CN110470621A - 土壤中重金属铬的检测分析方法 - Google Patents
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Abstract
本发明公开一种土壤中重金属铬的检测分析方法，包括以下步骤：（1）样品的采集与保存：将采集的土壤样品混匀后用四分法缩分，研磨压碎后通过尼龙筛除去以上的砂砾，用玛瑙研钵将通过尼龙筛的土样研磨至全部通过100目尼龙筛，混匀后备用；（2）样品溶液的制备：将样品置于微波消解罐中，用水润湿后加入硝酸、氢氟酸升温进行消解，冷却后将溶液转移至坩埚中，加入高氯酸，加热坩埚驱赶白烟并蒸至内容物呈粘稠状，稍冷后加入盐酸溶液，溶解可溶性残渣，全量转移至容量瓶中，加入氯化铵溶液，冷却后定容，摇匀即得样品溶液；（3）样品溶液铬含量测定：用原子吸收分光光度计法进行测定，根据公式计算得到样品溶液中铬的含量W(mg/kg）。
Description
技术领域
本发明涉及土壤中重金属含量测定的技术领域，具体指土壤中重金属铬的检测分析方法。
背景技术
由于近年来土壤和农产品重金属污染所引起的环境事故层出不穷，人民谈“重”色变， 重金属污染已经成为我国突出短板之一。
铬是重要的合金元素，所有铬的化合物都有毒性，六价铬的毒性最大，三价次之，二价 毒性最小，其中六价铬的毒性比三价铬几乎大100倍。六价铬被美国环境保护局确定为17种 高度危险的毒性物质之一，六价铬对人的致死量为5克。
铬对人体的毒害是全身性的，可导致皮肤过敏、溃疡，鼻中隔穿孔和支气管哮喘等，是 已知的致癌物。过量含铬化合物进入人体可能引起肾脏损伤，引发肾功能及尿中酶和蛋白含 量的改变，严重的可能导致肾脏坏死。六价的铬离子也是一种毒性很大的致畸、致突变剂， 其在体内会引起氧化应激、DNA损害、细胞凋亡、基因突变。
而当摄入量低时，三价的铬离子对人和动物则是必需的微量元素，三价铬通过增强胰岛 素的作用，影响机体内糖类、脂类、矿物代谢以及蛋白质和核酸的合成，改善畜禽的生长、 繁殖及免疫性能。
据有关调查显示，我国受重金属污染的耕地面积已达2000万hm2，占全国总耕地面积的 1/6，因此在开展农产品种植之前进行土壤重金属检测分析是农业种植中的关键工作，掌握土 壤重金属污染情况才能具有针对性地进行土壤改良工作。
发明内容
本发明旨在提供一种土壤中重金属铬的检测分析方法。
本发明的技术方案如下：
土壤中重金属铬的检测分析方法，包括以下步骤：
(1)样品的采集与保存：将采集的土壤样品混匀后用四分法缩分，缩分后的士样风干并 除去土样中石子和动植物残体等异物，研磨压碎后通过2mm尼龙筛除去2mm以上的砂砾， 用玛瑙研钵将通过2mm尼龙筛的土样研磨至全部通过100目尼龙筛，混匀后备用；
(2)样品溶液的制备：将样品置于微波消解罐中，用水润湿后加入6ml硝酸、2ml氢氟酸升温进行消解，冷却后将溶液转移至聚四氟乙烯坩埚中，加入2ml高氯酸，加热坩埚驱赶白烟并蒸至内容物呈粘稠状，取下坩埚稍冷，加入3ml盐酸溶液，溶解可溶性残渣，全量转移至容量瓶中，加入5ml氯化铵溶液，冷却后定容至标线，摇匀即得样品溶液；
(3)样品溶液铬含量测定：用原子吸收分光光度计法对空白样品和样品溶液进行测定， 根据公式计算得到样品溶液中铬的含量W(mg/kg)为：
式中：ρ—试液的吸光度减去空白溶液的吸光度，然后在校准曲线上查得铬的浓度，mg/L；
V—试液定容的体积，mL；
m—称取试样的重量，g；
f—试样中水分的含量，％。
步骤(3)中所述的校准曲线其绘制方法如下：
准确移取铬标准使用液0.00、0.50、1.00、2.00、3.00、4.00ml于50ml容量瓶中， 然后，分别加入5ml氯化铵溶液和3ml盐酸溶液，用水定容至标线，摇匀，其铬的浓度分 别为0.50、1.0、2.00、3.00、4.00mg/L；按低到高质量浓度顺序测定标准溶液的吸光度， 用标准溶液吸光度减去空白溶液的吸光度与相对应的铬的浓度绘制校准曲线。
所述空白溶液吸光度的测定方法如下：用去离子水代替样品溶液，采用与步骤(2)相同 的处理步骤和试剂，制备全程序空白溶液，并按铬标准溶液吸光度测定的条件进行空白溶液 吸光度的测定，每批样品至少制备2个以上的空白溶液。
所述坩埚的加热温度为150℃。
其特征在于步骤(2)所述盐酸的浓度为1.19g/mL，硝酸的浓度为ρ＝1.42g/mL。
所述铬标准使用液的浓度为50mg/L。
本发明的有益效果在于：
1.本发明所述的方法，可以检测分析出土壤中重金属铬的含量，掌握土壤重金属铬的污 染情况才能具有针对性地进行土壤改良工作，使种植地更适宜农作物的生长。
2.采用本发明所述的方法，检出限位5mg/kg，检出限低，准确度高。
3.在样品溶液制备过程中加入氯化铵可以抑制铁、钻、镍、钒、铝、镁、铅等共存离子 的干扰，使检测的准确度更高。
具体实施方式
下面对本发明作进一步的说明。
实施例1
本发明所述土壤中重金属铬的检测分析方法原理如下：
采用盐酸-硝酸-氢氟酸-高氯酸全分解的方法，破坏土壤的矿物晶格，使试样中的待测元 素全部进入试液，并且，在消解过程中，所有铬都被氧化成Cr2O7 2-。然后，将消解液喷入富 燃性空气-乙快火焰中，在火焰的高温下，形成铬基态原子，并对铬空心阴极灯发射的特征谱 线357.9nm产生选择性吸收，在选择的最佳测定条件下，测定铬的吸光度。
具体检测步骤如下：
(1)样品的采集与保存：将采集的土壤样品混匀后用四分法缩分，缩分后的士样风干并 除去土样中石子和动植物残体等异物，研磨压碎后通过2mm尼龙筛除去2mm以上的砂砾， 用玛瑙研钵将通过2mm尼龙筛的土样研磨至全部通过100目尼龙筛，混匀后备用。
(2)样品溶液的制备：将样品置于微波消解罐中，用水润湿后加入6ml硝酸、2ml氢氟酸升温进行消解，冷却后将溶液转移至聚四氟乙烯坩埚中，加入2ml高氯酸，加热坩埚驱赶白烟并蒸至内容物呈粘稠状，取下坩埚稍冷，加入3ml盐酸溶液，溶解可溶性残渣，全量转移至容量瓶中，加入5ml氯化铵溶液，冷却后定容至标线，摇匀即得样品溶液。
(3)采用的试剂如下：
盐酸:ρ＝1.19g/mL，优级纯；
硝酸:ρ＝1.42g/mL，优级纯；
氢氟酸:ρ＝1.49g/mL；
10％氯化铵水溶液：准确称取10g氯化铵，用少量水溶解后全量转移入100ml容量瓶中， 用水定容至标线，摇匀；
铬标准贮备液，ρ＝1.0mg/mL：准确称取0.2829g基准重铬酸钾，用少量水溶解后全量 转移入l00mL容量瓶中，用水定容至标线，摇匀，冰箱中2～8℃保存；
铬标准使用液，ρ＝50mg/L：移取铬标准储备液5.00mL于100mL容量瓶中，加水定容至标线，摇匀，临用时现配；
高氯酸：ρ＝1.68g/mL，优级纯。
(4)仪器和设备
原子吸收分光光度计，带铬空心阴极灯；微波消解仪；玛瑙研磨机。
(5)校准曲线的绘制：
准确移取铬标准使用液0.00、0.50、1.00、2.00、3.00、4.00ml于50ml容量瓶中， 然后，分别加入5ml氯化铵溶液和3ml盐酸溶液，用水定容至标线，摇匀，其铬的浓度分 别为0.50、1.0、2.00、3.00、4.00mg/L；按低到高质量浓度顺序测定标准溶液的吸光度， 用标准溶液吸光度减去空白溶液的吸光度与相对应的铬的浓度绘制校准曲线。
(6)空白溶液吸光度测定：
用去离子水代替样品溶液，采用与步骤(2)相同的处理步骤和试剂，制备全程序空白溶 液，并按铬标准溶液吸光度测定的条件进行空白溶液吸光度的测定，每批样品至少制备2个 以上的空白溶液。
(7)样品溶液铬含量测定：用原子吸收分光光度计法对空白样品和样品溶液进行测定， 根据公式计算得到样品溶液中铬的含量W(mg/kg)为：
式中：ρ—试液的吸光度减去空白溶液的吸光度，然后在校准曲线上查得铬的浓度，mg/L；
V—试液定容的体积，mL；
m—称取试样的重量，g；
f—试样中水分的含量，％。
采用上述实施例所述的方法，可以检测分析出土壤中重金属铬的含量，掌握土壤重金属 铬的污染情况才能具有针对性地进行土壤改良工作，使种植地更适宜农作物的生长。
采用本发明所述的方法，检出限位5mg/kg，检出限低，准确度高。
在样品溶液制备过程中加入氯化铵可以抑制铁、钻、镍、钒、铝、镁、铅等共存离子的干扰， 使检测的准确度更高。
Claims (6)
1.土壤中重金属铬的检测分析方法，其特征在于，包括以下步骤：
(1)样品的采集与保存：将采集的土壤样品混匀后用四分法缩分，缩分后的士样风干并除去土样中石子和动植物残体等异物，研磨压碎后通过2mm尼龙筛除去2mm以上的砂砾，用玛瑙研钵将通过2mm尼龙筛的土样研磨至全部通过100目尼龙筛，混匀后备用；
(2)样品溶液的制备：将样品置于微波消解罐中，用水润湿后加入6ml硝酸、2ml氢氟酸升温进行消解，冷却后将溶液转移至聚四氟乙烯坩埚中，加入2ml高氯酸，加热坩埚驱赶白烟并蒸至内容物呈粘稠状，取下坩埚稍冷，加入3ml盐酸溶液，溶解可溶性残渣，全量转移至容量瓶中，加入5ml氯化铵溶液，冷却后定容至标线，摇匀即得样品溶液；
(3)样品溶液铬含量测定：用原子吸收分光光度计法对空白样品和样品溶液进行测定，根据公式计算得到样品溶液中铬的含量W(mg/kg)为：
式中：ρ—试液的吸光度减去空白溶液的吸光度，然后在校准曲线上查得铬的浓度，mg/L；
V—试液定容的体积，mL；
m—称取试样的重量，g；
f—试样中水分的含量，％。
2.如权利要求1所述土壤中重金属铬的检测分析方法，其特征在于，步骤(3)中所述的校准曲线其绘制方法如下：
准确移取铬标准使用液0.00、0.50、1.00、2.00、3.00、4.00ml于50ml容量瓶中，然后，分别加入5ml氯化铵溶液和3ml盐酸溶液，用水定容至标线，摇匀，其铬的浓度分别为0.50、1.0、2.00、3.00、4.00mg/L；按低到高质量浓度顺序测定标准溶液的吸光度，用标准溶液吸光度减去空白溶液的吸光度与相对应的铬的浓度绘制校准曲线。
3.如权利要求2所述土壤中重金属铬的检测分析方法，其特征在于，所述空白溶液吸光度的测定方法如下：用去离子水代替样品溶液，采用与步骤(2)相同的处理步骤和试剂，制备全程序空白溶液，并按铬标准溶液吸光度测定的条件进行空白溶液吸光度的测定，每批样品至少制备2个以上的空白溶液。
4.如权利要求2所述土壤中重金属铬的检测分析方法，其特征在于，所述坩埚的加热温度为150℃。
5.如权利要求1所述土壤中重金属铬的检测分析方法，其特征在于步骤(2)所述盐酸的浓度为1.19g/mL，硝酸的浓度为ρ＝1.42g/mL。
6.如权利要求2所述土壤中重金属铬的检测分析方法，所述铬标准使用液的浓度为50mg/L。
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