基于分子流传感元件的真空腔体漏率测量方法

本文介绍了一种基于分子流传感元件的真空腔体漏率测量方法,该方法通过分子流传感元件测量真空腔体整体漏率,采用的测量装置由气体流量测量系统、真空抽气系统、恒温系统等部分组成.在测量系统中,流经传感元件的气流处于分子流状态,通过测量传感元件两端的差压,计算质量流量,可以得到真空腔体的整体漏率.实验中对多个真空腔体漏率的测量结...     

Dynamic extension - A new principle for a vacuum primary standard for UHV-range (10-10 Pa) calibration of hot cathode ionisation gauges

The main obstacle in the construction of primary vacuum standards for very low pressures - ultra-high vacuum (UHV) - is outgassing from the walls of the apparatus. Thus, principles utilising a higher pumping rate in the calibration chamber, e.g., the pressure ratio technique, seem to be more useful for this range. However, a serious problem is inherent in this method, namely, that the gas in the calibration chamber is not in equilibrium and thus cannot be characterised by a single scalar pressure value, although such a value is then used to evaluate the measurement. This discrepancy can be overcome by using a hot cathode ionisation gauge as a transfer standard calibrated by the dynamic extension method.The dynamic extension method is explained and compared with the pressure ratio technique. The basic conditions for achieving acceptable uncertainty values are considered.     

Vacuum membrane capacity meters with electrostatic compensation

We describe new features of vacuum membrane capacity meters with electrostatic compensation, which improves their performance and expands their functional applicability for measuring volumes with complex configurations and flow rates of small gas streams. The concept is based on introduction of an additional reservoir with mobile gas-impermeable gate. When connected to the chambers of pressure gauge converter, the unit reduces the chamber volume in the course of pressure measurement so as to modify the conversion ratio in the vacuum meter measurement equation.Translated from Izmeritel'naya Tekhnika, No. 6, pp. 9–10, June, 1993.     

Investigation of a set procedure for the stability of pressure control in the newly developed flow-control system at KRISS

Korea Research Institute of Standards and Science (KRISS) has assembled a new flow-control system (FCS-705) for the study of advanced applications and calibration of different types of vacuum gauges by comparison method. This report details the measurement of the outgassing rate of the main vacuum chamber by the pressure rate of rise method. Constant pressure was generated inside the vacuum chamber by employing a dynamic flow control method. Nitrogen gas flow data was recorded to demonstrate that constant pressure was controlled in the vacuum chamber. The measurements were performed in a sequence of increasing pressures.     

Method of determining the relative sensitivity of thermal vacuum gages to different gases

A new method is described for determining the relative sensitivity of thermal vacuum gages and their sensors (tranducers) to different gases. The method is based on compensation for the change in the transducer signal caused by the use of a gas other than nitrogen or air and by variation of the volume of the measurement chamber. This approach makes it possible to avoid some of the errors intrinsic to measurements of low pressures and small increments in the transducer signal. A vacuum system configuration that allows the given method to be realized is described. Translated from Izmeritel'naya Tekhnika, No. 1, pp. 31–32, January, 1997.     

Mechanical properties of composite structures fabricated with the vacuum induced preform relaxation process

A new technique called vacuum induced preform relaxation (VIPR) can be used to improve the processing of composite parts manufactured using vacuum resin infusion methods. The VIPR process is a method for manipulating and guiding the resin filling pattern during a vacuum assisted resin transfer molding (VARTM) manufacturing process with a relatively small external vacuum chamber. This VIPR chamber can be sealed against the flexible molding surface of a VARTM mold and used to create vacuum above the preform. This causes the compressive forces compacting the fabric to decrease allowing the resin to flow faster in the effected region under the chamber. Thus the chamber can influence the resin flow pattern as well as avoid the formation of voids due to merging flow fronts. When the regulated vacuum in the chamber is applied it temporarily decreases the fiber volume fraction of the preform. It is important to investigate if this relaxation has a permanent adverse effect on the mechanical properties of the composite. The results of these tests strongly suggest that the use of the VIPR process does not compromise the mechanical properties of composite structures.     

低压流场速度测量的不确定度分析

激光多普勒测速技术被广泛应用于流速测量领域。在搭建好的真空气流检测实验平台基础上,运用二维激光多普勒测速仪对真空腔室进行流速测量;为了减小测速系统的测量误差,对真空腔室流速测量不确定度的来源及评定进行了分析与说明,得到了真空腔室流速测量的合成相对标准不确定度和相对扩展不确定度。研究表明:LDV重复性测速和进气量估读引起的不确定度较大,而LDV系统误差和其它因素引起的不确定度较小。研究结果对后期真空腔室流速测量有一定指导意义。     

Study on Vacuum Materials Outgassing Rate Using the Method of Switching Between Two Pumping Paths

A new measurement apparatus for vacuum materials outgassing rate was developed, which is mainly composed of three systems, including ultra-high vacuum system, high vacuum system, switching between two pumping paths (SPP) measurement system. The test principle of the modified SPP method is described in details, and the newly-developed technique has two main advantages over the conventional one. Firstly, the errors due to the use of two gauges with different physical properties are avoided by using only one gauge during data processing. Secondly, the outgassing rate of sample chamber, the test chamber and the outgassing or pumping effect of the gauge head can be eliminated enormously. Based on the SPP method, this paper gives the details of the experiments and the results on specific outgassing rate of the 7075 aluminum alloy sample in different conditions, namely, at different times and at different temperatures generated by infrared light irradiation heating.     

固定流导法校准真空漏孔方法研究

固定流导法采用的是分压力测量技术,对质谱分析室的漏放气率的指标要求不高.通过实验得到四极质谱计的非线性引起的测量误差可达38%,在具体校准过程中能够很好调节稳压室中的气体压力,使通过小孔的气体流量与待校真空漏孔漏率非常接近,从而避免了四极质谱计的非线性影响.稳压室中的气体压力比较大,所以稳压室不需要特别严格的材料处理工艺,具体校准过程中也不需要彻底的烘烤出气就能得到纯净的单一气体.固定流导法校准真空漏孔的不确定度的评定值为2.6%,可以通过精确校准电容薄膜规和控制温度来进一步降低漏孔校准的不确定度.     

GC/MS with post-column switching for large volume injection of headspace samples: sensitive determination of volatile organic compounds in human whole blood and urine

When volatile or semivolatile compounds are measured by headspace (HS) gas chromatography (GC)/mass spectrometry (MS), the maximum gas volume to be injected is usually 0.5-1.0 mL; over the volume, the MS detector automatically shuts down due to impairment of the vacuum rate of the MS ionization chamber. To overcome the problem, we modified the gas flow routes of a new type of GC/MS instrument to create a postcolumn switching system, which can eliminate the large volume of gas before introduction of target compounds into the MS ionization chamber. Our HS-GC/MS system enabled injection of as large as 5 mL of HS gas without any disturbance. As the first example analysis, we tried to establish the analysis of naphthalene and p-dichlorobenzene in human whole blood and urine by this method with large volume injection. The limits of detection for both compounds in whole blood and urine were as low as about 10 and 5 pg/mL, respectively. The validation data and actual measurements were also demonstrated. The new GC/MS system has great potential to analyze any type of volatile or semivolatile organic compounds in biological matrixes with very high sensitivity and full automation.     

Capabilities for Dielectric-Constant Gas Thermometry in a Special Large-Volume Liquid-Bath Thermostat

Dielectric-constant gas thermometry is being further developed at PTB to measure thermodynamic temperature and the Boltzmann constant at the triple point of water. For this purpose, a huge liquid-bath thermostat with a liquid volume of about 800 L has been built to provide a suitable thermal environment in the central working volume (diameter 0.5 m, height 0.65 m), in which the vacuum chamber containing the measuring system is placed. Measurements of the temperature field in the working volume have been performed with and without the chamber using a mesh of 12 platinum resistance thermometers at appropriate positions. The results verify that the temperature inhomogeneity in the bath is well below 1 mK as necessary. The uncertainty of the temperature measurement inside the measuring system must be of the order of 0.1 mK. Its thermal conditions have been, therefore, investigated in detail, too. Special emphasis was given to the thermalization after temperature changes.     

Volume Determination of Vacuum Vessels by Gas Expansion Method

This paper presents a practical procedure for the determination and precision calibration of the volume ratio and absolute value of the volume of vacuum chamber by using static expansion method. Such systems for calculations of volume ratio consist from two vessels connected via a valve called the expansion valve. For determination of absolute value of the volume we added another volume with simple shape (determined by dimensional measurements). In such systems, under the isothermal conditions, the gas pressure is reduced by the ratio of the small volume to the sum of the first volume (small volume) and second volume. The uncertainty of measurement of the volume ratio and absolute volume is calculated as well. Relative volume calibration is performed with uncertainties below 0.75 %.     

Thermogravimetry-evolved gas analysis-mass spectrometry system for materials research

Thermal analysis is a widely used analytical technique for materials research. However, thermal analysis with simultaneous evolved gas analysis describes the thermal event more precisely and completely. Among various gas analytical techniques, mass spectrometry has many advantages. Hence, an ultra high vacuum (UHV) compatible mass spectrometry based evolved gas analysis (EGA-MS) system has been developed. This system consists of a measurement chamber housing a mass spectrometer, spinning rotor gauge and vacuum gauges coupled to a high vacuum, high temperature reaction chamber. A commercial thermogravimetric analyser (TGA: TG + DTA) is interfaced to it. Additional mass flow based gas/vapour delivery system and calibration gas inlets have been added to make it a versatile TGA-EGA-MS facility. This system which gives complete information on weight change, heat change, nature and content of evolved gases is being used for (i) temperature programmed decomposition (TPD), (ii) synthesis of nanocrystalline materials, (iii) gas-solid interactions and (iv) analysis of gas mixtures. The TPD of various inorganic oxyanion solids are studied and reaction intermediates/products are analysed off-line. The dynamic operating conditions are found to yield nanocrystalline products in many cases. This paper essentially describes design features involved in coupling the existing EGA-MS system to TGA, associated fluid handling systems, the system calibration procedures and results on temperature programmed decomposition. In addition, synthesis of a few nanocrystalline oxides by vacuum thermal decomposition, gas analysis and potential use of this facility as controlled atmosphere exposure facility for studying gas-solid interactions are also described.     

真空混合漏孔示漏气体的延迟和保持特性研究

真空混合漏孔 ,如漏孔通道内含有空腔、毛细管道等 ,示漏气体除存在超长反应时间外 ,还存在超长的延迟时间和保持时间。只有经该延迟时间后 ,检漏仪才能探得信号。为满足真空元件在生产中的快速检漏的要求 ,又避免常规质谱检漏法漏检混合漏孔的可能性 ,在真空室内对检漏元件集体充氦 ,然后在保持期内逐个检测氦气浓度来判断有无混合漏孔 ;也可用质谱计比较残余气质谱图中空气成分来确定     

Replacement tissue-equivalent proportional counter for the International Space Station

The tissue-equivalent proportional counter (TEPC)-based dosemeters used on the International Space Station have exceeded their planned useful lives, and are scheduled to be replaced with the new units taking advantage of improved technology. The original TEPC detectors used cylindrical geometry with field tubes to achieve good energy resolution and minimum sensitivity to noise created by vibration. The inside diameter of these detectors is 5.1 cm. The new detectors developed for this application produce the resolution and vibration resistance of the cylindrical detector with the isotropic response and compact size of a spherical detector. The cathode structure consists of conductive tissue-equivalent plastic A-150 layers separated by thin polyethylene layers perpendicular to the anode. Each conductive layer is held at the electrical potential needed to produce uniform electric field strength along the anode wire, and thus the same gas gain for electrons produced in different portions of the spherical volume. The new design contains the whole preamplifier inside the vacuum chamber to reduce electronic noise. Also the vacuum chamber has a novel design with a 0.020-inch-thick aluminium wall to allow a total wall thickness of 0.5 g cm(-2), which is typical of the shielding provided by a space suit. This feature will allow measuring the dose on the astronauts' skin due to low-energy electrons and protons produced during solar events. The vacuum chamber has a new bayonet clamping system that reduces the total detector weight to less than half that of the old TEPC.     

Laser calibration of drift chambers

A nitrogen laser was used to simulate tracks of charged particle in a drift chamber. With this technique it is possible to test a drift chamber with high spatial resolution in its entire volume. By changing the amount of ionization the behaviour of the chamber has been tested near the threshold and the response of the whole read-out chain has been adjusted for the range of signal amplitudes of the Landau distribution. A very precise drift speed measurement has been performed in different conditions of drift voltage and gas concentrations.     

Industrial leak testing of dangerous goods packagings

The Dangerous Goods Regulations currently do not include limit leakage rates or sensitivity requirements for industrial leak testing procedures that are equivalent to the bubble test, which is the prescribed test method for design type testing of dangerous goods packagings. During series production of such packagings, various methods are used, which often do not meet the requirements of the bubble test with regard to important criteria. Sensitivity, flow direction, pressure level and automatability are particularly important factors when selecting a suitable industrial leak testing method. The following methods are in principle both suitable and equally effective as the bubble test: pressure rise test (vacuum chamber), ultrasonic bubble leak detection and gas detection methods (pressure technique by accumulation and vacuum chamber technique). To ensure a uniform test level during design type testing and production line leak testing and therefore a comparable safety level as required by the Dangerous Goods Regulations, it is necessary to include a more precise specification in these regulations. This requires, on the one hand, information about the sensitivity of the bubble test and, on the other hand, the inclusion of a list of suitable, equally effective industrial test methods with their specific boundary conditions.     

Gas absorption and outgassing of metals

The solution of the diffusion equation is taken as a foundation of the theory of gas-metal interaction in high vacuum. The boundary conditions are formulated from the analysis of the gas balance equations on a metal surface and in a gas volume. The boundary conditions are generally non-linear but in some important cases linearization is permissible. In this way it is possible to obtain analytical expressions for the instantaneous gas flow on electron- and photon-induced desorption, low temperature thermal desorption and gettering at a constant pressure. By means of these formulae one can generalize the experimental data of various authors and calculate the kinetics of such processes as the outgassing of an electron collector, the gas desorption by synchrotron radiation in a vacuum chamber of electron or positron colliding-beam storage-rings, the degassing of an ultra-high vacuum system, the gas sorption by barium and titanium, etc.     

New Method of Testing Vacuum Gauges

A new original method for testing vacuum gauges is presented. It consists of two stages: in the first stage gas is continuously fed into a measurement chamber and in the second stage it is pumped out (in the same pressure range). By simultaneously solving the equations describing both stages, errors caused by secondary gasdynamic processes are eliminated and there is an increase in the overall accuracy of the testing.     

智能气调包装系统

针对我国气调保鲜包装技术及应用的落后状况,采用Mix9001气体混合器、CMV-2气体比例分析仪、DQB-700N气调包装机及PLC控制器,构建了基于气体在线检测与比例控制的智能气调包装系统。利用气体比例分析仪监控气体组分,PLC控制气体混合器和气调包装机,实现包装容器保鲜气体的比例混合和充气包装。实验表明,该系统可自动实现包装袋保鲜气体的比例混合和充气包装,减少了保鲜气体的耗气量,提高了工作效率,同时省却了传统气调包装的真空气室。