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。     

酶标分析仪检定用中性滤光片的校准

提出酶标分析仪检定用中性滤光片的校准方法,并用校准实例对校准方法进行了验证。结合校准方法,根据JJF 1059.1—2012《测量不确定度评定与表示》建立了数学模型,不确定度的来源有测量结果的重复性、分光光度计透射比误差、分光光度计杂散辐射、中性滤光片年稳定性、中性滤光片均匀性,按该校准方法校准的中性滤光片,校准结果的不确定度为U=0.005(k=2),校准结果能够满足JJG 861—2007《酶标分析仪检定规程》对中性滤光片不确定度U≤0.01(k=2)的要求,可用于开展酶标分析仪吸光度值的校准工作。     

比色法余氯在线分析仪校准方法

建立比色法余氯在线分析仪的校准方法。比色法余氯在线分析仪的校准包括仪器示值误差、测量重复性和示值稳定性3个项目。根据实验数据,结合各仪器的出厂技术指标要求,综合分析得出比色法余氯在线分析仪的计量性能指标：示值误差在±10%内,重复性不大于3%,示值稳定性在±10%内。示值误差测量结果的相对扩展不确定度为2.8%。该方法可用于评价比色法余氯在线分析仪的计量特性。     

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。     

电解法微量溶解氧分析仪校准装置的研制

基于法拉第电解定律研制电解法微量溶解氧分析仪校准装置。利用理论计算确定校准装置的技术指标及水中微量溶解氧浓度的不确定度,经与比色法比对,该装置用于校准微量溶解氧分析仪的可行性得到验证。     

环境空气监测气体分析仪在线校准装置研制

设计一种新型的膜渗透动态配气系统,将动态配气膜渗透技术、基体空气标准添加方法、大气采样技术相结合,研制环境空气监测气体分析仪在线校准装置.该装置实现了环境空气污染组分SO2、NO2、CO在线监测仪的连续、实时、基体添加校准,校准不确定度小于3％(k=2).设计的长寿命膜渗透动态配气系统制备的标准气体混合物,可以连续使用...     

非均匀梯度尿液分析仪测量不确定度评定

对非均匀梯度尿液分析仪测量不确定度进行评定。分别采用对称区间不确定度评定方法、选择校准点左右两侧分辨力较大者进行不确定度评定的方法、不对称区间不确定度评定方法对非均匀梯度尿液分析仪测量不确定度进行评定。采用常规的对称区间不确定度评定方法所得出的置信区间左右对称,不符合这类仪器低浓度范围分辨能力高于高浓度范围分辨能力的特性。如果选择校准点左右两侧分辨力较大者进行不确定度评定,虽较为稳妥,但其置信区间宽,不确定度偏大,测量结果准确度偏低。而通过不对称区间不确定度评定方法所得出的置信区间,左侧比右侧窄,且与仪器梯度相符,适合用于非均匀梯度尿液分析仪测量不确定度的评定。     

气相色谱法测定丙烯中的微量氧

用气相色谱法分析丙烯中的微量氧。先将液态丙烯汽化成气态,用气体进样阀将气态丙烯样品进样到气相色谱仪中,由5A分子筛填充柱进行分离,用TCD检测器检测,外标法定量。标准气体测定结果的相对标准偏差不大于1.076%(n=5),丙烯样品中氧含量的检出限为1.0mL/m3。用该方法对实际丙烯样品进行了分析。     

动态体积法乙醇气体发生装置的研制

根据呼出气体酒精含量检测仪检定工作需要,基于饱和蒸汽原理,研制了一种乙醇气体发生装置。该装置能够持续发生空气中乙醇气体,出口乙醇气体温度为(34±0.06) ℃、乙醇气体质量浓度误差绝对值最大为0.011 mg/L,相对扩展不确定度不大于3.2%,产生乙醇气体的稳定性不大于1.4%。采用Pt100铂电阻温度计对出口乙醇气体温度进行验证,用精密酒精检测仪和气相色谱仪对装置发生的乙醇气体质量浓度进行验证,该装置满足JJG 657—2019 《呼出气体酒精含量检测仪检定规程》对空气中乙醇气体发生源的要求,能够用于呼出气体酒精含量检测仪的量值传递。     

石油产品库仑氯分析仪校准方法

建立石油产品库仑氯分析仪的校准方法.根据仪器原理及使用情况,选取仪器的示值误差和重复性作为石油产品库仑氯分析仪的主要计量特性,讨论了各个计量特性的校准方法.用该方法对两种型号的仪器进行校准,仪器在不同测量段的示值误差和重复性有较大差异,因此分段制定技术指标.当测量质量浓度小于10.0 mg/L时,示值误差不大于±0.6...     

有机-无机杂化材料膜制备生物传感器用于在线生化需氧量的测定

用溶胶-凝胶与接枝共聚物组成的有机-无机杂化材料固定皮状丝孢酵母制备BOD生物传感器,在研制的在线BOD监测仪上考察其性能。结果表明,该传感器线性高达85．0mg／L BOD,稳定性良好、使用寿命长,可连续使用90d以上,保存14个月后仍可保持70％以上的活性。本方法用于实际样品分析,得到了与传统的5d法较一致的结果,可用于污水的在线监测。     

石油产品微量残炭测定仪的校准

通过分析石油产品微量残炭测定仪的工作原理,参考相应的国家技术规范,建立石油产品微量残炭测定仪的校准方法,提出了示值误差、重复性等校准项目。采用残炭值为2.03%的油品残炭标准物质对石油产品微量残炭测定仪进行校准,其示值误差为0.04%,重复性为0.03%,对石油产品微量残炭测定仪示值误差测量结果的不确定度进行了评定,其扩展不确定度为0.15%(k=2)。该校准方法切实可行,可用于石油产品微量残炭测定仪的校准。     

基于氦离子化气相色谱法测定微量氧、氮的影响因素

探讨氦离子化气相色谱法测定样品中微量氧、氮含量的影响因素。采用控制变量法,对色谱柱温度、进样流量、进样管道环境及极化电压等因素对微量氧、氮测定结果的影响进行讨论和分析。结果表明,当色谱柱温度为25~45℃时,色谱柱对氧、氮吸附量最小;当进样流量不小于70 mL/min时,微量氧、氮测定结果受外界干扰最小;当极化电压为80~160 V时,氧、氮具有最佳的响应值;初次测定样品中微量氧、氮含量时,需使进样管道表面吸附的氧、氮处于饱和状态,以便获得理想的测定结果。讨论的结果可为氦离子化气相色谱法测定相关样品中微量氧、氮含量时提供技术参考。     

Development of a simple and fast ultrasound-assisted extraction method for trace element determination in tobacco samples using ICP-MS

The current study describes a simple and fast method for the determination of Ba, Cd, Co, Cr, Cu, Mn, Ni and Pb in tobacco samples. Commercial cigarettes obtained from local market stores were analysed by inductively coupled plasma mass spectrometry (ICP-MS) after ultrasound-assisted extraction in acidic medium, and the results were compared to those obtained following microwave-assisted digestion of the samples. The sonication time was evaluated from 0 to 60 min, and a 30 min extraction time was selected. The concentration of HNO₃ was also optimised at 0.7 mol L^?1. In order to verify the accuracy of the proposed method, a certified reference material was submitted to the same extraction protocol adopted for the samples, and good agreement with the certified values was obtained at a 95% confidence level, except for Co. The extraction of Pb was also semi-quantitative. A total of four tobacco samples were analysed, with concentrations ranging from 0.4 for Cr to 214.6 µg g^?1 for Mn. The proposed method was demonstrated to be fast, sensitive, precise and accurate for the determination of Ba, Cd, Cr, Cu, Mn an Ni and for the semi-quantitative analysis of Co and Pb in tobacco samples.     

A new device for contamination-free injection for gas chromatographic trace estimation of oxygen and nitrogen

Summary The paper presents a new device modifying normal injection port of a gas chromatograph for eliminating air contamination thus enabling determination of traces of oxygen or nitrogen. Further modification is also proposed which enables the analysis to be carried out with a limited quantity of sample gas. Potential application of this device in the analysis of reactive gases like florine has been indicated.     

Development of a procedure for the sequential extraction of substances binding trace elements in plant biomass

This work investigates how the amounts of some important substances in a plant, and their behaviour inside the plant, depend on the levels of stress placed on the plant. To this end, model plant spinach (Spinacia oleracea L.) was cultivated on soil treated with sewage sludge. The sewage sludge contained various trace elements (As, Cd, Cu, Zn), and the uptake of these trace elements placed the plant under stress. Following this, a sequential extraction procedure was employed to determine the levels and distributions of trace elements within the most important groups of compounds present in the spinach plants. Since the usual five-step sequential extraction procedure provides only general information on the distributions of elements within individual groups of organic compounds, due to the wide range of organic compounds within the individual fractions, this scheme was extended and improved through the addition of two solvent extraction steps—a butanol step (between the ethyl acetate and methanol solvent steps) and an H₂O step (after the methanol+H₂O solvent step). The distributions and levels of the trace elements within the main groups of compounds in spinach biomass was investigated using this new seven step sequential extraction (water free solvents: petroleum ether (A) ethyl acetate (B) butanol (C) methanol (D) water solvents: methanol+H₂O (1+1; v/v) (E) H₂O (F) methanol+H₂O+HCl (49.3+49.3+1.4; v/v/v) (G)). The isolated fractions were characterized using IR spectroscopy and the trace element contents were determined in the individual fractions. Lipophilic compounds with low contents of Cd, Cu and Zn were separated in the first two fractions (A, B). Compounds with higher As contents (11.5–12.8% of total content) were also extracted in the second fraction, B. These two fractions formed the smallest portion of the isolated fractions. Low molecular compounds from secondary metabolism and polar lipids were separated in the third (C) and fourth (D) fractions, and high molecular compounds (mainly polypeptides and proteins) separated in the fifth and sixth fractions (E, F). The addition of the H₂O solvent step was particularly useful for separating compounds that have a significant impact on trace element bounds. The methanol fraction was dominant for all treatments, and a significant decrease in the spinach biomass separated in this fraction was observed when the soil was treated with sewage sludge. Most of the As (35.5–38.8% of total content), Cu (45.0–51.6%) and Zn (39.8–47.2%) was also determined in this fraction. The G fraction (obtained after acid hydrolysis) contained polar compounds. Most of the Cd was also found in this fraction, as was a significant amount of Zn. Non-extractable residues formed the last fraction (polysaccharides, proteins).     

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.     

Development of a gel monolithic column polydimethylsiloxane microfluidic device for rapid electrophoresis separation

A β-cyclodextrin (β-CD)-bonded gel monolithic column polydimethylsiloxane (PDMS) microfluidic device was developed in a simple and feasible way. Before preparation of gel monolithic column in PDMS microchannel, PDMS surface was activated by UV light to create silanol groups, which is an active molecule to covalently bond 3-(trimethoxysilyl)-propyl methacrylate (Bind-Silane) and seal microfluidic device. By the way, Bind-Silane is a bifunctional molecule to link polyacrylamide (PAA) gel and inner wall of PDMS microchannel covalently. Allyl-β-CD was used not only as a multifunctional crosslinker in PAA gel to control the size of the pores, but also as a chiral selector for the enantioseparation. The stability, transferring heat and optical characteristic of the microfluidic device were examined. The separation capability of the gel monolithic column was confirmed by the successful separation of fluorescein isothiocyanate (FITC)-labeled arginine (Arg), glutamine acid (Glu), tryptophan (Try), cysteine (Cysteine) and phenylalanine (Phe) in the PDMS microfluidic device less than 100 s at 36 mm effective separation length. A maximum of 2.06 × 10⁵ theoretical plates was obtained by the potential strength of 490 V/cm. A pair of FITC-labeled dansyl-d,l-threonine (Dns-Thr) was separated absolutely.     

Development of a downscale sedimentation field flow fractionation device for biological event monitoring

Classically described as a macroscale size-density based method, Sedimentation field flow fractionation (SdFFF) has been successfully used for cell sorting. The goal of this study was to develop a new SdFFF device for downscale applications, in particular for oncology research to rapidly monitor chemical biological event induction in a cell line. The development of a downscale SdFFF device required reduction of the separation channel volume. Taking advantage of a newly laboratory designed apparatus, channel volume was successfully decreased by reducing both length and breadth. To validate the apparatus and method, we used the well-known model of diosgenin dose-dependent induction of apoptosis or megakaryocytic differentiation in HEL cells. After a minute scale acquisition of a reference profile, the downscale device was able to perform fast, early, significant and reproducible monitoring of apoptosis and differentiation, two important biological mechanisms in the field of cancer research.