Abstract:During the synthesis of artificial diamond, the alloy catalyst is usually used to reduce the required high temperature and high pressure. However, the impurity elements in catalyst will enter into the interior of artificial diamond, which seriously influences the properties. The artificial diamond sample was pre-ashed at 750 ℃. After treatment with sulfuric acid and hydrochloric acid by heating, the sample was burned and ashed at 950 ℃ followed by dissolution with hydrochloric acid. Cr 267.716 nm, Mn 257.610 nm, Ni 221.648 nm, Al 309.271 nm, Fe 259.940 nm, Mg 279.553 nm and Ti 334.941 nm were selected as analytical lines. The content of seven elements in artificial diamond including Cr, Mn, Ni, Al, Fe, Mg and Ti was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The linear correlation coefficients of calibration curves of elements were r=0.999 4-0.999 9, indicating good linearity. The low limit of determination of elements were between 0.021 μg/g and 0.27 μg/g. The content of Cr, Mn, Ni, Al, Fe, Mg and Ti in artificial diamond sample was determined according to the experimental method. The relative standard deviations (RSD, n=6) were in the range of 0.75%-1.9%. The recoveries were between 93% and 107%. Three artificial diamond samples were pretreated according to the experimental method. The sample solution was determined by ICP-AES and inductively coupled plasma mass spectrometry (ICP-MS), respectively. The results were consistent with each other.
陶丽萍,刘氘,石华.高温分解测试高纯人造金刚石中的碳和硅[J].中国非金属矿工业导刊,2013(5):32-34.TAO Li-ping, LIU Dao, SHI Hua. High temperature decomposition of carbon and silicon in high-purity synthetic diamond[J].China Nonmetallic Minerals Industry, 2013(5):32-34.
[3]
蔡绍勤,李川世.高纯金属和半导体材料分析[M].北京:冶金工业出版社,1995:328-329.
[4]
郑友进,马红安,周林,等.铁镍触媒合成的金刚石中包裹体的探讨[J].人工晶体学报, 2008, 37(1):49-51ZHENG You-jin, MA Hong-an, ZHOU Lin, et al. Study on inclusion in diamond synthesized using FeNi as catalyst[J].Journal of Synthetic Crystals, 2008, 37(1):49-51.
[4]
周伟,马福康,吕海波,等.关于人造金刚石热稳定性与其包裹体关系的初步探索[J].粉末冶金材料科学与工程(Materials Science and Engineering of Powder Metallargy),1996(2):17-22.
[5]
方建锋,张晋远,金成海,等.人造金刚石中包裹体含量的测定[J].金刚石与磨料磨具工程,2001(1):13-16.FANG Jian-feng,ZHANG Jin-yuan,JIN Cheng-hai,et al.Determination of impurity inclusions content in synthetic diamond by means of X-ray fluorescence and X-ray absorption analysis[J].Diamond & Abrasives Engineering,2001(1):13-16.
[6]
吴伦强,张连平,杨光文,等.XRF法无标分析人造金刚石原料锭中Fe,Ni,Cr,Co组分及其分布[J].核电子学与探测技术,2007,27(6):1227-1230.WU Lun-qiang,ZHANG Lian-ping,YANG Guang-wen,et al.Analyze content and distribution of Fe, Ni, Cr, Co inartificial diamond raw material ingot by XRF standardless method[J].Nuclear Electronics and Detection Technology,2007,27(6):1227-1230.
[7]
赵玉珍,薛进敏. ICP-AES法同时测定纯铁中八种杂质元素[J].光谱实验室,1999,16(1):79-82.ZHAO Yu-zhen, XUE Jin-min.Simultaneous determination of eight impurity elements in pure iron by ICP-AES[J]. Chinese Journal of Spectroscopy Laboratory, 1999,16(1):79-82.
[8]
张萍.微波消解ICP-AES法同时测定花岗石中铜、镉、铬和砷[J].光谱实验室,2002,19(3):338-340.ZHANG Ping.Simultaneous determination of harmful elements Pb, Cd, Cr and As in granite with microwave digestion-ICP-AES[J].Chinese Journal of Spectroscopy Laboratory, 2002,19(3):338-340.
[9]
莫定奇,倪月勇,黄志.微波消解ICP-AES法测定化妆品中无机元素的研究 Ⅰ.固体类化妆品中As,Pb,Cd,Sr,Cr,Bi和Se等的分析方法研究[J].光谱学与光谱分析,1999,19(4):598-600.MO Ding-qi,NI Yue-yong,HUANG Zhi.Study on the elements in cosmetics by microwave digestion-ICP-AES Ⅰ.The determination of Pb, As, Cr, Cd, Sr, Bi and Se in solid state cosmetics[J]. Spectroscopy and spectral analysis, 1999,19(4):598-600.
[10]
叶苑才,孟广政,杨菊亭,等. ICP-AES法在钢铁及其合金分析中的应用[J].光谱学与光谱分析,1991,11(4):61-70.YE Yuan-cai,MENG Guang-zheng,YANG Ju-ting,et al.Analysis of iron and steel by ICP-AES[J].Spectroscopy and Spectral Analysis,1991,11(4):61-70.