合后,置于磁力搅拌器上80℃下搅拌,消解2h;
步骤三:将消解产物烘干;
步骤四:向烘干的消解物产物中加入500mL超纯水,并置于电热炉上加热至70℃后,加入NaI物质浮选,期间不断进行搅拌,并确保最终NaI溶液密度达到2.5g/cm3后静置沉淀,整个浮选过程恒温70℃;
步骤五:取碘化钠浮选液经过醋酸纤维滤膜进行抽滤;
步骤六:取下上步骤的滤膜放入烘箱烘干至恒重;
步骤七:使用体视显微镜观察烘干的滤膜,挑出微塑料疑似颗粒后,使用傅里叶显微红外光谱法找到目标物,将目标物的红外光谱图与标准谱图联机检索对照,根据拟合度定性分析和定量分析。
优选的,所述步骤一、步骤三和步骤六中,干燥温度为90℃,烘干至恒重。
优选的,所述步骤二中,所用消解液为1.5mol/L的KOH溶液。
优选的,所述步骤二中,磁力搅拌器的速度为130r/min,温度为80℃,消解时间为2h。
优选的,所述步骤五中,滤膜为孔径为0.5µm醋酸纤维滤膜。
优选的,所述步骤七中,傅里叶显微红外光谱系统分析选择反射模式,MCT检测器,波数范围为4000cm-1-750cm-1,分辨率为4cm-1,光栅大小与累积次数随目标物大小变化,累加次数随光栅增大而减小。
与现有技术相比,本发明的有益效果是:
1. 该发明提供了一种环境监测领域中的沉积物中微塑料检测方法,通过采用1.5mol/L氢氧化钠溶液消解沉积物中有机物,消除了有机物对微塑料红外光谱获取的干扰,微塑料测定准确率较高。
2. 通过提高消解温度,有效的缩减了消解时间,使得消解效率显著提高;
3. 通过加热配制出密度很高的浮选液,可浮选出种类齐全的微塑料,实验的准确性较高。
附图说明
图1为本发明的一种浅河区域沉积物中微塑料的检测方法的工作流程图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。
请参阅图1,本发明提供的一种实施例:一种浅河区域沉积物中微塑料的检测方法,包括如下步骤:
步骤一:将采集的浅河区域沉积物用5目筛子过筛后,称取250g沉积物烘干至恒重,称重,并记录沉积物的干重;
步骤二:称取100g烘干的沉积物于1000mL烧杯中,加入400mL 1.5mol/L KOH后将烧杯置于磁力搅拌器上加热至80℃,在130r/min下磁力搅拌消解2h;
步骤三:将消解产物烘干;
步骤四:向烘干的消解物产物中加入500mL超纯水,并置于电热炉上加热至70℃后,加入NaI物质浮选,期间不断搅拌,并确保NaI溶液最终密度达到2.5g/cm3后静置沉淀,整个浮选过程恒温70℃;
步骤五:取碘化钠浮选液经过0.5µm醋酸纤维滤膜进行抽滤;
步骤六:取下上步骤的滤膜放入烘箱烘干至恒重;
步骤七:使用体视显微镜观察烘干的滤膜,挑出微塑料疑似颗粒后,使用傅里叶显微红外光谱法找到目标物,将目标物的红外光谱图与标准谱图联机检索对照,根据拟合度定性分析和定量分析。
进一步,步骤一、步骤三和步骤六中,干燥温度为90℃,烘干至恒重,烘箱的温度控制在60~280℃。
进一步,步骤二中,所用消解液为1.5mol/L的KOH溶液,消解的目的是去除有机物,消除有机物对微塑料红外光谱测定的干扰。
进一步,步骤二中,磁力搅拌器的速度为130r/min,温度为80℃,消解时间为2h。
进一步,步骤五中,滤膜为孔径为0.5µm醋酸纤维滤膜,过滤前用超纯水对滤膜清洗至少三次。
进一步,步骤七中,傅里叶显微红外光谱系统分析选择反射模式,MCT检测器,波数范围为4000cm-1-750cm-1,分辨率为4cm-1,光栅大小与累积次数随目标物大小变化,累加次数随光栅增大而减小。
对于本领域技术人员而言,本发明不限于上述示范性实施例的细节,在不背离本发明的精神或基本特征的情况下,还可以以其他的具体形式实现本发明。这些均在本发明的保护范围内。
Claims (6)
1.一种浅河区域沉积物中微塑料的检测方法,其特征在于,包括如下步骤:
步骤一:将采集的浅河区域沉积物过筛后,称取沉积物干燥至恒重,称重,并记录沉积物的干重;
步骤二:将烘干的浅河区域沉积物和1.5mol/L KOH混合后,置于磁力搅拌器上80℃下搅拌,消解2h;
步骤三:将消解产物烘干;
步骤四:向烘干的消解物产物中加入500mL超纯水,并置于电热炉上加热至70℃后,加入NaI物质浮选,期间不断进行搅拌,并确保最终NaI溶液密度达到2.5g/cm3后静置沉淀,整个浮选过程恒温70℃;
步骤五:取碘化钠浮选液经过醋酸纤维滤膜进行抽滤;
步骤六:取下上步骤的滤膜放入烘箱烘干至恒重;
步骤七:使用体视显微镜观察烘干的滤膜,挑出微塑料疑似颗粒后,使用傅里叶显微红外光谱法找到目标物,将目标物的红外光谱图与标准谱图联机检索对照,根据拟合度定性分析和定量分析。
2.根据权利要求1所述的一种浅河区域沉积物中微塑料的检测方法,其特征在于:所述步骤一、步骤三和步骤六中,干燥温度为90℃,烘干至恒重。
3.根据权利要求1所述的一种浅河区域沉积物中微塑料的检测方法,其特征在于:所述步骤二中,所用消解液为1.5mol/L的KOH溶液。
4.根据权利要求1所述的一种浅河区域沉积物中微塑料的检测方法,其特征在于:所述步骤二中,磁力搅拌器的速度为130r/min,温度为80℃,消解时间为2h。
5.根据权利要求1所述的一种浅河区域沉积物中微塑料的检测方法,其特征在于:所述步骤五中,滤膜为孔径为0.5µm醋酸纤维滤膜。
6.根据权利要求1所述的一种浅河区域沉积物中微塑料的检测方法,其特征在于:所述步骤七中,傅里叶显微红外光谱系统分析选择反射模式,MCT检测器,波数范围为4000cm-1-750cm-1,分辨率为4cm-1,光栅大小与累积次数随目标物大小变化,累加次数随光栅增大而减小。
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