标定罩使用对气体报警器检定结果的影响

为指导检定人员在气体报警器检定时对气体标定罩的正确使用,对标准罩、大罩、小罩、不带罩4种情况进行试验,并对气体报警器检定结果的绝对误差、响应时间、重复性等参数进行对比分析。结果表明,在满足绝对误差±5%FS之内、响应时间不大于60 s、重复性不大于2%的技术指标要求时,使用标准罩能够得到更准确、稳定、符合现场模拟真实数值的检定结果。该研究有利于提高气体报警器检定结果的准确性。     

氰化氢气体检测报警器的校准

建立氰化氢气体检测报警器的校准方法.通过模拟实际的气体扩散状况,分别对扩散式电化学传感原理的氰化氢气体检测报警器的示值误差、重复性、响应时间等项目进行校准.总结了多台仪器的校准结果,提出了科学合理的氰化氢气体检测仪校准的技术指标:绝对误差为±2μmol/mol,或者相对示值误差不大于10％,满足其一即可;重复性不大于3...     

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 mg/L,重复性标准差不大于0.3 mg/L;当测量质量浓度不小于10.0 mg/L时,示值误差不大于±8%,重复性相对标准差不大于3%。据此对影响仪器主要性能的各个参数进行全面评价,确认各项性能指标控制在合理范围内。该校准方法切实可行,可满足石油产品库仑氯分析仪量值溯源的需求和仪器性能的评价。     

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。     

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。     

定碳定硫分析仪检定规程的探讨和修订建议

JJG 395–1997《定碳定硫分析仪检定规程》中的部分技术要求和检定项目已不能满足现代碳硫分析仪器检定/校准的要求。对规程的适用性、称量稳定性、示值误差、标准物质、重复性、分析时间等进行了探讨,并给出了修订建议。探讨了评定仪器检测空白的可能性,提出了依据碳硫测定基准国标方法的仪器检定/校准方法,以评定不同用途的测试仪器,并扩展了仪器检定/校准的范围。为计量部门修订规程提供参考,同时也为实验室合理评价,验收碳硫分析仪,及时掌握仪器的运行状况,保证分析数据的准确性、一致性和溯源性提供借鉴。     

水分活度仪校准方法

探讨水分活度仪的计量特性和校准方法。校准项目主要包括外观、温度示值误差、温度稳定性、示值误差、重复性、响应时间。在分析校准试验数据的基础上,提出了校准项目的性能指标:温度示值误差在±1℃之内,温度稳定性在±1.5℃之内,示值误差在±0.05之内,重复性不大于3%,响应时间在30min之内。用该方法可对影响仪器性能的参数进行综合评价,确认各项性能指标是否控制在合理范围内,保证水分活度仪性能正常。     

固体进样总有机碳分析仪校准方法

建立固体进样总有机碳分析仪的校准方法.根据仪器原理及使用情况,选取线性、示值误差、重复性作为仪器的主要计量特性,并探讨各个计量特性的校准方法.用该方法对某型号的仪器进行校准,得线性相关系数为0.998,示值误差为0.86％,重复性为0.39％,并对示值误差测量结果不确定度进行了评定,扩展不确定度为0.94％(k=2)....     

煤矿束管监测系统红外线气体分析仪的校准

根据JJF 1094–2002 《测量仪器特性评定》的要求,研究了煤矿束管监测系统红外线气体分析仪的校准方法。选用氮中氧气体标准物质作为仪器零点校准气体,流量控制在1 000～1 500 mL/min,在每一量程内配制一种浓度的混合气体标准物质,能够满足校准需求。确定的仪器计量技术指标:示值误差不大于5%FS,测量结果的重复性不大于2%,响应时间不大于120 s。该方法成功用于ULTRAMAT 23型红外线气体分析仪的校准,可用于实验室仪器的验收和评价,对该类仪器技术规范的制订有借鉴意义。     

激光甲烷气体测定器的校准

建立激光甲烷气体测定器的校准方法。根据仪器原理和使用情况,选取仪器的示值误差、重复性、响应时间、信号传输误差、报警声级强度、绝缘电阻等项目进行校准,探讨了各个项目的校准方法,给出了具体技术指标。当甲烷气体的摩尔分数为0～1%时,示值的绝对误差（摩尔分数）为±0.06%,当甲烷气体的摩尔分数为1%～100%时,示值的相对误差为±6%;重复性不大于1%;响应时间不大于25 s;信号传输误差不大于1%;报警声级强度不小于80 dB(A计权);绝缘电阻不小于50 MΩ。该校准方法对激光甲烷气体测定器的量值溯源进行了探索,验证试验表明该校准方法切实可行,技术指标要求合理。     

基于气相色谱法危废品仓库中非甲烷总烃在线监测系统研制

研制了一套基于气相色谱法的危废品仓库中非甲烷总烃的在线监测系统。该系统采用气相色谱原理对样品进行分离,经火焰离子化检测器电离形成微电流,通过信号放大器检测并换算成烃类含量。经联动调试检测显示,系统的示值误差小于±2.5%,零点漂移小于±5%F.S.(传感器满量程误差的百分数),量程漂移小于±5%F.S.,响应时间小于300 s,系统各项技术性能指标均满足并优于《上海市固定污染源非甲烷总烃在线监测系统验收及运行技术要求》,具备推广和应用价值。     

线型光束可燃气体探测器的校准

介绍线型光束可燃气体探测器的的校准方法。对线型光束可燃气体探测器的示值误差、报警功能、响应时间、光强衰减性能和抗日光干扰性能等主要计量特性及技术指标进行校准,给出了各主要计量特性的校准条件、试验设备和具体校准方法。对两台线型光束可燃气体探测器进行了校准,其示值误差用相对误差表示分别为–5%和4%,用引用误差表示分别为–4%FS和3%FS。经验证,上述结果均未超出设定指标,响应时间等其它主要计量特性也符合方法要求。该方法校准后的计量特性及技术指标较为合理,校准方法切实可行,可以用于线型光束可燃气体探测器的校准。     

Determination of individual sulfur-containing compounds in gas condensate and petrol by gas chromatography

A procedure is developed for the determination of more than 60 individual sulfur-containing compounds (SCC) in liquid hydrocarbon raw materials and in liquid fuels using gas chromatography on a 25-m WCOT column, inner diameter 0.32 mm, with a nonpolar dimethylpolysiloxane stationary phase (layer thickness 5 μm) and chemiluminescence detection. SCC were identified by individual standard substances and published data. Quantitative determination was carried out by the internal standard method. The results of determination of individual SCC in petrol and stable gas condensate are presented. The most high-boiling SCC found in significant amounts (more than 0.005 wt % of sulfur) were C₂-benzothiophenes (in petrol) and C₄-dibenzothiophenes (in gas condensate).     

Thermal decomposition of hydrotalcite-like compounds studied by a novel tapered element oscillating microbalance (TEOM): Comparison with TGA and DTA

For the first time, we report on the application of a tapered element oscillating microbalance (TEOM) as a novel technique to investigate the thermal decomposition of hydrotalcite-like compounds (HTlcs) in air. Experiments were performed in the temperature range of 323-973 K with Mg-Al, Ni-Al, and Co-Al-HTlcs. The TEOM technique measures mass changes based on inertial forces, presenting important advantages over conventional thermogravimetric analyzers, such as the very rapid time response and the well-defined flow pattern. In general terms, excellent agreement between TEOM, TGA, and DTA techniques during HTlc decomposition was obtained. Interestingly, transition temperatures in the TEOM were lower than in TGA and DTA, particularly for removal of interlayer water but also for dehydroxylation of the brucite-like layers and decarbonation. This was attributed to the flow-through operation in the tapered element of the TEOM as compared to the recognized gas stagnancy and bypass in sample crucibles of conventional thermogravimetric analyzers. Our results conclude that the TEOM technique is suitable for temperature-programmed studies. However, due to its operation principle, blank runs are required in contrast to the more automatic operation in commercial thermogravimetric units. Besides, a careful sample loading and packing in the micro-reactor is essential for reproducible results.     

Development and applications of industrial process analyzers

Contacts between users and suppliers is essential to ensure cost-effectiveness of process analyzers. Technical consideration of in-line, on-line and off-line measurements as well as analytical procedures are needed for selection of the most appropriate system. Quantitative performance specifications are often set too high, resulting in a sophisticated analyzer with excessive investment and maintenance costs. Process parameters such as time constant, sampling point and environmental conditions must be considered. Rules for decision-making are reviewed; autocorrelation, cross-correlation, controllability and information theory are useful in making efficient decisions on appropriate analyzers. Examples related to sulphur dioxide in stack gas scrubbers, chlorine in water supplies and sodium in boiler feed water are discussed.     

Fundamental study on decontamination of tritium from gaseous phases by copper oxide

Some fundamental studies on removal of tritium from gaseous streams by a small column of copper oxide were carried out. An about 10 cm length of column packed with 100 g of copper oxide was examined on the conversion ratios of hydrogen and tritium into water. The experiment with hydrogen of 0.1% in argon showed that the logarithmic plot of remaining ratio of hydrogen by passing through the column is proportional to the reciprocal of gas flow rate and to the length of oxide column. The oxide column was also used for treating tritium-bearing waste gas from an evacuating system of alpha D-T neutron generator. It was observed that at column temperatures lower than 450 degrees C the conversion ratio of tritium in the waste gas into water is considerably smaller than that of hydrogen of 0.1% in argon.     

Production of Hydrogen-Rich Synthesis Gas by Pulsed Atmospheric Plasma Submerged in Mixture of Water with Ethanol

Hydrogen-rich synthesis gas was produced by pulsed dc plasma submerged into ethanol–water mixtures using an original system with a coaxial geometry. The ignition of the discharge is immediately followed by production of hydrogen and after a short time necessary for filling the outlet tubing a flame can be ignited. No auxiliary gas was used for the reforming process. The synthesis gas containing up to 60% of hydrogen was formed, at the outflow rate of 250 sccm at the average power as low as 10 W. The hydrogen production efficiency corresponds to 12 kWh/kg H₂.     

大范围高灵敏度纳米尺度氨气传感器的制备

介绍了基于碳纳米管与聚苯胺纳米纤维的两种氨气传感器的制备与测试,综合运用两种传感器,兼顾了高灵敏度和大范围测量两项互相制约的要求.使用近场电纺技术制备单根聚苯胺纳米纤维传感器,对1×10-6氨气灵敏度达到2.7％,比较了聚苯胺纳米纤维结构和薄膜结构的响应特性.纳米纤维的立体结构可提升传感器性能.使用双向电泳技术制备碳纳米管传感器,对浓度大于20× 10-6 (V/V)的氨气有良好的线性响应.分析了主要功能材料的微结构,阐述了制备技术,比较了响应特性,分析了纤维中气体三维扩散模型,通过计算和测试值,表明响应时间与纤维直径存在反相关性.     

高浓度二氧化氯气体的在线检测研究

在40℃下,高浓度ClO2气体在盘管中迅速溶解于水中达到平衡,使用分光光度法检测平衡溶液的浓度,从而间接测定出ClO2气体的浓度。该方法可检测体积分数大于0.14%的ClO2,响应时间为15~30s,相对标准偏差为0.3%,与连续碘量法相比测定结果没有显著性差异(P<0.01),全过程中未使用化学试剂,操作简便,干扰小,适用于的高浓度ClO2气体在线检测。     

Comparison of negative ion electrospray mass spectra measured by seven tandem mass analyzers towards library formation

A library of negative ion electrospray ionization mass spectra and tandem mass spectra (MS/MS) of sulfonated dyes has been developed for fast identification purposes. The uniform protocol has been elaborated and applied to the measurements of more than 50 anionic dyes. Three collision energies are selected in our protocol which ensures that at least one of them provides a suitable ratio of product ions to the precursor ion. The robustness is investigated with altered values of tuning parameters (e.g. the pressure of the nebulizing gas, the temperature and the flow rate of drying gas, and the mobile phase composition). The results of the inter-laboratory comparison of product ion mass spectra recorded on seven different tandem mass spectrometers (three ion traps, two triple quadrupoles and two hybrid quadrupole time of flight instruments) are presented for four representative anionic dyes--azo dye Acid Red 118, anthraquinone dye Acid Violet 43, triphenylmethane dye Acid Blue 1 and Al(III) metal-complex azo dye. The fragmentation patterns are almost identical for all tandem mass analyzers, only the ratios of product ions differ somewhat which confirms the possibility of spectra transfer among different mass analyzers with the goal of library formation.