微波消解-电感耦合等离子体发射光谱法测定DD6 单晶合金中铝、铬、钴
朱天一,冯典英,李本涛,巩琛,李颖,黄辉
中国兵器工业集团第五三研究所,济南 250000
Determination of aluminum, chromium and cobalt in DD6 single crystal superalloys by microwave digestion-inductively coupled plasma optical emission spectrometry
朱天一,冯典英,李本涛,巩琛,李颖,黄辉
CNGC Institue 53, Jinan 250000, China
摘要:建立电感耦合等离子体发射光谱法测定DD6 单晶高温合金中铝、铬、钴元素含量的方法。采用密闭微波消解法对样品进行前处理,利用模拟溶液分别考察基体元素和共存元素的光谱干扰及非光谱干扰对测定结果的影响,确定了铝、铬、钴的分析谱线分别为394.401,267.716,228.616 nm,通过基体匹配法对非光谱干扰进行补偿。待测元素在各自的质量浓度范围内与光谱强度呈良好的线性关系,相关系数均为0.999 9,铝、铬、钴的检出限分别为0.110,0.018,0.003 μg/mL。测定结果的相对标准偏差为0.99%~1.21%(n=11),铝、铬、钴的加标回收率在分别为96.45%~103.69%,98.20%~99.40%,100.22%~102.85%。该方法简便、快速,具有较高的准确度,适用于镍基单晶高温合金中铝、铬、钴元素的测定。
Abstract:A method for determining the contents of aluminum, chromium and cobalt in DD6 single crystal superalloy
by inductively coupled plasma emission spectrometry was established. The sample was decomposed in microwave digestion
instrument. The effects of the spectral interference and non-spectral interference of matrix elements and coexisting elements
on the determination results were investigated by using simulated solutions. The analytical lines of Al, Cr and Co were
394.401, 267.716, 228.616 nm, respectively. The non-spectral interference was eliminated by matrix matching method.
The elements to be measured had good linear relationship with the spectral intensity in their respective mass concentration
range, the correlation coefficients were all 0.999 9, and the detection limits of Al, Cr and Co were 0.110, 0.018, 0.003 μg/
mL, respectively. The relative standard deviation of determination results was 0.99%-1.21%(n=11), and the recovery rates
of Al, Cr and Co were 96.45%-103.69%, 98.20%-99.40%, 100.22%-102.85%, respectively. This method is simple, rapid
and accuracy, it is suitable for the determination of aluminum, chromium and cobalt in nickel base single crystal superalloy.
关键词:电感耦合等离子体发射光谱法;镍基单晶高温合金;光谱干扰;非光谱干扰
Keywords:inductively coupled plasma optical emission spectrometry; nickel base single crystal superalloy; spectral interference; non-spectral interference
本文引用格式:
朱天一,冯典英,李本涛,等. 微波消解- 电感耦合等离子体发射光谱法测定DD6 单晶合金中的铝、铬、钴[J]. 化学分析计量,2020,29(2):87-90.
ZHU T Y,FENG D Y,LI B T,et al. Determination of aluminum,chromium and cobalt in DD6 single crystal superalloys by microwave digestion-inductively coupled plasma optical emission spectrometry[J]. Chemical analysis and meterage,2020,29(2):87-90.
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