微波消解-电感耦合等离子体原子发射光谱法测定3D硬金饰品中铅、砷、汞、镉的含量
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摘要
取硬金样品约0.1g,加入新配制的盐酸-硝酸(3+1)混合酸6mL,按消解程序进行微波消解。待消解结束后将溶液于80℃加热赶去氮氧化物,冷却至室温后用水定容至50mL,用电感耦合等离子体原子发射光谱法测定其中铅、砷、汞、镉的含量。各元素的质量浓度均在0.10～10.0mg·L~(-1)内与对应的发射强度呈线性关系,检出限(3s)为2.0～8.0mg·kg~(-1)。加标回收率为91.0%～103%。应用该方法分析了21批次3D硬金饰品,测定结果与电感耦合等离子体质谱法的一致,测定值的相对标准偏差(n=6)小于3.0%。
The sample(about 0.1 g) was added into 6 mL of a mixture of hydrochloric acid and nirtic acid(3+1) for microwave digestion according to digestion program.After the digestion was completed,the solution was heated at 80 ℃ to remove nitrogen oxide,cooled to room temperature,and made up to 50 mL with water.The contents of lead,arsenic,mercury and cadmium in the solution was determined by inductively coupled plasma atomic emission spectrometry.Linear relationships were found between emission intensity and mass concentration of the 4 elements in the same range of 0.10-10.0 mg·L~(-1) ,with detection limits(3 s) in the range of 2.0-8.0 mg·kg~(-1) .Values of recovery obtained by standard addition method were in the range of 91.0%-103%.The proposed method was applied to determination of the 4 elements in 21 batches of hard gold jewelry samples,giving results in consistency with those obtained by inductively coupled plasma mass spectrometry,and RSDs(n=6) were less than3.0%.
The sample(about 0.1 g) was added into 6 mL of a mixture of hydrochloric acid and nirtic acid(3+1) for microwave digestion according to digestion program.After the digestion was completed,the solution was heated at 80 ℃ to remove nitrogen oxide,cooled to room temperature,and made up to 50 mL with water.The contents of lead,arsenic,mercury and cadmium in the solution was determined by inductively coupled plasma atomic emission spectrometry.Linear relationships were found between emission intensity and mass concentration of the 4 elements in the same range of 0.10-10.0 mg·L~(-1) ,with detection limits(3 s) in the range of 2.0-8.0 mg·kg~(-1) .Values of recovery obtained by standard addition method were in the range of 91.0%-103%.The proposed method was applied to determination of the 4 elements in 21 batches of hard gold jewelry samples,giving results in consistency with those obtained by inductively coupled plasma mass spectrometry,and RSDs(n=6) were less than3.0%.
引文
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[2] 黄云光,王昶,袁军平.首饰制作工艺学[M].武汉:中国地质大学出版社,2010.
[3] 徐强,杨光敏,刘莹莹.3D硬千足金首饰的市场分析[J].市场研究,2014(9):45-46.
[4] 刘正伟.硬金镀层的研究进展[J].电镀与精饰,2011,33(7):13-17.
[5] 陈丁滢,吴奕阳,谢启耀.饰品中有害元素的限定及无损检测方法的前瞻[J].上海计量测试,2009,211(3):2-3.
[6] GB 28480-2012 饰品有害元素限量的规定[S].
[7] GB/T 28020-2011 饰品有害元素的测定X射线荧光光谱法[S].
[8] GB/T 28021-2011 饰品有害元素的测定光谱法[S].
[9] 张磊,王晓艳,李波.微波消解技术在金属分析中的应用[J].光谱实验室,2010,27(3):953-957.
[10] 郭满栋,马淑君,王晓华,等.微波在分析化学及有机合成中的应用[J].理化检验-化学分册,2002,38(3):158-161.
[11] 王璇,段飞,朱勇,等.“3D硬金”饰品内部缺陷筛查方法试验研究[J].黄金,2017,38(11):4-8.
[12] 杜中文.首饰用千足硬金的主要物性分析及行业标准探讨[D].武汉:中国地质大学,2010.