Determination of boron in high-purity tantalum materials by on-line matrix separation/inductively coupled plasma mass spectrometry.
Determination of boron in high-purity tantalum materials by on-line matrix separation/inductively coupled plasma mass spectrometry.
复制标题
在线基质分离/电感耦合等离子体质谱法测定高纯钽材料中的硼。
DOI：
10.1039/b201019b
复制
发表时间：
2002
期刊：
影响因子：
--
通讯作者：
H. Haraguchi
中科院分区：
文献类型：
--
作者：
Shuji Kozono;Shigeto Takahashi;H. Haraguchi
本文介绍了高纯钽材料[金属钽、氧化钽、五氧化二钽和五乙醇钽]中超痕量硼的测定方法。采用在线阴离子交换基体分离-电感耦合等离子体质谱（ICP-MS）联用技术测定了ng g（-1）水平的硼。在分析之前，使用HF和/或HNO 3溶解钽材料。样品制备过程中硼的损失被视为在分解前向每个钽材料样品中加入一定量的硼来回收硼，并且它几乎可以忽略不计。在使用0.1 M HF载体溶液的阴离子交换法中，样品溶液中的钽和硼首先吸附在强碱性阴离子交换树脂上。接着，用5 M HCl从树脂洗脱硼，而钽保持强烈吸附。将洗脱的硼直接引入ICP-MS系统中，在m/z 10和11下进行定量分析。由于硼的洗脱时间长，瞬态信号在色谱图上的时间范围70-300 s内积分。虽然硼的洗脱在时间范围内是约。当进样溶液中总硼含量为40%时，金属钽、氧化钽、五氧化二钽和五乙醇钽的测定限（10 σ）分别为30、25、15和13 ng g（-1）。方法用于高纯钽原料中硼的测定，硼的含量在ng g（-1）~ μ g g g（-1）范围内。
A method for the determination of ultratrace amounts of boron in high-purity tantalum materials [tantalum metal, tantalum(v) oxide, tantalum pentachloride and tantalum pentaethoxide] is described. On-line anion-exchange matrix separation combined with inductively coupled plasma mass spectrometry (ICP-MS) was employed for the determination of boron at the ng g(-1) level. Tantalum materials were dissolved using HF and/or HNO3 prior to analysis. The loss of boron in the sample preparation procedure was examined as the recovery of boron by adding a definite amount of boron to each tantalum material sample before decomposition, and it was almost negligible. In an anion-exchange method using 0.1 M HF carrier solution, tantalum and boron in the sample solution were first adsorbed on a strongly basic anion-exchange resin. Next, boron was eluted from the resin with 5 M HCl, whereas tantalum was retained strongly adsorbed. The eluted boron was introduced directly into the ICP-MS system for quantitative analysis at m/z 10 and 11. Because of the long elution time of boron, the transient signal was integrated in the time range 70-300 s on the chromatogram. Although the elution of boron in the time range was ca. 40% of total boron in the sample solution injected, the determination limits (10sigma) obtained by the present method were 30, 25, 15 and 13 ng g(-1) for tantalum metal, tantalum(v) oxide, tantalum pentachloride and tantalum pentaethoxide, respectively. The method was applied to the determination of boron in commercially available high-purity tantalum materials and it was found that the concentrations of boron were in the ng g(-1)-microg g(-1) range.