痕量臭氧标准气体发生装置的研制

研制了一种新型的痕量臭氧标准气体发生装置,可输出设定量值的稳定臭氧标准气体,24 h连续运行,输出量值相对标准偏差小于1.2%。发生臭氧浓度范围为25～1 000 nmol/mol。该装置可输出一组按顺序增大或减小的臭氧标准气体,可与被校准仪器连接进行比对试验或检定校准。与美国国家标准局(NIST)臭氧基准测量装置SPR41比对试验研究表明,研制的臭氧标准气体发生装置具有很好的准确性,定值不确定度小于1%(k=2)。     

烟道气国际比对中低浓度一氧化碳的精确测量

研究了烟道气体中低浓度一氧化碳(CO)的精确分析方法.结果显示,使用非色散红外光谱法的重复性明显优于气相色谱法,但烟道气中高浓度二氧化碳( CO2)的存在会影响光谱法对CO的精确测量,因此测量样品时采用含有CO2成分的标准气体作为标准.由不确定度评定结果及比对样品重复性测量结果可知,本方法精确度高.通过参加国际计量局物...     

二氧化碳中一氧化氮气体标准物质研制

研制二氧化碳中一氧化氮气体标准物质。以高纯二氧化碳和一氧化氮气体标准物质为原料,采用称量法制备二氧化碳中一氧化氮气体标准物质,用气体分析仪对制备的标准物质浓度进行检测,并对该标准物质定值结果的不确定度进行评定。研制的二氧化碳中一氧化氮气体标准物质中一氧化氮的浓度为5,25,50 μmol/mol,相对扩展不确定度为3.0% (k=2)。该气体标准物质具有良好的均匀性和稳定性,可用于食品级二氧化碳分析方法的确认和评价。     

用天然气气相色谱分析仪快速分析天然气组分及性能参数

介绍用天然气气相色谱分析仪分析天然气中无机组分、有机组分和热值的方法,确定了分析方法和条件,该方法测量结果的相对标准偏差小于1%。采用该方法对制备的标准气体进行了考察,并将该方法用于天然气气体标准物质的性能评价和国际实验室间的比对,天然气组分含量比对相对误差在±1%之内,热量值比对相对误差在±3%之内,取得了国际等效性。     

可调样量进样技术在全面禁止核试验条约氙监测中的应用

氙的气相色谱测量是全面禁止核试验条约放射性核素核查的重要内容之一。应用设计的可调调样量进样装置,实现了单一浓度标准气体样品的多点外标曲线刻度和负压条件下样品气体的色谱进样测量,测量结果表明:氙样品浓度测量结果的相对标准偏差(RSD,n=3)小于0.50%,不确定度为1.50%;同时,本进样装置可以实现对未知容积和压力的测量,测量结果的不确定度分别为1.04%和1.05%。     

氮中低含量一氧化碳气体标准物质的定值方法

介绍氮中低含量CO气体标准物质定值的方法，对气体滤光相关分析法进行了探讨，给出了该方法的实验务件和精密度。将气体滤光相关分析法的测量值与重量法配制值、气相色谱法分析值进行了比对。气体滤光相关分析法重现性好，分析结果准确、可靠，     

氮气中六氟化硫气体标准物质的研制

建立了制备氮气中六氟化硫气体标准物质的方法。以称量法制备气体标准物质并计算定值,采用气相色谱法对制备的气体标准物质的均匀性和稳定性进行考察。将所制备的标准物质与中国计量院提供的氮气中六氟化硫气体标准物质进行比对分析验证,确保了气体标准物质量值的准确可靠。结果表明,所研制的浓度为10μL/L的氮气中六氟化硫气体标准物质定值的扩展不确定度为2%,贮存有效期为1年,完全能够满足电力部门仪表的检定与校准要求。     

组合回归分析法——盐酸标准滴定溶液浓度的标定

介绍和讨论了计量学中组合测量的概念和方法.在最小二乘法原理的基础上,结合化学计量学方法和化学滴定分析计量测试的特点,并参照 GB/T601-2002 标准,设计出盐酸标准滴定溶液浓度的组合回归标定方法,其内容包括:工作基准试剂 Na2CO3 的组合称量操作程序及其数据处理;试样溶液的组合滴定操作程序及其数据处理;常规测...     

氢同位素气体在线分析装置研制及分析方法建立

为了实现氢同位素气体在线检测,利用气体低气压辉光放电性质,设计加工了氢同位素在线测定装置并建立了辉光放电原子光谱法在线测定氢同位素的分析方法。该装置由辉光放电管、激发光源、真空–微量进气系统、光谱仪及数据采集系统等部件组成。采用不同含量的系列氕氘气体作为标准气体,绘制标准工作曲线,建立了氢同位素在线检测分析方法,氕氘气体的检出限均为0.04%,氕浓度、氘浓度和氕氘浓度比测量的相对标准偏差分别为3.6%,5.2%和2.4%(n=6)。该分析装置性能稳定可靠,操作简单,可实现氢同位素气体在线检测。     

CCQM-K74国际比对中二氧化氮浓度的测量

介绍了国际比对样品中10μmol/mol NO2气体浓度精确分析方法的建立过程。该方法的建立包括标准物质的制备、分析仪器的选择和测量结果的不确定度3个主要的方面。标准物质的制备及其量值的不确定度评价采用了气体标准物质定值的基准方法——称量法。对傅立叶变换红外光谱法(FTIR)和化学发光光谱法进行了比较研究。确定了更适合于本次国际比对样品的分析方法为化学发光光谱法,测量结果的相对扩展不确定度为1.0%(k=2)。本次比对的最终结果报告显示,所建立的分析方法准确可靠。     

Mass spectrometric analysis of carbon monoxide-nitrogen mixtures

A method for the analysis of gas mixtures containing both carbon monoxide and nitrogen, by using a single-focussing mass spectrometer, is described. It involves measurement of the mass spectrum of a gas sample before and after conversion of the carbon monoxide present into carbon dioxide by means of the Schütze catalyst.     

Determination of carbon monoxide with palladium chloride

The gas sample transfer apparatus, as shown in Fig. 1, was designed to facilitate the analysis of several carbon monoxide samples during a normal work day. With this apparatus, gas samples were accurately transferred from the Tedlar bags leak free through the system to the reaction flask. Changing from one gas concentration to another was greatly simplified by using the quick-connect fittings; gas volumes were readily calculated from direct readings taken from the differential pressure gauge.Tests were conducted to assess the performance of the PdCl₂ method and the sampling system with various gas mixtures. The proposed PdCl₂ method utilizing this particular sampling scheme is capable of successfully measuring carbon monoxide in nitrogen cylinder gas at levels of 0.1, 0.05, and 0.01% with expected average recoveries of 96, 96, and 93%, respectively.     

Experimental Study of Nitrogen Oxides and Ozone Generation by Corona-Like Dielectric Barrier Discharge with Airflow in a Magnetic Field

We investigated nitrogen monoxide, nitrogen dioxide and ozone generation for corona-like dielectric barrier discharge in a stationary magnetic field with airflow. The magnetic field was produced by the permanent magnet. We showed that nitrogen monoxide could be easily generated at relatively low voltages, by application of a magnetic field on the hollow needle to mesh with a dielectric barrier discharge. For higher voltages generation of nitrogen monoxide falls to zero, and generation of nitrogen dioxide and ozone with increasing voltage increases. We also demonstrated that simultaneous application of the magnetic field with airflow through the needle electrode affects the transition of the discharge from the high to the low voltage regime. This transition is accompanied by important changes in the production of nitrogen oxides and ozone. Changes in the discharge regime are reflected by changes in the voltage–current waveforms. The obtained results could be interesting for various biomedical applications or bacterial decontamination of surfaces.     

Development of an automatic static volumetric method based on loop injection

A prototype of an automatic static volumetric method based on the injection of a pure compound by means of a loop instead of a manual syringe was constructed, fitting for both laboratory use and field applications. The crucial point, the evaluation of the loop volumes, was solved developing two techniques allowing traceability to SI units. Gas mixtures of nitrogen monoxide (NO) in nitrogen in the 10⁻⁹ V/V range and carbon monoxide (CO) in air in the 10⁻⁶ V/V range were generated and successfully compared to other primary calibration techniques. Relative expanded uncertainties (k=2) of 1.1% (compared to 0.8% of the manual static volumetric method [1]) for NO gas mixtures and 0.3% CO gas mixtures were estimated.     

Study on the Physical and Chemical Characteristics of DBD: The Effect of N2/O2 Mixture Ratio on the Product Regulation

Plasma Chemistry and Plasma Processing - The chemical product behaviors of dielectric barrier discharge (DBD) in N2/O2 gas mixtures are investigated. Besides ozone mode and nitrogen oxides mode, a...     

高灵敏度的脉冲氦离子化检测器分析混合气体中的Kr、Xe

使用高灵敏度的脉冲氦离子化检测器（PDHID）气相色谱法对Kr、Xe浓度进行定量分析,并通过采用反应床除去杂质气体或与Kr、Xe难以分离的干扰组分N2、CH4和CO等,可使最低检测限达到Kr为7．931×10^-8、Xe为7．186×10^-8．对Kr的测量相对偏差在2％以内,对Xe的测量相对偏差在6％以内．     

Spectroscopic investigations of high-power laser-induced dielectric breakdown in gas mixtures containing carbon monoxide

Large-scale plasma was created in gas mixtures containing carbon monoxide by high-power laser-induced dielectric breakdown (LIDB). The composition of the mixtures used corresponded to a cometary and/or meteoritic impact into the Earth's early atmosphere. A multiple-centimeter-sized fireball was created by focusing a single 85 J, 450 ps near-infrared laser pulse into the center of a 15 L gas cell. The excited reaction intermediates that formed in various stages of the LIDB plasma chemical evolution were investigated by optical emission spectroscopy (OES) with temporal resolution. Special attention was paid to any OES signs of molecular ions. However, carbon monoxide cations were registered only if their production was enhanced by Penning ionization, i.e., excess He was added to the CO. The chemical consequences of laser-produced plasma generation in a CO-N 2-H 2O mixture were investigated using high resolution Fourier-transform infrared absorption spectroscopy (FTIR) and gas chromatography (GC). Several simple inorganic and organic compounds were identified in the reaction mixture exposed to ten laser sparks. H 2 (18)O was used to avoid possible contamination. The large laser spark triggered more complex reactivity originating in carbon monoxide than expected, when taking into account the strong triple bond of carbon monoxide causing typically inefficient dissociation of this molecule in electrical discharges.     

Modification of zeolites usingin situ generated active species in the gas phase: II. Redox processes over the Mo5+ isolated sites in zeolites ZSM-5 and beta

The redox ability of isolated Mo⁵⁺ cations in model MoH-beta and MoH-ZSM-5 systems is studied byin situ ESR. The oxidation of reduced samples by nitrogen monoxide at 20°C proceeds much faster than oxidation by oxygen. The interaction between Mo⁵⁺ ions and propene at 20°C results in the formation of a complex in which the oxidizability of Mo(V) by NO is substantially enhanced. UV irradiation increases the oxidation rate for Mo⁵⁺ ions in HZSM-5 by nitrogen monoxide at 20°C, indicating the possibility for the photochemical activation of the process. The step of active site reduction during the interaction of the samples with the H₂ + NO + He gas mixtures of various compositions at 500°C is fast, and the dynamic equilibrium of the redox Mo(V) ai Mo(VI) reaction is shifted to the left Deceased.     

Nonstationary effects in ozone generation by barrier discharges in N<Subscript>2</Subscript>/O<Subscript>2</Subscript> mixtures

The yield of ozone in barrier discharges in oxygen–nitrogen mixtures containing 0.001 to 40% of nitrogen is investigated experimentally. Phenomena of the nonstationarity of processes of ozone generation that differ from the known ozone-zero phenomenon (OZP) apparent in the reduced efficiency of ozone generation in very high purity oxygen at long periods (from hours to tens of hours) of ozonator operation are found. It is established that the characteristic times (from minutes to tens of minutes) of ozone attaining stationary values after changes in the discharge parameters indicate slow adjustment of the surface condition of insulators and thus the heterogeneous decay of ozone to more rapidly changing flows of neutral and charged particles from gas discharge plasma on the surfaces of dielectrics. The possibility of such a scenario is confirmed using a new analytical approach and numerical calculations of the plasma–chemical kinetics of N₂/O₂ mixtures presented in the accompanying theoretical study.