一、前言
谷类作物亦称"禾谷类作物",它是以子实为人们提供食粮和为牲畜提供饲料的作物。粮食作物主要包括稻子、小麦、大麦、黑麦、燕麦、玉米、高粱、粟、黍、稷等。谷类作物除提供精饲料以外,在子粒成熟前,可收割作青饲料或青贮用。其秸秆、糖麸大多可作饲料用。谷类作物的种类和每种作物的类型、品种繁多,能分别适应各地的不同自然条件,摄取太阳能的效率较高,生长期长短不一,绝大多数属于一年生作物。为检测不同谷类作物中的重金属元素含量,选择微波消解对其进行前处理,探索最适合的消解参数,该方法还有回收率高、空白低等特点,有利于后续对多种无机元素的快速准确测定。
二、仪器与试剂
2.1、仪器
新仪TANK微波消解仪,赶酸器,分析天平(十万分之一)等
2.2、试剂
硝酸(68%),过氧化氢(30%),氢氟酸(40%)
三、实验方法
3.1、样品制备
取大米、小麦、玉米、高粱、燕麦样品,分别烘干粉碎后备用。
3.2、大米样品
称取大米样品约0.2g(精确至0.1mg)置于消解罐底部,加入8mL硝酸和1mL过氧化氢,静置10min左右,组装消解罐,按照如下设置参数进行消解实验:
3.3、小麦样品
称取小麦样品约0.5g(精确至0.1mg)置于消解罐底部,加入6mL硝酸和2mL过氧化氢,静置15min左右,组装消解罐,按照如下设置参数进行消解实验:
3.4玉米样品
称取玉米样品约0.5g(精确至0.1mg)置于消解罐底部,加入10mL硝酸,将消解罐放置在赶酸器上120℃预处理30min左右,待黄烟冒尽后取下冷却,,组装消解罐,按照如下设置参数进行消解实验:
3.5、高粱样品
称取高粱样品约0.2g(精确至0.1mg)置于消解罐底部,加入8mL硝酸和1mL氢氟酸,静置10min左右,组装消解罐,按照如下设置参数进行消解实验:
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DNSmfVUdMFpSBqThIdolnprDpquqAURM1JokM0K51VR00XlIKoOUl0iGals+qo6YJSEDUniQ7RrHRWHTVdUAqi5iTRIZqVzqqjpgtKQdScJDpEs9JZddR0QSmImpNEh2hWOquOmi4oBVFzkugQzUpn1VHTBaUgak4SHaJZ6aw6arqgFETNSaJDNCudVUdNF5SCqDlJdIhmpbPqqOmCUhA1J4kO0ax0Vh01XVAKouYk0SGalc6qo6YLSkHUnCQ6RLPSWXXUdEEpiJqTRIdoVjqrjpouKAVRc5LoEM1KZ9VR0wWlIGpOEh2iWemsOmq6oBREzUmiQzQrnVVHTReUgqg5SXSIZqWz6qjpglIQNSeJDtGsdFYdNV1QCqLmJNEhmpXOqqOmC0pB1JwkOkSz0ll11Hx8Qfn8/PyFR8g/RI0xZE9qq5IE944cZgzgT/xkvbi2ynf6sPo8nntVn1nij9HnlnXy+jvNH19QGAxCz3PK7+zh04qGP4rO+8/O5Dr9yXP+wfW4DtmqNvN71fmV52S2eY6z7uZdeV/F1ppMUDyZ6PArMpdzgCi/s1+dJFsM4EssEPmR782v5ria1ZX3ySxHcck6eX6lf3fYfnxByVBygcnrd8xXJ8no4fLe8CUWlKy7t047V/WrWV11j5HdzBo6d/Me+XmlrFVB4bf8o3+nXglpz/bqJBk9XPoIX6I/WffuBx59o8/v0mf2uNfdvFezbVNQGKwnPsjVPuUiER8NOaH48kFH/zDGfrYtW9Sp7KMvlXbvtoUvcrhb/oXB3bxXc2lTUAgGAXrao1ztz14RIKPYR34uKKRR0/M3kaPvnBGDO3nX3FC30q6g7CWTfvU6zacVlHgzFhXKMMfPodhW/0xqNSve88o+M45n3c07+rJi/OiCwsofv410Qfn6q8jZQxmxyo8/z2e2quQ4753aHr+8nufvxAJ3eXR0WVDiI3xiQKJ/Kx7IqFDkc6kTizF0+G996sN36K5qq1ldeS9+dwd+8cOfX+Hsu3lfef+R7UcXFDjMoLGQPPFBrvKJRSKywDg+YP4mDPJcTPgA8n7KV/Q4+11a5hjn8Y5R/k73j3fk+H2iyxvd0D/pkcyKyA1Yhkc+idXQQQtPEZgWlFxVPf/z/x9jHubhN/C1fHyVnKpP3mwCJvA3E3BB+Zuj77ubQDGB/wG6eryPQ/dt7gAAAABJRU5ErkJggg==)
3.6、燕麦样品
称取燕麦样品约0.2g(精确至0.1mg)置于消解罐底部,加入8mL硝酸和1mL过氧化氢,静置15min左右,组装消解罐,按照如下设置参数进行消解实验:
![](data:image/png;base64,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)
3.7、赶酸定容
实验结束,待冷却至60℃以下,取出消解罐,将消解罐转移至通风橱中缓慢打开,放置在赶酸器上于160℃赶酸至0.5mL左右。消解罐放冷后,将消化液转移至25mL容量瓶中,用少量水洗涤消解罐2次~3次,合并洗涤液于容量瓶中并用水定容至刻度,混匀备用。
四、结果与讨论
实验选择大米、小麦、玉米、高粱、燕麦五类谷物样品,分别采用不同的参数进行实验,最高温度190℃,样品均可完全消解。
五、参考文献
GB/T 35871-2018 粮油检验 谷物及其制品中钙、钾、镁、钠、铁、磷、锌、铜、锰、硼、钡、钼、钴、铬、锂、锶、镍、硫、钒、硒、铷含量的测定 电感耦合等离子体发射光谱法
六、注意事项
1、实验中加入氢氟酸,后续必须进行赶酸处理,防止氢氟酸对玻璃器皿造成腐蚀和影响检测结果。
2、消解结果以消解液澄清程度而定,是定性而非定量的结论,因样品种类、来源、取样量等原因,消解程序可能需要适当调整,此方案只供大家参考,用户可根据具体情况和经验优化消解方案。如适当调整保温时间或者消解温度等。