Qualitative and quantitative tests of gemstones and diamonds are routinely performed nondestructively in the laboratory of Gemmological Institute of India (GII), Mumbai, India. Qualitative tests are based on microscopic examination. Energy Dispersive X-Ray Fluorescence (EDXRF) spectrometry is used in the laboratory for quantitative analysis of elements. However, in some cases like determination of trace levels of cubic zirconia (CZ) in diamond powder, it is difficult to estimate simultaneously both CZ and diamond powder directly using EDXRF method. In view of this, a method was developed for estimation of ZrO₂ present at low levels in diamond powder. In this method, EDXRF spectra of a series of simulated mixtures containing ZrO₂ were measured. Peak areas under the characteristic K_α x-ray of Zr (15.7 keV) in each mixture were computed and, a calibration plot was made between the peak areas and % fractions of ZrO₂. From the calibration plot, a dynamic range of 0.1%–10% was obtained. From XRF spectra of the test sample, in duplicate, of diamond powder, Zr was estimated using the peak area and the percentage fraction was found to be 0.181 ± 0.020. Neutron activation analysis (NAA) was used for method validation with the same set of simulated samples used in EDXRF analysis. Results obtained by both the methods are found to be in good agreement and this newly developed method based on EDXRF spectrometry is in regular use in GII.

中文翻译：

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用于定量金刚石基质中立方氧化锆的能量色散 X 射线荧光方法的开发和验证

宝石和钻石的定性和定量测试通常在印度孟买印度宝石学院 (GII) 的实验室进行。定性测试基于显微镜检查。能量色散 X 射线荧光 (EDXRF) 光谱测定法在实验室中用于元素的定量分析。然而，在某些情况下，例如测定金刚石粉末中痕量立方氧化锆 (CZ)，很难直接使用 EDXRF 方法同时估算 CZ 和金刚石粉末。鉴于此，开发了一种用于估计金刚石粉末中低含量的ZrO ₂的方法。在该方法中，测量了一系列含有ZrO ₂的模拟混合物的EDXRF光谱。计算各混合物中Zr的特征KαX射线(15.7keV)下的峰面积，并在峰_{面积和ZrO 2}的％分数之间绘制校准图。从校准图中，获得了 0.1%–10% 的动态范围。根据金刚石粉末测试样品的 XRF 光谱（一式两份），使用峰面积估算 Zr，发现百分比分数为 0.181 ± 0.020。中子活化分析 (NAA) 用于通过 EDXRF 分析中使用的同一组模拟样品进行方法验证。两种方法获得的结果非常一致，这种基于 EDXRF 光谱测定的新开发方法已在 GII 中得到常规使用。