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以高纯硫化氢和高纯甲烷为原料,采用称重法制备甲烷中硫化氢气体标准物质。采用气相色谱法(FPD)进行均匀性、稳定性考察。结果表明用称量法制备的浓度为10μmol/mol的甲烷中硫化氢气体标准物质均匀性良好,稳定性可靠,符合气体标准物质制备的要求。该气体标准物质相对扩展不确定度Urel=2%,k=2。 相似文献
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《中国测试》2020,(8)
介绍一种三聚甲醛挥发经过转换器加热裂解得到甲醛的新方法,通过补充适量的平衡气进行稀释,采用称量法制备得到目标浓度的高压瓶装甲醛气体标准物质。实验表明(210±5)°C为最佳的裂解温度,采用气相色谱质谱联用的方法对裂解产物进行分析,甲醛的纯度为99.525%。使用经过内壁特殊处理的铝合金气瓶对研制的氮中甲醛气体标准物质进行存储,量值水平1~5μmol/mol,成功通过国家二级标准物质定级评审,标物编号为GBW(E)083617。将研制的4.92μmol/mol氮中甲醛气体标准物质,气瓶编号L55016195,送至英国国家物理研究院进行比对,测试结果为4.81μmol/mol,采用En值进行判定,比对结果为满意,也进一步验证称量法制备定值得到的瓶装甲醛气体标准物质的准确性。 相似文献
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研制了2,3,4-三氯苯甲醚标准物质,介绍了其制备与定值方法。将制备的2,3,4-三氯苯甲醚标准物质分装成500瓶样品,随机抽取其中11瓶做均匀性检验,经F检验和t检验,结果表明在95%置信范围内样品均匀性良好。按短期与长期稳定性分别进行稳定性检验,结果表明在常温20℃下,2,3,4-三氯苯甲醚的稳定期不少于12月。采用液相色谱法和差示扫描量热法2种不同原理的方法对2,3,4-三氯苯甲醚标准物质纯度定值及不确定度评定,并采用液相色谱标准添加的方法确认了2,3,4-三氯苯甲醚标准物质中的主要杂质2,3,6-三氯苯甲醚。定值结果为99.56%± 0.40%(k=2)。 相似文献
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《计量技术》2019,(12)
介绍了两种静态容量法制备不同浓度的挥发性有机物(VOCS)混合气体样本,利用稀释钢瓶装标准气体做标准曲线进行定值分析,其中稀释气体法所配制得到的气体样本在较高浓度范围内的相对误差较小,配制结果与理论浓度误差均在5%左右。而稀释液体法的配制精确度整体上不如稀释气体法,同时从相对误差分布可以看出,稀释液体法更适用于较低浓度气体的配制,在较高浓度范围时误差增长到不可接受的程度。利用稀释气体法制备的不同浓度的模拟样本绘制标准曲线,其线性度良好,且优于稀释液体法。因此,采用静态容量法和稀释气体法结合作为实验室模拟样本制备的方法,引入的方法误差较小且制备结果具有良好的线性。 相似文献
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National and international measurements are underpinned by accurate, low concentration standards. These standards are typically produced gravimetrically, or volumetrically, by a series of dilutions of the pure material by the balance gas. This blend technique is time-consuming and may involve the handling of pure, hazardous material. These problems have been overcome by developing a novel blend technique whereby the process gas stream, from an appropriate permeation tube, was cryogenically trapped in an aluminum cylinder. The permeation rate of the component is monitored by real time mass determinations using a magnetic suspension balance system. With the combination of the real-time calculated permeation rate, plus the use of a dilution system, a one step production of a very low concentration of the minor component in nitrogen gas can be achieved. This method was used to prepare low μmol/mol standards of propane, a known stable compound. Analysis of a conventional gravimetrically prepared 10 μmol/mol propane standard and a cryogenically prepared standard via a permeation gas stream resulted in agreement between the two of <0.1% at 10 μmol/mol, confirming the accuracy of the permeation method. After confirmation of the validity of the permeation/cryogenic trapping system, the propane permeation tube was replaced with a methyl mercaptan tube (a toxic, reactive compound) in balance nitrogen. After cryogenically trapping the methyl mercaptan output stream from the permeation system into a cylinder, the output stream and the cylinder gas mixture were analyzed. The results showed agreement of <0.6% for methyl mercaptan at 5, 10, 15, and 20 μmol/mol to the expected blend concentration, thereby demonstrating the validity of the method. 相似文献
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Primary gravimetric gas cylinder standards containing 30 volatile organic compounds (VOCs) in nitrogen were prepared using a procedure previously developed to prepare gas mixture cylinder standards of VOCs at the 5 nmol/mol level. This set of primary standards was intercompared to existing gas cylinder standards, containing as many as 19 of the 30 volatile organics present in these new primaries, using gas chromatography with a hydrogen flame ionization detector coupled with cryogenic preconcentration. The linear regression analysis showed excellent agreement among the standards for each compound. Similar mixtures containing many of these compounds in treated aluminum gas cylinders have been evaluated over time and have shown stability for as much as 10 years. The development of these 30-component primary standards led to the preparation and certification of a reissue of Standard Reference Material (SRM) 1804 at the nominal amount-of-substance fraction of 5 nmol/mol for each analyte. A lot of 20 cylinders containing the mixture was prepared at NIST following previously demonstrated protocols for preparation of the cylinders. Each cylinder was analyzed against one cylinder from the lot, designated as the "lot standard," for each of the 30 compounds. As a result of the uncertainty analysis, the data showed that rather than declaring the lot homogeneous with a much higher uncertainty, each cylinder could be individually certified. The expanded uncertainty limits ranged from 1.5 to 10% for 28 of the 30 analytes, with two of the analytes having uncertainties as high as 19% in those SRM cylinders certified. Due to stability issues and some high uncertainties for a few analytes in 2 of the samples, 18 of the 20 candidate SRM samples were certified. These volatile organic gas mixtures represent the most complex gas SRMs developed at NIST. 相似文献
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Robert F. Berg Stuart A. Tison 《Journal of research of the National Institute of Standards and Technology》2004,109(4):435-450
We describe two primary standards for gas flow in the range from 0.1 to 1000 μmol/s. (1 μmol/s ≅ 1.3 cm3/min at 0 °C and 1 atmosphere.) The first standard is a volumetric technique in which measurements of pressure, volume, temperature, and time are recorded while gas flows in or out of a stainless steel bellows at constant pressure. The second standard is a gravimetric technique. A small aluminum pressure cylinder supplies gas to a laminar flow meter, and the integrated throughput of the laminar flow meter is compared to the weight decrease of the cylinder. The two standards, which have standard uncertainties of 0.019 %, agree to within combined uncertainties with each other and with a third primary standard at NIST based on pressure measurements at constant volume. 相似文献
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G. D. Mitchell A. A. Bell 《Journal of research of the National Institute of Standards and Technology》1991,96(5):547-550
The coulometric method presented here is a reliable method for the direct analysis of CO2/air cylinder gas mixtures. It is based on Faraday’s laws of electrolysis and therefore no external standardization is required. A series of CO2/air cylinder gas mixtures ranging in concentration from 300 to 375 µmol/mol (ppm) were analyzed and the results compared to those results obtained by non-dispersive infrared (NDIR) analysis with traceability to gravimetric standards. The coulometric method is rapid, sensitive, precise, and with the proper experimental controls, will yield accurate results. 相似文献
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提出一种基于FTIR的氟化氢标准气体分析方法,使用其特征吸收区域(波数4100~4300cm-1)进行定量分析。通过稀释方法形成120、 100、 80.0、 60.0、 40.0、 20.0μmol/mol共6个浓度点的氟化氢标准气体,并对其重复性、标准曲线线性、检出限进行考察。结果显示:在20.0~120μmol/mol范围内仪器响应值与标气浓度呈线性,R2为0.9979; 各浓度点的重复性介于0.34%~1.1%之间; 检出限约为2.04μmol/mol。 相似文献
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目前普遍采用称量法制备标准气体,在此过程中气瓶体积膨胀所引入的空气浮力的不确定度贡献不可忽视。设计了一个气瓶充气膨胀率测量装置,该装置可以控制气瓶内充入气体的压力,并利用精密移液管测量气瓶体积的膨胀量,从而准确计算出气瓶的充气膨胀率。利用该装置对国内常见的2L、4L和8L铝合金气瓶进行了测量,结果显示气瓶体积的膨胀与充入气体的压力近似成线性正相关。而且气瓶外观体积越大,充气膨胀率的数值越大,量值之间也呈现出较强的相关性。基于获得的气瓶充气膨胀率数据,可以进一步降低气瓶体积膨胀对瓶内充入气体质量的不确定度贡献,从而使气体质量的计算更加精确。 相似文献
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Natural gas liquid standards consist of various components primarily in the C1-C6 range; they are available in three types of cylinder packages: piston cylinders and two other types of standard cylinders with eductor tubes. The three cylinder packages have different operation conditions and thus a sample may behave differently in each of the packages. The piston cylinder maintains the components in a single liquid phase at a constant pressure, while the standard cylinders maintain the components as a two-phase mixture. Typically, the components may distribute between the two phases in different concentrations depending on the various thermodynamic variables, such as temperature, pressure, and volume. This study will examine the integrity of the sample in the three cylinder packages during a controlled cylinder depletion. The results for the various cylinders will be compared with a theoretical model of the experiments. 相似文献