气体基本定律在建立气体测量仪计量检定装置中的应用

遵循道尔顿定律建立的双压力法恒湿气体发生器,各项技术指标高于湿度计量一等标准要求,可用于校准和测量湿度仪器及测湿元件;遵循理想气体状态方程及静态容积法配制乙醇标准气体,建立的呼出气体酒精含量探测器检定装置,其不确定度优于被检探测器允许相对误差的三倍以上,可以满足呼出气体酒精含量探测器检定的需要。     

复合式气体报警器检定装置的研制

提出一种新型复合式气体报警器检定方法,根据此方法设计一套复合式气体检测报警器检定装置。该检定装置由工作柜、气瓶存储柜、气体输送气路、流量控制器、气体稀释装置、旋转工作台6部分组成。其中气体输送气路共有6路通道,气体稀释装置的重复性不大于0.5%。旋转工作台可同时对多台仪器进行测量,另外还配备了证书编辑软件。该装置检定结果的扩展不确定度不大于5%(k=2),其中:用于0~100%LEL CH4检定的扩展不确定度为3.0%(k=2);用于0~100μmol/mol H2S检定的扩展不确定度为5.0%(k=2);用于0~100μmol/mol CO检定的扩展不确定度为4.2%(k=2);用于0~20.9%O2检定的扩展不确定度为3.4%(k=2)。该检定装置工作效率高,采用PLC和上位机的控制方式能够实现检定过程自动化测量。该装置主要适用于CH4,H2S,CO,O2气体报警器的检定。     

总悬浮颗粒物测试仪检定结果的不确定度评定

对总悬浮颗粒物测试仪检定结果的不确定度进行了评定,分析了检定过程中不确定度的主要来源,如计量标准、测量重复性、检定装置示值误差等.对各不确定度分量进行了量化,求得检定结果的相对扩展不确定度为1.8%(k=2).对检定结果不确定度评定的合理性进行了验证.     

电导率仪电计与电导池配套检定时检定装置配置的探讨

根据JJF1059－1999《测量不确定度评定与表示》，JJG376－1985《电导仪试行检定规程》，经过测量不确定度分析。探讨了在进行电计与电导池配套检定时，由不同级别的国家电导率指标物质及配套设备组成的检定装置所适合检定的电导率仪，以及检定装置的最佳配置。     

天然气气相色谱仪检定装置的建立

为了保证天然气工业用气相色谱仪分析结果准确可靠和量值溯源有效,依据JJG 1055—2009《在线气相色谱仪》、JJF1033—2016《计量标准考核规范》等规程规范要求,配置建标所需计量标准器,研究开展了重复性试验、不确定度评定、检定结果的验证等工作,建立了天然气气相色谱仪检定装置,通过了国家市场监督管理总局的现场考...     

薄层色谱扫描仪检定方法探讨

为了解决薄层色谱扫描仪没有统一的量值溯源方法和标准装置的问题,建立薄层色谱扫描仪检定方法。通过对薄层色谱扫描仪各部分的结构进行分析,建立了薄层色谱扫描仪检定项目及计量性能要求。采用低压汞灯为标准器进行波长示值误差和重复性检定,采用薄层色谱标准板进行仪器重复性和线性检定。该检定方法能准确评价薄层色谱扫描仪的性能,为薄层色谱扫描仪的量值溯源提供技术支持。     

可移动式微量氧分析仪检定装置研制

研制一种新型可移动式微量氧分析仪检定装置。该装置由标准气体、零点气、脱氧纯化器、减压阀、调节阀、4通阀、5通阀、不锈钢管路、流量控制系统、移动平台等组成。该装置气密性好,15 min内可将装置内氧气浓度由20.9%降至不大于0.1μmol/mol,对于0~10μmol/mol的微量氧分析仪检定结果的扩展不确定度为Urel=1.7%FS(k=2)。该装置满足气体标准物质的连续切换和在线检定的需要,检定时间短,结果准确可靠,可为在线式和非在线式微量氧分析仪的量值溯源提供有效保障。     

在线酸度仪校准装置的研制

为了提高在线酸度监测仪表的计量精度,使计量校准实现动态测量,研究了在线式酸度监测仪的校准方法,并根据校准方法研制了一种在线动态计量检定校准装置,该装置利用国家一级标准物质进行量值传递。整套装置模拟了在线酸度仪的工作状态,工作流速30－250mL／min,校准结果的不确定度为0．01pH,满足校准的要求。     

微波加热测定水泥或粉煤灰中游离氧化钙的方法

本发明公开了微波加热测定水泥或粉煤灰中游离氧化钙的方法及装置。将水泥或粉煤灰与游离氧化钙溶出剂一同装于磨口锥形瓶中,在微波炉中回流加热后,游离氧化钙溶出后通过苯甲酸标准溶液滴定,最终确定试样中的游离氧化钙的含量。装置包括微波炉上连接加热功率旋钮和加热时间旋钮,微波炉内腔置锥形瓶,锥形瓶上端插入一根冷凝管,其冷凝管上端与循环冷却水箱相通连接、其下端与循环水泵相通连接,锥形瓶内腔装有水泥或粉煤灰试样与游离氧化钙溶出介质。     

一种气体仪表检定装置

本发明公开了一种气体仪表检定装置,包括用于安放待检流量计的检定台位,检定台位至少依次连接有滞止容器、音速喷嘴、负压管道及采用变频控制的罗茨真空泵,所述检定台位及其进气口设置于一可封闭的检定室中,且所述真空泵的排气口通过地下管道与该检定室相通。     

溶解氧测定仪示值误差的不确定度评定

对溶解氧测定仪示值误差的不确定度进行了评定。分析了各个不确定度分量,溶解氧测定仪示值误差的扩展不确定度为0．05mg／L。     

A Dissolved Oxygen Analyzer with an Optical Sensor

A serial analyzer of dissolved oxygen, Expert-009, based on the optical detection method is created. The sensitive element of the sensor is a polymer film with a dye—a metal complex of fluorine-substituted porphyrin—distributed in it. The method is based on the quenching of the phosphorescence of the dye by molecular oxygen, which the analyzer recounts to the concentration value by the calibration curve method. The metrological characteristics of the analyzer are determined.     

Determination of nickel,cobalt, copper and uranium in water by cathodic stripping chronopotentiometry with continuous flow

The potential of cathodic stripping chronopotentiometry for the determination of trace metals in a continuous-flow system is investigated. An automated analyzer with a fast rate of data acquisition (250 kHz) is described. The cathodic scans are preceded by adsorptive collection of surface-active metal complexes on the hanging mercury drop electrode. The scans are done by passing a constant current of between 0.8 (in deaerated solution) and 60 μA (in solutions saturated with air) through the working electrode. Copper, uranium, and nickel can be determined in the presence of dissolved oxygen, but the sensitivity for nickel is then much reduced. The sensitivity of stripping chronopotentiometry in the presence of dissolved oxygen is similar to that of fast linear-sweep voltammetry in the absence of dissolved oxygen. The limits of detection were 0.1 nM Ni, 0.1 nM Co, 1.8 nM Cu and 1.6 nM U, when the measurements were preceded by 60-s stirred adsorption; in the presence of dissolved oxygen the limit of detection for nickel was higher at 0.6 nM, and cobalt could not be determined, as its peak was located on top of the oxygen peak. The determinations of copper and uranium were not adversely affected by dissolved oxygen. The limits of detection can be lowered further by using a prolonged collection period (up to 300 s). The technique was successfully tested by measuring nickel with continuous flow in water pumped on board of a small vessel in the Tamar estuary.     

The Management of Dissolved Oxygen by a Polypropylene Hollow Fiber Membrane Contactor Affects Wine Aging

Background: Numerous oenological practices can cause an excess of dissolved oxygen in wine, thus determining sensory and chromatic defects in the short- to long-term. Hence, it is necessary to manage the excess of oxygen before bottling. Methods: In this study, the management of the dissolved oxygen content by a polypropylene hollow fiber membrane contactor apparatus was performed in two wines from different grape varieties (Aglianico and Falanghina). The wines were analyzed after an 11-month aging. Anthocyanins and acetaldehyde content were evaluated by HPLC. In addition, other phenolic compounds and chromatic characteristics were analyzed by spectrophotometric methods. NMR and HR ESIMS analyses were conducted to evaluate the amount of pyranoanthocyanins and polymeric pigments. Results: After 11 months of aging, in both wines a decrease of free and total SO₂ with respect to initial values was detected. In the wines with the highest dissolved oxygen levels, a more remarkable loss was observed. No significant differences in terms of color parameters were detected. In red wine with the highest oxygen content, a massive formation of polymeric pigments and BSA reactive tannins was observed, as opposed to wines with lower oxygen levels. Conclusion: The study demonstrated that the membrane contactor can prove a successful tool to manage dissolved oxygen in wines as to prevent their oxidative spoilage.     

A multisyringe flow injection Winkler-based spectrophotometric analyzer for in-line monitoring of dissolved oxygen in seawater

An integrated analyzer based on the multisyringe flow injection analysis approach is proposed for the automated determination of dissolved oxygen in seawater. The entire Winkler method including precipitation of manganese(II) hydroxide, fixation of dissolved oxygen, dissolution of the oxidized manganese hydroxide precipitate, and generation of iodine and tri-iodide ion are in-line effected within the flow network. Spectrophotometric quantification of iodine and tri-iodide at the isosbestic wavelength of 466 nm renders enhanced method reliability. The calibration function is linear up to 19 mg L⁻¹ dissolved oxygen and an injection frequency of 17 per hour is achieved. The multisyringe system features a highly satisfying signal stability with repeatabilities of 2.2% RSD that make it suitable for continuous determination of dissolved oxygen in seawater. Compared to the manual starch-end-point titrimetric Winkler method and early reported automated systems, concentrations and consumption of reagents and sample are reduced up to hundredfold. The versatility of the multisyringe assembly was exploited in the implementation of an ancillary automatic batch-wise Winkler titrator using a single syringe of the module for accurate titration of the released iodine/tri-iodide with thiosulfate.     

湿法脱硫中亚硫酸盐非催化氧化本征动力学

亚硫酸盐的氧化是湿法烟气脱硫工艺中的重要过程. 利用间歇式反应装置, 研究了亚硫酸盐非催化氧化的本征反应动力学. 结果表明, 该反应分为两个阶段进行, 即富氧区的快速反应和贫氧区的慢速反应. 在富氧区, 亚硫酸盐和溶解氧的分级数分别为1.0和1.0, 反应的表观活化能为49.3 kJ•mol^－1; 在贫氧区, 亚硫酸盐和溶解氧的分级数分别为2.0和0, 反应的表观活化能为122.6 kJ•mol^－1. 对反应的机理进行了预测, 结果与实验现象有较好的吻合.     

苯酚抑制条件下亚硫酸盐氧化的本征反应动力学

亚硫酸盐的氧化是湿法烟气脱硫工艺中的重要过程. 利用间歇式反应装置, 研究了苯酚抑制条件下亚硫酸盐氧化的本征反应动力学. 结果表明, 该复杂的反应过程分两个阶段进行, 即富氧区的快速反应和贫氧区的慢速反应. 在富氧区, 苯酚、亚硫酸盐和溶解氧的分级数分别为－0.5, 1.0和2.0, 反应的表观活化能为99.2 kJ•mol－1; 在贫氧区, 苯酚、亚硫酸盐和溶解氧的分级数分别为－0.5, 1.5和0, 反应的表观活化能为 129.7 kJ•mol－1. 结合实验结果, 对苯酚抑制条件下亚硫酸盐氧化的宏观反应动力学过程进行了推断.     

Indirect determination of formaldehyde by alternating-current voltammetry at a hanging mercury drop in the presence of oxygen

An alternating-current voltammetric procedure has been developed for the indirect determination of formaldehyde as its hydrazone at a stationary hanging mercury drop over the formaldehyde concentration range from 0.2 to 15 mg/L in a buffer solution of pH 5.6 ± 0.4 without removing dissolved oxygen. An EKOTEST-VA miniature voltammetric analyzer connected to a computer was used. The detection limit for formaldehyde in the proposed procedure was 0.2 mg/L.     

Experimental characterization of straight spectrometer slits

A technique for calibrating slit width for straight spectrometer slits based on the diffraction of laser radiation is described. Related slit properties and calibration apparatus are discussed.     

Determination of fructose using immobilized glucose isomerase in an on-line analyzer

The determination of fructose using a continuous analyzer based on analyte conversion in enzyme reactors followed by amperometric oxygen measurement is described. Two experimental setups were compared, allowing determinations in the ranges 0–180 and 0–25 mM fructose. In the former, fructose was continuously dialyzed versus a buffer stream conducting fructose to an enzyme reactor. This reactor contained two immobilized enzyme preparations, one with immobiized glucose isomerase (E.C. 5.3.1.5) that isomerized fructose to glucose and another that subsequently oxidized the former glucose by immobilized glucose oxidase (E.C. 1.1.3.4) with the consumption of dissolved oxygen. In the latter set-up, fructose was first isomerized in a glucose isomerase reactor, then glucose was continuously dialyzed and oxidized by glucose oxidase as above. This set-up was run in continuous operation for 1000 measurement cycles with a total decrease in response less than 15%.