气相色谱—质谱联用仪校准装置
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本计量标准由三种国家二级标准物质、铂电阻温度计、气相色谱仪检定装置等部分组成,
1、八氟萘-异辛烷溶液标准物质,100pg/μl。该标准物质用于测试GC-MS负CI和EI源灵敏度,使用微量注射器进1.0μl标准物质,提取m/z=272离子,再现质量色谱图,根据公式(1)计算S/N。
S/N=H 272 /H噪声 (1)
式中:
H272:提取离子(m/z)的峰高
H噪声:基线噪声。
2、苯甲酮-异辛烷溶液标准物质,10.0ng/?L。该标准物质用于测试GC-MS正CI源灵敏度,使用微量注射器进1.0μl标准物质,提取m/z=183离子,再现质量色谱图,根据公式(1)计算S/N。
3、六氯苯-异辛烷溶液标准物质,10.0ng/?L。该标准物质用于测试GC-MS测量重复性,使用微量注射器进1.0μl标准物质,连续测量六次,提取六氯苯特征离子m/z=284,再现质量色谱图,按质量色谱峰进行面积积分,根据公式(2)计算RSD:
×100%(2)
式中:
RSD-相对标准偏差(%);
xi-六氯苯第i 次测量峰面积;
-六氯苯6次测量峰面积算术平均值;
i-测量序号。
This metrological standard comprises three national secondary reference materials, a platinum resistance thermometer, a gas chromatograph verification device, and other components.
1. Octafluoronaphthalene-isooctane solution reference material, 100 pg/μL. This reference material is used to test the sensitivity of GC-MS negative CI and EI sources. Inject 1.0 μL of the reference material with a microsyringe, extract the ion at m/z = 272 to generate the mass chromatogram, and calculate the signal-to-noise ratio (S/N) according to Equation (1):
$S/N = H_{272} / H_{ ext{noise}}$ (1)
Where:
$H_{272}$: Peak height of the extracted ion (m/z)
$H_{ ext{noise}}$: Baseline noise.
2. Benzophenone-isooctane solution reference material, 10.0 ng/μL. This reference material is used to test the sensitivity of GC-MS positive CI source. Inject 1.0 μL of the reference material with a microsyringe, extract the ion at m/z = 183 to generate the mass chromatogram, and calculate the S/N ratio according to Equation (1).
3. Hexachlorobenzene-isooctane solution reference material, 10.0 ng/μL. This reference material is used to test the measurement repeatability of GC-MS. Inject 1.0 μL of the reference material with a microsyringe, perform six consecutive measurements, extract the characteristic ion at m/z = 284 of hexachlorobenzene to generate the mass chromatogram, conduct area integration based on the mass chromatographic peaks, and calculate the relative standard deviation (RSD) according to Equation (2):
$ imes100\%$ (2)
Where:
$ ext{RSD}$: Relative standard deviation (%)
$x_i$: Peak area of the i-th measurement of hexachlorobenzene
$ar{x}$: Arithmetic mean of the peak areas of six measurements of hexachlorobenzene
$i$: Measurement serial number.
提供机构:
国家计量科学数据中心创建时间:
2019-12-11



