CN1701224A - Low power gas leak detector - Google Patents
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Abstract
Description
背景 background
本申请要求享有于2002年9月27日提交的题为“相控传感器”的美国临时专利申请No.60/414211的优先权,该文献通过引用结合于本文中。This application claims priority to US Provisional Patent Application No. 60/414,211, filed September 27, 2002, entitled "Phase Control Sensor," which is incorporated herein by reference.
本发明涉及气体的检测、鉴定和分析。相关领域的可燃气体泄漏检测器可能是低成本的(并且部分地具有合理的灵敏度),然而却不能鉴别燃气泄漏(天然气、沼气、丙烷或汽油蒸气)的性质,而另一些装置如便携式GC(气相色谱仪)具有适中的灵敏度并且能够鉴别燃气,但它们非常昂贵,速度慢(响应时间超过约10秒),并且需要消耗很多功率。The present invention relates to the detection, identification and analysis of gases. Related art combustible gas leak detectors may be low cost (and in part have reasonable sensitivity), yet cannot identify the nature of gas leaks (natural gas, biogas, propane or gasoline vapor), while other devices such as portable GC ( Gas Chromatographs) have moderate sensitivity and are capable of discriminating gases, but they are very expensive, slow (response time greater than about 10 seconds), and consume a lot of power.
在下述文献中公开了涉及到气体检测器的结构和处理的各个方面:2002年5月28日授权的题为“具有增强灵敏度的相控加热器的气体传感器”的美国专利No.6393894,其通过引用结合于本文中;以及1990年7月24日授权的题为“热导率和比热测量”的美国专利No.4944035,其通过引用结合于本文中。Various aspects related to the construction and processing of gas detectors are disclosed in U.S. Patent No. 6,393,894, issued May 28, 2002, entitled "Gas Sensor with Phased Heater with Enhanced Sensitivity," which Incorporated herein by reference; and US Patent No. 4,944,035, issued Jul. 24, 1990, entitled "Thermal Conductivity and Specific Heat Measurement," which is incorporated herein by reference.
概要 summary
气体泄漏检测器和分析器可通过可负担的、原位式、超灵敏、低功率、低维护性和紧凑的微量检测器和分析器来实现,这种微量检测器和分析器可以无线式地或通过另一媒介(例如导线或光纤)将其检测和/或分析结果发送给中央的或其它的人工控制站。微量流体分析器可结合有相控加热器阵列、浓缩器、分离器来作为增强的检测器,从而提高了低成本的多气体分析器和系统的提供气体泄漏检测的实用性。Gas leak detectors and analyzers are enabled by affordable, in-situ, ultra-sensitive, low-power, low-maintenance and compact trace detectors and analyzers that wirelessly Or send the detection and/or analysis results to the central or other manual control stations through another medium (such as wires or optical fibers). Microfluidic analyzers can incorporate phased heater arrays, concentrators, and separators as enhanced detectors, thereby increasing the availability of low-cost multi-gas analyzers and systems for providing gas leak detection.
该气体泄漏检测器是低功率的、快速的、紧凑的、低成本的、智能的、无线式或非无线式的、低维护的、稳健的和高灵敏度的。它是基于相控加热器的泄漏检测器,其可在约一秒内作出反应,使用不足一瓦的功率,能够通过其成分来鉴别燃气的性质,并且是掌上型的,因此非常易于携带。The gas leak detector is low power, fast, compact, low cost, intelligent, wireless or non-wireless, low maintenance, robust and highly sensitive. It is a phased heater based leak detector that responds in about a second, uses less than a watt of power, is able to identify the nature of the gas by its composition, and is palm-sized so it is very portable.
相控加热器阵列的加热元件可在其两个表面即顶面和底面上涂覆吸附材料,以实现低功耗和更有效地加热输入检测气体。加热元件可具有针对该较小功耗的较窄宽度。还设有包括较少数量锚固点的加热器膜片,用于使来自加热元件的热传导较少。The heating element of the phased heater array can be coated with adsorption material on its two surfaces, the top surface and the bottom surface, to achieve low power consumption and more efficient heating of the input detection gas. The heating element can have a narrower width for this less power consumption. There is also a heater membrane comprising a reduced number of anchor points for less heat conduction from the heating element.
加热器阵列的内部通道的表面可涂覆非吸附性绝热层,但那些特地设计成涂覆有吸附材料的表面除外。可以减小吸附性涂层或薄膜的厚度,从而缩短吸附和解吸所需的时间。可以采用比较节约的泵来抽取待检查的流体样品,以便检测从某处泄漏出来的可能气体。可以使用在不用时处于睡眠状态的低功率电子装置。因此,该泄漏检测器只消耗非常少的功率。The surfaces of the internal channels of the heater array may be coated with a non-absorptive insulating layer, except those surfaces specifically designed to be coated with an adsorbent material. The thickness of the adsorptive coating or film can be reduced, thereby shortening the time required for adsorption and desorption. A relatively economical pump can be used to draw a sample of the fluid to be checked in order to detect possible gas leaks from somewhere. Low power electronics that sleep when not in use may be used. Therefore, the leak detector consumes very little power.
气体泄漏检测器可通过传统的半导体工艺或微电机系统(MEMS)技术而集成在芯片上。这类加工导致了检测器的低功耗、紧凑性和原位布置的特征。空气或气体样品通过检测器的流率可以是非常小的。另外,样品的载气不是必须要的,因此载气的这种缺乏可以降低被测试样品的稀释,此外还消除了与高压气罐操纵有关的维护和所需容积。这种方法允许传感器提供快速的分析和迅速的结果,可能比一些相关领域的装置至少快一个数量级。它避免了人工密集型实验室分析技术的延迟和高成本。传感器是智能的,其可具有用于所检测气体的分析和确定的集成式微控制器,并且保持精确且成功的操作,以及与无人看管的远程位置之间传递信息。传感器可经由公用线路或光学或无线媒介来传递检测器的信息、分析和结果,并且能够通过“即插即用”式适配和简化性来在远程距离上与主机系统进行完全双工通信。该系统可通过网络来工作。它可与其它气体样品调节器件(颗粒过滤器、阀、流量和压力传感器)、局部维护控制点互连,并能提供经由因特网的气体泄漏监控。该检测器是稳健的。它可在高电磁干扰(EMI)环境中、例如在具有非常强的电场和磁场的电力分配子站的附近保持精度。检测器具有高灵敏度。它提供了亚ppm(百万分之一)级的检测,这比相关领域技术、例如可提供1到10ppm范围内灵敏度的传统气相色谱仪高100到10000倍。其中,检测器是气相色谱仪的低功率、更快速、更紧凑以及更灵敏和可负担得起的变型。它还比现有类型相控加热器检测器的已有型号更低功耗和更快速,这种相控加热器检测器需要必须多次充电和放电的重型电池,而本发明的检测器避免了这种电池。本发明的检测器具有结构完整性,在非常大的差压范围内检测和分析高压流体样品的应用中具有非常低的泄漏危险,或者没有泄漏危险。Gas leak detectors can be integrated on-chip through conventional semiconductor processes or micro-electromechanical systems (MEMS) technology. Such processing results in low power consumption, compactness, and in situ arrangement characteristics of the detector. The flow rate of the air or gas sample through the detector can be very small. In addition, sample carrier gas is not necessary, so this absence of carrier gas reduces dilution of the sample being tested, and also eliminates the maintenance and required volumes associated with the handling of high pressure gas tanks. This approach allows the sensor to provide rapid analysis and prompt results, potentially at least an order of magnitude faster than some related art devices. It avoids the delays and high costs of labor-intensive laboratory analysis techniques. The sensor is intelligent, it can have an integrated microcontroller for the analysis and determination of the detected gas, and maintain accurate and successful operation, as well as transfer information to and from unattended remote locations. Sensors can communicate detector information, analysis and results via public lines or optical or wireless media and are capable of full duplex communication with host systems over long distances with "plug and play" adaptation and simplicity. The system can work through the network. It can be interconnected with other gas sample conditioning devices (particulate filters, valves, flow and pressure sensors), local maintenance control points, and can provide gas leak monitoring via the Internet. This detector is robust. It maintains accuracy in high electromagnetic interference (EMI) environments, such as in the vicinity of power distribution substations with very strong electric and magnetic fields. The detector has high sensitivity. It provides sub-ppm (parts per million) level detection, which is 100 to 10,000 times better than related art technologies such as conventional gas chromatographs which can provide sensitivities in the 1 to 10 ppm range. Among them, the detector is a lower power, faster, more compact and more sensitive and affordable variant of the gas chromatograph. It also consumes less power and is faster than existing models of existing types of phased heater detectors that require heavy batteries that must be charged and discharged multiple times, while the detector of the present invention avoids this battery. The detector of the present invention has structural integrity and has very low or no risk of leakage in applications of detecting and analyzing high pressure fluid samples over a very large differential pressure range.
在泄漏检测器中,小型泵如Honeywell MesoPumpTM优选将样品抽入到系统中,但仅有一部分样品在由阀(可以是HoneywellMesoValveTM或Hoerbiger PiezoValveTM)控制的流率下流经相控加热器传感器。这种方法可在较长的采样路径上实现快速的样品采集,并且为泄漏检测器提供了经调节的约1到3立方厘米/分钟的流量。泄漏检测器的泵可设置成经由过滤器来抽取样品气体,使得可提供快速样品采集和经相控加热器传感器的调节流。In a leak detector, a small pump such as a Honeywell MesoPump TM preferably draws the sample into the system, but only a portion of the sample flows through the phased heater sensor at a flow rate controlled by a valve (could be a Honeywell MesoValve TM or a Hoerbiger PiezoValve TM ) . This method allows for rapid sample acquisition over a long sampling path and provides a regulated flow of approximately 1 to 3 cc/min to the leak detector. The pump of the leak detector can be arranged to draw sample gas through the filter so that fast sample collection and regulated flow through the phased heater sensor can be provided.
当样品泵抽取样品气体经过泄漏检测器时,气体会膨胀,并因此增大其体积和线速度。控制电路可被设计成补偿这一速度变化,以便将加热器“波”保持为与传感器中的变化的气体速度同步。为了补偿样品气体在被迫流过加热器通道时其体积的变化,加热器的电子装置需要调节流量控制和/或加热器“波”的速度,从而使内部气流速度保持与加热器“波”同步。When the sample pump draws sample gas past the leak detector, the gas expands, thus increasing its volume and linear velocity. The control circuitry can be designed to compensate for this speed change in order to keep the heater "wave" in sync with the changing gas speed in the sensor. To compensate for the change in volume of the sample gas as it is forced through the heater channels, the heater electronics need to adjust the flow control and/or the speed of the heater "wave" so that the internal gas flow velocity remains in line with the heater "wave" Synchronize.
在泄漏检查操作期间,该检测器的能力(类似于任何其它较慢的GC)可检测空气的多种痕量成分,例如约330到700ppm的CO2、约1到2ppm的CH4和约0.5到2.5%的H2O。这使得可在线式地校准输出洗脱时间,并且检查例如可能代表天然气的乙烷、丙烷或其它气体管道泄漏物的其它峰的存在。因此,样品气体成分的峰高之比可能揭示了关于包括汽车废气或汽油蒸汽的痕量气体来源的线索。During leak checking operations, the detector's capability (similar to any other slower GC) detects a wide variety of trace components of air, such as about 330 to 700 ppm CO 2 , about 1 to 2 ppm CH 4 , and about 0.5 to 2 ppm 2.5% H2O . This allows the output elution time to be calibrated on-line and to check for the presence of other peaks such as ethane, propane or other gas pipeline leaks that may represent natural gas. Therefore, the ratio of the peak heights of the sample gas components may reveal clues about the origin of trace gases including automobile exhaust or gasoline vapors.
传感器可具有一定的灵敏度、速度、便携性和低功率,使得传感器尤其适用于对沿着传输或分配管道系统的天然气或丙烷气体以及化工厂中的其它气体进行安全方面强制性的定期泄漏检查。Sensors can have sensitivity, speed, portability, and low power that make them especially useful for safety-mandated periodic leak checks of natural or propane gas along transmission or distribution piping systems and other gases in chemical plants.
在其泄漏检测应用中,传感器使用一些或全部样品气体成分(及其峰比率)作为校准标记(洗脱时间鉴别出气体成分的性质)和/或泄漏源标识。如果只存在某种峰如甲烷(其在山地空气中以约1到2ppm的浓度存在),那么信息不足以表示该成分来源于沼气、天然气或管道气或其它流体。In its leak detection application, the sensor uses some or all of the sample gas constituents (and their peak ratios) as calibration markers (elution times identify the nature of the gas constituents) and/or leak source identification. If there is only a certain peak such as methane (which is present in mountain air at a concentration of about 1 to 2 ppm), then there is not enough information to indicate that the composition is derived from biogas, natural gas or pipeline gas or other fluids.
该泄漏传感器可用作便携式装置或安装在固定的位置处。与相关领域的相当传感器相比,它比便携式火焰离子化检测器更加紧凑,不需要体积庞大的氢罐,它比热丝或金属氧化物可燃气体传感器更快速和更灵敏,并且比传统的和/或便携式的气相色谱仪更加快速、更加紧凑和更加节省能量。The leak sensor can be used as a portable device or installed at a fixed location. Compared with comparable sensors in related fields, it is more compact than portable flame ionization detectors, does not require bulky hydrogen tanks, is faster and more sensitive than hot wire or metal oxide combustible gas sensors, and is more efficient than traditional and And/or portable gas chromatographs are faster, more compact and more energy efficient.
附图简介 Brief introduction to the drawings
图1是一种可能的泄漏检测器监控系统的框图;Figure 1 is a block diagram of a possible leak detector monitoring system;
图2显示了微量气体检测器装置的细节;Figure 2 shows the details of the trace gas detector setup;
图3是显示了示例性传感器装置的操作原理的布局;Figure 3 is a layout showing the principle of operation of an exemplary sensor device;
图4是图3中的示例性传感器装置的侧剖视图;FIG. 4 is a side cross-sectional view of the exemplary sensor device of FIG. 3;
图5是图3中的示例性传感器装置的端面剖视图;5 is an end cross-sectional view of the exemplary sensor device of FIG. 3;
图6是显示了示例性加热器温度的图形,还显示了在传感器装置的各加热元件处产生的相应浓度脉冲;Figure 6 is a graph showing exemplary heater temperatures and also showing corresponding concentration pulses generated at each heating element of the sensor device;
图7是显示了若干加热元件以示出分析物浓度的逐步增强的图形;Figure 7 is a graph showing several heating elements to illustrate the gradual increase in analyte concentration;
图8是显示了达到约100%浓度水平的浓度脉冲的图形;Figure 8 is a graph showing concentration pulses to a concentration level of about 100%;
图9是另一示例性传感器组件的布局;Figure 9 is a layout of another exemplary sensor assembly;
图10是如何应用该传感器来对流体流(例如烟道气)进行采样以便对其进行气体组成分析的示意图;Figure 10 is a schematic diagram of how the sensor can be used to sample a fluid stream (e.g. flue gas) for gas composition analysis;
图11是显示了图10所示传感器组件的操作的时序图;Figure 11 is a timing diagram showing the operation of the sensor assembly shown in Figure 10;
图12是包括传感器、浓缩器、分离器和传感器的集成电路的基本布局;和Figure 12 is a basic layout of an integrated circuit including sensors, concentrators, separators and sensors; and
图13是显示了关于气体泄漏检测器的各部分的不同功耗水平的表格。Fig. 13 is a table showing different power consumption levels for various parts of the gas leak detector.
描述 describe
图1显示了低功率泄漏检测器系统11的示例性视图。来自环境空间或容积体41中的输入流体25可进入到导管或管19中,而管19与低功率泄漏检测器15的输入端34相连。流体25可由检测器15来处理。处理过的流体37可离开检测器15的输出端36,并经由导管或管39排放到所指定的任一位置处的容积体中。用语“流体”作为通用用语使用,其包括气体物质和液体物质。结果或发现可被发送到微控制器/处理器29中以供分析。微控制器或处理器29可发送各种信号给检测器36,以用于控制、调节、校准或其它用途。分析计算、结果或其它信息可被发送给调制解调器35,用于转化成信号而经由线路、光纤或其它类似媒介而发送给站31。另外,这种到调制解调器35的输出可替代地或同时地发送给发射器33,以便与关于例如经由GPS所得到的检测器实际位置的信息一起无线传输给站31,尤其是在它被用作便携式装置的情况下。另外,站31可发送各种信号给调制解调器35和接收器33,这些信号可被传递给微控制器或处理器29,以用于控制、调节、校准或其它用途。FIG. 1 shows an exemplary view of a low power leak detector system 11 . An
图2显示了微量气体装置15。含有来自可能泄漏源处的气体的样品流25从管或吸入管19进入到输入端口34中。在此处设有颗粒过滤器43,用于从进入装置15的流体25的流中去除脏物和其它颗粒。这种去除是用于保护装置,过滤不应降低装置的用来精确分析流体25的组成的能力。不洁流体(带有悬浮的固体或液体的非挥发颗粒)可能会损害正确的传感器功能。流体25的一部分45可流经差动热导率检测器或传感器127,而流体25的另一部分47流经管49而到达单向阀51。通过将“T”管设置成与入口45紧密相邻,就可以最小的时延来实现采样,这是因为相对较大流量的流47有助于缩短过滤器的冲洗时间。泵53可使流体47从颗粒过滤器43的输出端中流经管49和阀51。调节阀51通过调节管129中的泵55的抽吸压力来控制经由管45通过传感器的流量。上述流动结构因此可同时实现两种益处。这些益处包括最少的采样时延和流量控制。泵55使流体45从过滤器43的输出端中流过检测器127、浓缩器124、流量传感器125、分离器126、热导率检测器或传感器128以及管129。泵55泵送流体经过管57而到达管59处,在这里流体45与流体47汇合成组合流体61。泵55可用在系统中,这取决于泵53的抽吸能力(10-300立方厘米/分钟)和泵55的足够低的流量(0.1-3立方厘米/分钟)。流体61通过泵53泵送给输出端口36。流体61作为流37经由出口管39而流出。来自检测器127和128的数据可被发送给控制器130,而它又将数据转发给微控制器和/或处理器29以供处理。最终的信息可被发送给站31。FIG. 2 shows a
图3是传感器装置10或15中的代表图2中的浓缩器124或分离器126的那一部分的示意图。传感器装置可包括衬底12和控制器130。控制器14可结合在衬底12中,也可不必如此。衬底12可具有多个位于其上的薄膜加热元件20,22,24和26。虽然仅显示了四个加热元件,然而可提供任意数量的加热元件,例如2个到1000个之间,但通常处于20-100个的范围内。加热元件20,22,24和26可由任何适当的电导体、稳态金属或合金薄膜制成,例如镍铁合金,其有时称为坡莫合金,具有80%的镍和20%的铁的组分;以及铂、硅化铂和多晶硅。加热元件20,22,24和26设置在薄的、低热质量、低面内热传导的支撑件30上,如图4和5所示。支撑件或膜片可由Si3N4或其它适当或类似的材料制成。加热元件可由Pt或其它适当或类似的材料制成。FIG. 3 is a schematic diagram of that portion of
图4和5显示了具有通道31和32的双通道式相控加热器机构41。衬底12和部分或晶片65具有用于接受流式样品流体45的限定通道31和32。通道可通过选择性地蚀刻支撑件30下方的硅通道晶片或衬底12和支撑件上方的通道晶片或部分65来加工。通道可包括用于流式样品流体45的进入端口34和排出端口36。4 and 5 show a two-channel phased
传感器装置还可包括多个位于通道31和32内从而暴露在流式样品流体45中的交互式元件。各交互式元件可设置成与相应的加热元件相邻,即形成可能的最接近接触。例如在图4中,交互式元件40,42,44和46可设置在通道32内的支撑件30的下表面上,并且分别与加热元件20,22,24和26相邻。另外,交互式元件140,142,144和146可设置在通道31内的支撑件30的上表面上,并且分别与加热元件20,22,24和26相邻。还可设置带有额外的交互式薄膜元件的其它通道,其未在该示例性例子中显示。交互式元件可由常用于液相或气相色谱仪的多种薄膜来形成,例如硅胶、聚甲基硅氧烷、聚二甲基硅氧烷、聚乙二醇、多孔硅石、NanoglassTM、活性炭和其它类似的聚合物质。此外,上述交互式物质可通过适当的掺杂剂来改性,以实现不同程度的极性和/或疏水性,从而实现目标分析物的最佳吸附和/或分离。The sensor device may also include a plurality of interactive elements positioned within the
图5显示了相控加热器机构41的端面剖视图。支撑件30可连接在顶部结构65上。锚固件67可将支撑件30相对于通道31固定位。较少的锚固件67连接点降低了从支撑件30到结构41的其它部分的热传导损耗。与普通的锚固方法相比,该示例具有较少的锚固点,这导致节约了约1.5倍的剩余加热元件输入功率。FIG. 5 shows a cross-sectional end view of the phased
交互式薄膜元件可通过使载有所需吸附剂的材料流经过通道32来形成。这便在整个通道中提供了交互层。如果希望有单独的交互式元件,那么可通过经由加热元件20,22,24和26来为涂层提供温度变化而进行选择性“显影”。在涂层被显影后,可提供溶剂流经过通道32,以便去除任何位置处的涂层,但已经显影或与适当的溶剂如丙酮聚合化的涂层除外,使得只有与加热元件相邻的溶剂材料。可在通道31和32的内壁上涂覆非吸附性绝热材料的涂层65,但设计有存在吸附剂涂覆表面如交互式元件的位置除外。该涂层可将所需的加热元件功率降低约1.5倍。这些材料的热导率应当远远低于通道壁所用材料的热导率。通道壁所用材料可以是硅。涂层65的备选材料可包括二氧化硅或其它金属氧化物。涂层65可降低支撑件30中的加热元件所用的功率。在保证流动/固定相体积的合理比率的同时,加热元件膜片以及吸附膜的大小(宽度、长度和厚度)的降低或减小可以导致约四倍的功率减小。降低或减小的吸附膜厚度可缩短吸附-解吸所需的时间,并且使每次流体分析所需的能量节约大约1.5倍。使用这种特别节约但又具备足够功能的泵53和/或55和120以及用于控制器130和/或微控制器/处理器29的低功率电子装置(其在不使用时处于睡眠模式)导致在这种功率方面大约两倍的降低,上述泵53和/或55和120在浓缩器的起动和/或分析器系统11的测量循环之前运行大约1秒或更少。An interactive thin film element can be formed by flowing a material laden with the desired sorbent through
图13中的表格显示了运行泄漏检测器系统11所需的整体功率,该系统类似于约100毫瓦或更少的系统,并具有上述设计特征的每三秒进行一次分析循环的系统。如表所示,系统11的能量节约措施可将每次分析(每三秒启动一次)所需的能量从约1.7焦和约1280毫瓦的峰值功率降低到约0.4焦和220毫瓦的峰值功率。The table in FIG. 13 shows the overall power required to run a leak detector system 11 similar to a system of about 100 milliwatts or less with an analysis cycle every three seconds with the design features described above. As shown in the table, the energy saving measures of the system 11 can reduce the energy required per analysis (once every three seconds) from about 1.7 joules and a peak power of about 1280 milliwatts to about 0.4 joules and a peak power of 220 milliwatts .
控制器14或130可与各加热元件20,22,24,26以及检测器50电连接,如图3所示。控制器14或130可通过时相顺序(见图6中的下部)来激励加热元件20,22,24和26,使得大约在由一个或多个上游交互式元件产生的上游浓度脉冲到达该交互式元件处的时候,各个相应的交互式元件40,42,44和46被加热,并将选定成分解吸到流式样品流体45中。可采用任意数量的交互式元件来在浓度脉冲中实现构成气体的所需浓度。所得浓度脉冲可被提供给检测器50,128,164,以供检测和分析。检测器50,127,128或164可以是热导率检测器、放电电离检测器,或者任何其它类型的检测器,例如通常用于气相或液相色谱仪中的检测器。
图6是显示了示例性的加热器温度以及在各加热元件处产生的相应浓度脉冲的图形。如上所述,控制器14或130以时相顺序来激励加热元件20,22,24和26。加热元件20,22,24和26的示例性时相加热器温度分别以温度曲线或线条60,62,64和66示出。Figure 6 is a graph showing exemplary heater temperatures and corresponding concentration pulses generated at each heating element. As described above, the
在所示示例中,控制器14,130(图3)可首先激励第一加热元件20以提高其温度,如图6中的线60所示。由于第一加热元件20与第一交互式元件40热连接,因此第一交互式元件将选定成分解吸到流式样品流体45中,在检测器128或50或164处产生第一浓度脉冲70,如果没有其它的加热元件产生脉冲的话。流式样品流体携带第一浓度脉冲70朝向第二加热元件22向下游运动,如箭头72所示。In the example shown, controller 14 , 130 ( FIG. 3 ) may first energize
控制器14(或130)然后激励第二加热元件22以提高其温度,如线62所示,其始于作用在元件20上的能量脉冲已经停止时或在此之前。由于第二加热元件22与第二交互式元件42热连接,因此第二交互式元件也将选定成分解吸到流式样品流体45中,产生第二浓度脉冲。控制器14,130可激励第二加热元件22,使得第二浓度脉冲基本上重叠在第一浓度脉冲70上,从而产生更高的浓度脉冲74,如图6所示。流式样品流体携带较大的浓度脉冲74朝向第三加热元件24向下游运动,如箭头76所示。Controller 14 (or 130) then energizes second heating element 22 to increase its temperature, as indicated by line 62, beginning at or before the energy pulse on
控制器14,130然后激励第三加热元件24以提高其温度,如图6中的线64所示。由于第三加热元件24与第三交互式元件44热连接,因此第三交互式元件44可将选定成分解吸到流式样品流体中,产生第三浓度脉冲。控制器14,130可激励第三加热元件24,使得第三浓度脉冲基本上重叠在由第一加热元件20和第二加热元件22所提供的较大浓度脉冲74上,从而产生还更高的浓度脉冲78。流式样品流体45携带该更大的浓度脉冲78朝向第N个加热元件26向下游运动,如箭头80所示。The
控制器14,130然后激励第N个加热元件26以提高其温度,如线66所示。由于第N个加热元件26与第N个交互式元件46热连接,因此第N个交互式元件46可将选定成分解吸到流式样品流体45中,产生第N个浓度脉冲。控制器14,130可激励第N个加热元件26,使得第N个浓度脉冲基本上重叠在由前面N-1个交互式元件所提供的较大浓度脉冲78上。流式样品流体携带第N个浓度脉冲82到分离器126或检测器50或128或164中,如下所述。The
如上所述,加热元件20,22,24和26可具有共同的长度。这样,通过为各加热元件提供相同的电压、电流或功率脉冲,控制器14,130就可实现加热元件的相同温度。电压、电流或或功率脉冲可具有任何所需的形状,包括三角形、方形、钟形或任何其它的形状。可采用大致方形的电压、电流或功率脉冲来实现如图6所示的温度曲线60,62,64和66。As noted above,
图7是显示了多个加热元件的图形,其显示出:第一,浓度如何在后续元件的解吸适当地同步于流式样品流体速度时逐步增大;第二,单个元件的长度如何在浓度水平和梯度增大时与质量扩散通量的预期增大率相匹配。在这里应当指出,在图7所示的元件之前,分析物浓度已经被放大了一个因子F,这是通过使初始元件的脉冲长度比元件100的脉冲长度(H1)长F倍来实现的,或者是通过使元件1,2,...,F同时地产生脉冲并且在仍冷却的元件100(H1)产生脉冲之前用它来收集所有解吸分析物来实现的。可以认识到,由于扩散的存在,在经过下方通道32时,各浓度脉冲的振幅减少但长度增加。为了容纳这一增大的长度,可以设想沿着流式样品流体来增大各个连续加热元件的长度。例如,第二加热元件102可具有比第一加热元件100的长度W1更大的长度W2。类似的,第三加热元件104可具有比第二加热元件102的长度W2更大的长度W3。因此可以设想,各加热元件100,102和104的长度相对于相邻的上游加热元件来说更长,增量对应于上游加热元件的浓度脉冲因扩散而预期增加的长度。Figure 7 is a graph showing multiple heating elements showing: first, how the concentration increases stepwise when the desorption of subsequent elements is properly synchronized with the flow sample fluid velocity; The levels and gradients increase to match the expected rate of increase in the mass diffusion flux. It should be noted here that prior to the element shown in Figure 7, the analyte concentration has been amplified by a factor F by making the pulse length of the initial element F times longer than the pulse length (H1) of element 100, Or by pulsing elements 1, 2, . It will be appreciated that, due to the presence of diffusion, each concentration pulse decreases in amplitude but increases in length as it passes through the
为了简化加热元件的控制,各连续加热元件的长度可保持恒定,从而在加热元件之间产生相同的整体加热器电阻,从而允许使用相同的电压、电流或功率脉冲来产生类似的温度曲线。或者,加热元件可具有不同的长度,控制器可为加热元件提供不同的电压、电流或功率脉冲振幅,从而产生类似的温度曲线。To simplify control of the heating elements, the length of each successive heating element can be kept constant, resulting in the same overall heater resistance between heating elements, allowing the use of the same voltage, current or power pulses to produce similar temperature profiles. Alternatively, the heating elements can be of different lengths and the controller can provide different voltage, current or power pulse amplitudes to the heating elements to produce similar temperature profiles.
图8是显示了达到100%浓度水平的浓度脉冲110的图形。可以认识到,即使浓度脉冲110达到了预定浓度阈值如100%,但仍可确定相应成分的浓度。为了这样做,检测器50,128,164可检测浓度脉冲110,控制器14,130将一段时间内的检测器输出信号综合起来,以便确定原始样品流45中的相应成分的浓度。Figure 8 is a graph showing the
加热元件20,22,24和26可以是涂覆在顶面和底面上的GC膜,因此可将加热元件表面的宽度和功耗降低约两倍。这些加热元件的制造涉及到两次涂覆步骤,其中第二步骤要求在保护第二晶片内的第一涂层和溶解第一晶片之后进行晶片-晶片结合和涂覆。The
图9是类似于图3所示的另一示例性传感器组件15的示意图。该传感器组件可包括更简单的螺线管泵120、流式样品流体122、浓缩器124、分离器126、检测器128和控制器14或130。应控制器14,130的请求,螺线管泵120可通过单向阀134来从烟道气体流132中抽取样品45。控制器14,130然后可使螺线管泵120在所需的压力下将流式样品流体45提供给浓缩器124。FIG. 9 is a schematic diagram of another
浓缩器124可包括两个或多个与流式样品流体45相通的交互式元件。浓缩器124还可包括两个或多个与交互式元件热连通的加热元件。在被激励时,各加热元件加热相应的交互式元件,导致交互式元件将选定成分解吸到流式样品流体中。如上所述,控制器14,130可以时相顺序来激励加热元件,从而提供增强的浓度脉冲。
流式样品流体45可将浓度脉冲携带至分离器126。分离器126从浓度脉冲中分离出选定的成分,并将所分离的成分提供给检测器50,128,164。该检测器可提供信号给控制器14,130,从而指示出各成分的浓度水平。控制器14,130还可通过将所检测到的浓度水平除以由各交互式元件的吸附材料所提供的浓度放大系数和由相控加热器装置所提供的乘数效应来确定原始气体样品中各成分的实际浓度水平。
图10是另一示例性传感器组件15的示意图。图11是显示了图10所示传感器组件15的操作的时序图。传感器组件15可包括泵152、气体预热器154和微桥型集成电路芯片156。该微桥型集成电路芯片156包括通道158,32、多个加热元件160a,160b,160c和160d、分离加热器162和检测器164,128,50。各个加热元件160a,160b,160c和160d、分离加热器162以及检测器164均设置在支撑件30上,该支撑件30在通道158,32的上方延伸(例如图5b)。在通道158,32内设有交互式元件(未明确示出),其与各个加热元件160a,160b,160c和160d热连接。FIG. 10 is a schematic diagram of another
微桥型集成电路芯片156还可包括加热器控制块166和多个激励晶体管168a,168b,168c,168d和170。加热器控制块166可通过分别激发相应的激励晶体管168a,168b,168c,168d来单独地激励各个加热元件160a,160b,160c和160d。类似的,加热器控制块166可通过接通晶体管170来激励分离加热器162。加热或冷却块169(图10中)帮助预热器154保持对传感器组件15的操作来说为最优的平均或整体温度。The microbridge
传感器组件的控制块180指挥传感器组件15的整体操作。传感器组件控制块180首先确定到泵152的流量控制信号190。流量控制信号190如图11所示。作为响应,泵152从烟道气182中抽取样品,并且在所需的压力下将样品提供给预热器154,并最终提供给通道158,32。预热器154进行预热,加热器将样品气体保持在最佳操作元件温度下,因此可以帮助防止因浓缩而产生的样品损失,并且增加积聚在各个交互式元件中的成分的量。The
流式样品流体向下经过通道158,32达预定的时间间隔192,直到交互式元件到达流式样品流体中的一种或多种成分的吸附基本上饱和的状态并且达到平衡时为止。之后,传感器组件控制块180通知加热器控制块166开始以时相顺序来加热这些加热元件。加热器控制块166首先提供第一加热器使能信号194和分离加热器使能信号196,如图11所示。第一加热器使能信号194接通晶体管168a,分离加热器使能信号196接通晶体管170。晶体管168a提供电流给第一加热元件160a,导致第一加热元件160a的温度升高。这便加热了相应的交互式元件,其以第一浓度脉冲的形式将一种或多种成分解吸到流式样品流体中。第一浓度脉冲被流式样品流体向下游携带到第二加热元件160b中。这一过程针对第三、第四和第N个元件重复进行。The streaming sample fluid is passed down the
加热器控制块166然后提供第二加热器使能信号198,其接通晶体管168b。晶体管168b提供电流给第二加热元件160b,导致第二加热元件160b的温度升高。这便加热了相应的交互式元件,其以第二浓度脉冲的形式将一种或多种成分解吸到流式样品流体中。加热器控制块166可对第二加热器使能信号198进行时控,使得第二浓度脉冲基本上重叠在第一浓度脉冲上。第一和第二浓度脉冲均被向下携带至第三加热元件160c中。The heater control block 166 then provides a second heater enable
可通过之前的校准来建立第二加热器使能信号198相对于第一加热器使能信号194的时控。然而,加热器控制块166可检测到第二加热元件160b的电阻。可以认识到,当第一浓度脉冲到达第二加热元件160b处,第二加热元件160b的电阻将开始变化,这是因为第一浓度脉冲通常比流式样品流体更热。一旦在第二加热元件160b中检测到预定的电阻变化,加热器控制块166便经由晶体管168b来激励第二加热元件160b。其余的加热器使能信号可类似地控制。The timing of the second heater enable
加热器控制块166然后提供第三加热器使能信号202,其接通晶体管168c。晶体管168c提供电流给第三加热元件160c,导致第三加热元件160c的温度升高。这便加热了相应的交互式元件,其在第三浓度脉冲之前将一种或多种成分解吸到流式样品流体中。加热器控制块166可对第三加热器使能信号200进行时控,使得第三浓度脉冲基本上覆盖在第一和第二浓度脉冲上。第一、第二和第三基本上重叠的浓度脉冲向下游被携带至第N个加热元件160d。The heater control block 166 then provides a third heater enable
加热器控制块166然后提供第N个加热器使能信号200,其接通晶体管168c。晶体管168c提供电流给第N个加热元件160d,导致第N个加热元件160c的温度升高。这便加热了相应的交互式元件,其在第N个浓度脉冲之前将一种或多种成分解吸到流式样品流体中。加热器控制块166可对第N个加热器使能信号202进行时控,使得第N个浓度脉冲基本上覆盖在前面产生的浓度脉冲上。所得的浓度脉冲向下游被携带至分离器加热器162。分离器加热器162与通道158相结合地将浓度脉冲中的选定成分分离成单独的组成成分。分离器的温度逐渐升高不应早于发送给第N个浓缩器元件的第N个脉冲结束的时候。因此,脉冲196在脉冲202结束后开始,如图11所示。各个组成成分可包括一种或多种化合物,这取决于包括所提供样品气体在内的多个因素。The heater control block 166 then provides the Nth heater enable
晶体管170然后在图11中的脉冲196开始时激励分离加热器162,导致加热器162的温度在脉冲196的约一半长度的时间内从室温上升到约200摄氏度(或其它设计温度),然后保持在该温度下达到脉冲196的剩余时间。加热器162如上所述地将各种成分分离成单独的组分。所分离出的成分通过流式样品流体向下游携带至检测器164。检测器164可以是可以是热导率检测器、放电电离检测器,或者任何其它类型的检测器,例如通常用于气相或液相色谱仪中的检测器。检测器164可检测各种单独组成成分的浓度水平,并且提供相应的信号给放大器210。放大器210可放大检测器的输出信号,并将该检测器输出信号提供给数据处理单元以供分析。加热器控制块166可提供检测器使能信号212,从而仅在单独组成成分存在时启动检测器。
图12是包括了微量气体装置15的浓缩器、分离器和检测器的集成电路的基本布局。该集成电路可包括通道250,其在芯片上来回穿过,如图12所示。通道250的第一部分具有检测器263,以及多个在支撑件、例如上述支撑件30上延伸的加热元件252。交互式元件(未明确示出)设置在通道250中并与各加热元件相邻。虽然仅显示了一排加热元件252,然而可以构思出各个通道支路254a-h均可具有一排加热元件252。沿着通道250可间隔开地设置2到1000个加热元件。FIG. 12 is the basic layout of the integrated circuit including the concentrator, separator and detector of the
通道250的第二下游部分具有在其上延伸的分离加热器260。分离加热器可帮助分离由加热元件252所提供的浓度脉冲中的各种成分。最后,在通道250上的分离加热器260的下游设置了检测器264。检测器可检测由分离器提供的各单独组成成分的浓度。The second downstream portion of
由于浓缩器、分离器和检测器设置在一个集成电路上,因此其它传统的电子电路可以容易地与之集成在一起。相控加热器控制块270和放大器272可制造在该同一衬底上。化学传感器、尤其是所介绍的化学微传感器可以提供许多有吸引力的特征,例如低成本、高灵敏度、坚固和很小的尺寸。Since the concentrator, separator and detector are set on one integrated circuit, other conventional electronic circuits can be easily integrated with it. Phased heater control block 270 and
虽然已经针对至少一个示例性实施例来介绍了本发明,然而在阅读了本说明书之后,本领域的技术人员将清楚许多变更和修改。因此,所附权利要求的意义应根据现有技术来尽可能宽广地解释,以便包括所有这种变更和修改。While the invention has been described with respect to at least one exemplary embodiment, numerous alterations and modifications will become apparent to those skilled in the art after reading the present specification. Therefore, the meaning of the appended claims should be interpreted as broadly as possible in light of the prior art so as to include all such changes and modifications.
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| CN103698380A (en) * | 2013-11-05 | 2014-04-02 | 上海昶艾科技发展有限公司 | Electrochemical trace oxygen analyzer for effectively prolonging usage life of sensor |
| CN112345657B (en) * | 2019-08-08 | 2023-03-31 | 宝武碳业科技股份有限公司 | Array sensing gas chromatograph and method for detecting multiple VOCs gases |
| KR102703191B1 (en) * | 2019-09-20 | 2024-09-04 | 인피콘 아크티엔게젤샤프트 | Method for determining pressure and pressure sensor |
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