二苯并噻吩硫元素含量标准物质的研制

王海峰; 李佳; 孙国华; 苗雨

doi:10.12338/j.issn.2096-9015.2021.0622

二苯并噻吩硫元素含量标准物质的研制

doi: 10.12338/j.issn.2096-9015.2021.0622

中国计量科学研究院，北京 100029

基金项目: 国家市场监督管理总局科技计划项目（2021MK150）；国家市场监督管理总局能力提升项目（31-ANL1814）。

详细信息

作者简介:
王海峰（1978-），中国计量科学研究院副研究员，研究方向：水分和有机元素计量技术，邮箱：wanghf@nim.ac.cn

计量
- 文章访问数: 344
- HTML全文浏览量: 136
- PDF下载量: 43
- 被引次数: 0
出版历程
- 收稿日期: 2021-11-10
- 录用日期: 2022-03-23
- 网络出版日期: 2022-04-24

Development of Reference Materials for Sulfur Contents of Dibenzothiophene

National Institute of Metrology, Beijing 100029, China

摘要

摘要: 固体和液体燃料的硫元素含量测定，缺乏量值准确可靠的有机纯物质硫元素含量标准物质，不能满足量值溯源的需求。研制了二苯并噻吩硫元素含量标准物质（GBW 06204），采用国际上先进的有机纯物质元素含量定值方法，即根据各组分含量及其分子中待测元素含量，计算得到标准物质的元素含量认定值。其中，有机杂质含量采用了气相色谱-质谱法和差示扫描量热法两种方法联合定值；水分采用卡尔·费休库仑法定值；无机杂质采用灼烧残渣称重法定值。标准物质的特性量值溯源至纯物质质量和温度等SI单位以及原子量上，标准物质的硫元素含量的认定值17.403%，不确定度（U）为0.005%，达到了国际先进水平。该标准物质适用于杜马斯法等有机元素分析仪的校准，可用于油品硫含量标准物质的配制，有利于保障燃料硫元素含量的量值准确可靠。
- 有机元素含量 /
- 二苯并噻吩 /
- 硫 /
- 标准物质 /
- 不确定度
Abstract: Measurement of sulfur content of solid and liquid fuels is restricted by the lack of certified reference material (CRM) of organic pure substance for sulfur, which can not meet the demand for traceability. In this paper, the CRM of dibenzothiophene for sulfur content labeled as GBW 06204 was developed, and an internationally advanced method for determining the elemental content of organic pure substances was adopted, that is, based on the content of each component and its molecular content of the element to be measured, the elemental content of the standard substance was calculated to obtain the determined value. Among them, the organic impurity content was determined by using gas chromatography-spectrometry and differential scanning calorimetry. The water content was determined by Karl Fischer coulometric titration. The inorganic impurity content was determined by the residue on ignition. The certified value of CRM was traceable to the mass of pure substances, temperature, and atomic weight. The certified sulfur content of CRM was 17.403% with an uncertainty (U) of 0.005%, which has reached the international advanced level. This CRM is suitable for the calibration of elemental analyzers such as the Dumas method, and the preparation of CRM of petroleum for sulfur content, which is helpful for the accuracy and reliability of sulfur content results of fuels.
- organic elemental content /
- dibenzothiophene /
- sulfur /
- certified reference material /
- uncertainty

HTML全文

图 1 二苯并噻吩提纯过程照片

注：从左至右分别为提纯0、1、2、3和4次

Figure 1. Photographs of dibenzothiophene purification process

下载: 全尺寸图片幻灯片

图 2 DSC测定的温度—热流曲线

Figure 2. Temperature versus heat flow curve measured by DSC

下载: 全尺寸图片幻灯片

参考文献(17)

[1]	国家质量监督检验检疫总局. 煤中全硫的测定方法: GB/T 214-2007[S]. 北京: 中国标准出版社, 2007.
[2]	国家质量监督检验检疫总局. 煤中全硫测定红外光谱法: GB/T 25214-2010[S]. 北京: 中国标准出版社, 2010.
[3]	American Society of Testing and Measurement (ASTM). Standard test method for total sulfur in coal and coke combustion residues using a high-temperature tube furnace combustion method with infrared absorption: ASTM D5106[S]. West Conshohocken, USA: ASTM, 2008.
[4]	冯涛, 唐兆官. 高温燃烧热导法测定煤中碳氢氮硫[J]. 冶金分析, 2017, 37(12): 71-76.
[5]	国家质量监督检验检疫总局. 轻质烃及发动机燃料和其他油品中总硫含量的测定紫外荧光法: GB/T 34100-2017[S]. 北京: 中国标准出版社, 2017.
[6]	国家石油和化学工业局. 轻质烃及发动机燃料和其他油品的总硫含量测定法紫外荧光法: SH/T0689-2000 [S]. 北京: 中国标准出版社, 2000.
[7]	国家质量监督检验检疫总局. 石油产品硫含量的测定波长色散X射线荧光光谱法: GB/T 11140-2008[S]. 北京: 中国标准出版社, 2008.
[8]	周燕萍, 王雪蓉, 王倩倩, 等. 紫外荧光测硫仪示值校准不确定度的评定[J]. 计量科学与技术, 2020(10): 9-11. doi: 10.3969/j.issn.2096-9015.2020.10.03
[9]	KITAMAKI Y, SHIMIZU Y, YOSHIMURA E. Development of high purity dibutyl sulfide certified reference material(NMIJ CRM 4221-a) for Determination of Sulfur in Fuels[J]. Journal of the Japan Petroleum Institute, 2014, 57(2): 78-83. doi: 10.1627/jpi.57.78
[10]	孙国华, 李佳, 吴冰, 等. 苯甲酸标准物质制备中区域熔融提纯装置的研制[J]. 计量学报, 2014, 35(2): 180-183. doi: 10.3969/j.issn.1000-1158.2014.02.19
[11]	American Society of Materials Measurement (ASTM). Standard test method for purity by differential scanning calorimetry: ASTM E928-03[S]. PA, USA: ASTM international, 2003.
[12]	MA K, WANG H, ZHAO M, et al. Purity determination and uncertainty evaluation of theophylline by mass balance method, high performance liquid chromatography and differential scanning calorimetry[J]. Analytica Chimica Acta, 2009, 57(2): 78-83.
[13]	WANG H, LI J, SUN G, et al. Purity determination of 8-hydroxyquioline aluminum by differential scanning calorimetry[J]. Synthetic Metals, 2009, 159(1-2): 162-165. doi: 10.1016/j.synthmet.2008.06.006
[14]	徐永强, 赵瑞玉, 商红岩, 等. 二苯并噻吩合成方法的改进[J]. 化学试剂, 2003, 25(3): 163-165. doi: 10.3969/j.issn.0258-3283.2003.03.013
[15]	国家市场监督管理总局. 纯度标准物质定值计量技术规范有机物纯度标准物质: JJF 1855-2020[S]. 北京: 中国标准出版社, 2020.
[16]	国家技术监督局. 一级标准物质技术规范: JJF 1006-1994[S]. 北京: 中国质检出版社, 1994.
[17]	International Organization for Standardization (ISO). Reference materials-General and statistical principles for certification: ISO Guide 35[S]. Geneva, Switzerland: ISO, 2006.