阅读说明：本技术 一种离子探针实验室监控系统及方法 (Ion probe laboratory monitoring system and method ) 是由 杨晴 夏小平 张万峰 张彦强 杨亚楠 何妙 于 2020-02-27 设计创作，主要内容包括：本发明公开一种离子探针实验室监控系统及方法,涉及实验室仪器状态及实验环境检测技术领域,包括温湿度监测单元、冷却系统监测单元、离子流强度监测单元以及特定分析结果监测单元,温湿度监测单元控制二次离子质谱仪周围的温湿度探头,冷却系统监测单元控制二次离子质谱仪的冷却水路上的冷却水流速表,离子流强度监测单元控制二次离子质谱仪一次离子源处的一次离子源强度获取装置,特定分析结果监测单元控制二次离子质谱仪接收器部分的离子接收器。本发明的有益效果是：通过在离子探针实验室布控监控系统,使得工程师能够精准地获取实验室的实时情况,减少仪器非分析机时的损耗,提高仪器的使用效率。(The invention discloses an ion probe laboratory monitoring system and method, which relate to the technical field of laboratory instrument state and experimental environment detection and comprise a temperature and humidity monitoring unit, a cooling system monitoring unit, an ion current intensity monitoring unit and a specific analysis result monitoring unit, wherein the temperature and humidity monitoring unit controls temperature and humidity probes around a secondary ion mass spectrometer, the cooling system monitoring unit controls a cooling water flow velocity meter on a cooling water path of the secondary ion mass spectrometer, the ion current intensity monitoring unit controls a primary ion source intensity acquisition device at a primary ion source of the secondary ion mass spectrometer, and the specific analysis result monitoring unit controls an ion receiver of a receiver part of the secondary ion mass spectrometer. The invention has the beneficial effects that: through deploying the control monitored control system at the ion probe laboratory for the engineer can accurately obtain the real-time condition in laboratory, loss when reducing the non-analysis of instrument machine improves the availability factor of instrument.)

1. An ion probe laboratory monitoring system, characterized in that: including humiture monitoring unit (4), cooling system monitoring unit (5), ion current intensity monitoring unit (6) and specific analysis result monitoring unit (7), humiture probe (8) around humiture monitoring unit (4) control secondary ion mass spectrometer (2), cooling water velocity of flow table (9) on the cooling water route of cooling system monitoring unit (5) control secondary ion mass spectrometer (2), ion current intensity monitoring unit (6) control secondary ion mass spectrometer (2) primary ion source intensity acquisition device (10) of department, specific analysis result monitoring unit (7) control secondary ion mass spectrometer (2) receiver partial ion receiver (11).

2. The ion probe laboratory monitoring system of claim 1, wherein: the temperature and humidity probe (8) is a wireless probe, the temperature precision and the temperature accuracy are respectively 0.01 ℃ and +/-0.2 ℃, and the humidity precision and the temperature accuracy are respectively 0.1% and +/-0.5%.

3. The ion probe laboratory monitoring system of claim 1, wherein: the cooling water flow meter (9) is a Proteus Flowmeter flow meter.

4. An ion probe laboratory monitoring method for use in the ion probe laboratory monitoring system according to any one of claims 1 to 3,

the instrument state monitoring software (3) integrates the acquired data of the temperature and humidity monitoring unit (4), the cooling system monitoring unit (5), the ion current intensity monitoring unit (6) and the specific analysis result monitoring unit (7) into a monitoring interface;

the temperature and humidity monitoring unit (4) acquires temperature and humidity signals of the surrounding environment of the secondary ion mass spectrometer (2) through a temperature and humidity probe (8), the read temperature and humidity signals are transmitted back to the temperature and humidity monitoring unit (4) in the computer (1) through a wireless receiving module, a threshold value is set in the instrument state monitoring software (3), and when temperature and humidity fluctuation exceeds the threshold value, the instrument state monitoring software (3) automatically sends information to an engineer or automatically stops the operation of an instrument;

the cooling system monitoring unit (5) acquires a rotating speed signal of cooling water through a cooling water flow rate meter (9), the rotating speed signal is fed back to the cooling water monitoring unit (5) in the computer (1) in real time for storage, and when the cooling system is occasionally or intermittently failed, the instrument state monitoring software (3) automatically sends information to an engineer or automatically stops the operation of the instrument;

the primary ion current intensity monitoring (6) unit reads the intensity of the primary ion current of the instrument in real time through the primary ion source intensity acquisition device (10), the instrument state monitoring software (3) sets a fluctuation threshold and a maximum and minimum threshold, and when any one of the thresholds is exceeded, the instrument state monitoring software (3) automatically sends information to an engineer or automatically stops the operation of the instrument;

the specific analysis result monitoring unit (7) presets corresponding threshold values according to analysis systems of different substances, monitors specific analysis data of different analysis methods through the ion receiver (11), and when the specific analysis data exceed the threshold values, the instrument state monitoring software (3) automatically sends information to an engineer or automatically stops running of the instrument.

Technical Field

The invention relates to the technical field of laboratory instrument state and experimental environment detection, in particular to an ion probe laboratory monitoring system and method.

Background

The secondary ion mass spectrometry is an advanced method for micro-area in-situ analysis, has the advantages of high sensitivity, high spatial resolution and high precision, is rapidly developed in related fields of geography in recent years, and has no alternative application value in geoscience. However, the price of the large-scale secondary ion mass spectrometer is high (about 4000 ten thousand RMB), the number of the large-scale secondary ion mass spectrometers in China is small, the application amount is large, the demand is strong, and therefore the instrument testing machine is very tense.

Therefore, the loss of the instrument when the instrument is not an analyzer is reduced, and the use efficiency of the instrument is improved, which is a common urgent need of all laboratories of the same type in the world.

Disclosure of Invention

Aiming at the problems, the invention provides an ion probe laboratory monitoring system and method, which are used for monitoring the room temperature and humidity of a laboratory, an instrument cooling system, the ion current intensity of an instrument, a specific analysis result and the like in real time by developing a software and hardware monitoring device, so that the use efficiency of the instrument is improved when the instrument is not operated effectively.

In order to solve the technical problems, the technical scheme of the invention is as follows:

the utility model provides an ion probe laboratory monitored control system, including humiture monitoring unit, cooling system monitoring unit, ion current intensity monitoring unit and specific analysis result monitoring unit, humiture probe around the humiture monitoring unit control secondary ion mass spectrometer, cooling water velocity of flow table on the cooling water route of cooling system monitoring unit control secondary ion mass spectrometer, the primary ion source intensity acquisition device of ion current intensity monitoring unit control secondary ion mass spectrometer primary ion source department, the ion receiver of specific analysis result monitoring unit control secondary ion mass spectrometer receiver part.

On the basis, an ion probe laboratory monitoring method is further provided, which is used for the ion probe laboratory monitoring system of the first embodiment, and specifically comprises the following steps:

integrating the data obtained by the temperature and humidity monitoring unit, the cooling system monitoring unit, the ion current intensity monitoring unit and the specific analysis result monitoring unit into a monitoring interface by instrument state monitoring software;

the temperature and humidity monitoring unit acquires temperature and humidity signals of the ambient environment of the secondary ion mass spectrometer through a temperature and humidity probe, the read temperature and humidity signals are transmitted back to the temperature and humidity monitoring unit in the computer through the wireless receiving module, a threshold value is set in the instrument state monitoring software, and when temperature and humidity fluctuation exceeds the threshold value, the instrument state monitoring software automatically sends information to an engineer or automatically stops the operation of the instrument;

the cooling system monitoring unit acquires a rotating speed signal of cooling water through a cooling water flow meter, the measured rotating speed signal is fed back to the cooling water monitoring unit in the computer in real time for storage, and when the cooling system has occasional or intermittent faults, the instrument state monitoring software automatically sends information to an engineer or automatically stops the operation of the instrument;

the primary ion current intensity monitoring unit reads the intensity of the primary ion current of the instrument in real time through the primary ion source intensity acquisition device, the instrument state monitoring software sets a fluctuation threshold and a maximum and minimum threshold, and when any threshold is exceeded, the instrument state monitoring software automatically sends information to an engineer or automatically stops the operation of the instrument;

the specific analysis result monitoring unit presets and sets corresponding threshold values according to analysis systems of different substances, monitors specific analysis data of different analysis methods of the ion receiver, and when the specific analysis data exceed the threshold values, the instrument state monitoring software automatically sends information to an engineer or automatically stops running of the instrument.

The invention has the beneficial effects that:

1. through deploying the control monitored control system at the ion probe laboratory for the engineer can accurately obtain the real-time condition in laboratory, loss when reducing the non-analysis of instrument machine improves the availability factor of instrument.

2. By developing and detecting software and hardware systems, real-time monitoring is carried out on the temperature and humidity of the experimental room, a cooling system, the ion current intensity, specific analysis results and the like, a threshold value is set, and an engineer is timely informed of the condition of exceeding the threshold value, so that the environmental change, the instrument fault, the instrument state change and the invalid analysis time can be timely intervened, and the normal operation time of a secondary ion mass spectrometer instrument is improved.

Drawings

FIG. 1 is a schematic diagram of the construction of an ion probe laboratory monitoring system according to the present invention;

FIG. 2 is a flow chart of a laboratory monitoring method for ion probes in accordance with the present invention.

Wherein: the method comprises the following steps of 1-a computer, 2-a secondary ion mass spectrometer, 3-instrument state monitoring software, 4-a temperature and humidity monitoring unit, 5-a cooling system monitoring unit, 6-an ion current intensity monitoring unit, 7-a specific analysis result monitoring unit, 8-a temperature and humidity probe, 9-a cooling water flow velocity meter, 10-a primary ion source intensity obtaining device and 11-an ion receiver.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention clearer and clearer, the following detailed description of the present invention is provided with reference to the accompanying drawings and detailed description. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be further noted that, for the convenience of description, only some but not all of the relevant aspects of the present invention are shown in the drawings.

In the practical operation process of the secondary ion mass spectrometer, many factors can influence the normal operation of the instrument, so that the use efficiency of the instrument is damaged. These factors, by analysis, mainly include: 1) experimental room temperature humidity change: the magnetic field of the instrument and the like are influenced by the humidity of the room temperature of the experiment; 2) instrument cooling system: a switch that directly affects the instrument ion source; 3) primary ion current change: the change of the instrument ion source can directly cause the change of the analysis test result; 4) analyzing test data anomalies: the reproducibility of the analysis test standard sample data directly determines the result of the sample analysis in the same time period, and obviously and unreasonably eliminates unknown sample data and the like. The method comprises the following specific steps:

(1) experimental room temperature humidity changes. The mass spectrum analysis system of the secondary ion mass spectrometer adopts a double focusing mode of a fan-shaped electric field and a fan-shaped magnetic field, the magnetic field is obtained by adding a magnet weighing 4 tons and a specific voltage change, and the system is very sensitive to temperature and humidity. When the temperature changes, the change of the magnetic field can be detected obviously. The result of the analysis data is changed due to the irregular change of the magnetic field, the temperature and humidity change exceeds a certain range, the data result exceeds an tolerable error range and is meaningless, and the change is uncontrollable. Therefore, monitoring the change in temperature and humidity is essential.

(2) An instrument cooling system. The primary ion excitation device of the secondary ion mass spectrometer 1280-HR comprises a dual plasma ion source DUO or a thermal ionization cesium ion source, wherein both sources are monitored by a part with a function of monitoring the operation of a cooling system, but the monitoring only indicates whether the operation of the cooling system is normal through an indicator lamp, a water lamp and a vacuum safety lamp of an oxygen source are turned off to indicate a fault, a vacuum safety lamp of the cesium source is turned on to indicate a fault, and the ion source stops working as long as the fault occurs, but the temperature and flow rate change of the cooling liquid are not necessarily monitored in real time. Sometimes the cooling system is only occasionally or intermittently malfunctioning and the indicator lights do not change state when checked, which increases the difficulty of diagnosing the malfunction. And under the unattended condition, the fault cannot be notified in time. Therefore, it is very necessary to develop a monitoring cooling system which is visible in real time.

(3) The primary ion current varies. At present, the secondary ion mass spectrometer 1280-HR instrument analysis and test can realize point selection in advance, and then the point sequence is analyzed one by one. In the analysis process, an experimenter or a user cannot continuously look at experimental conditions and data for 24 hours, so that sometimes violent change of a primary ion source of the instrument (such as extinguishing of the primary ion source, sharp increase or decrease of the energy of the ion source and the like) will happen, and if the violent change is not interfered in time after the situation happens (such as unattended situation), the machine and time waste of the instrument is caused. Primary ion current quenching is the most desirable deterioration result because only the machine is wasted and no damage is done to the sample; poor ion current stability may result in data being unusable and samples being reprocessed and reanalyzed; too large an ion current can damage the sample and the instrument receiver. Therefore, it is necessary to monitor the stability of the primary ion flow in real time.

(4) And analyzing the test data to be abnormal. In secondary ion mass spectrometry, elements or isotopes are not ionized in the proportions inherent in the sample, i.e., instrumental fractionation, which exhibits significant changes due to the different matrix composition of the sample being analyzed, known as the matrix effect. Due to the existence of matrix effect, accurate in situ analysis of micro-areas must use a sample with the same chemical composition and uniform composition of elements or isotopes to be analyzed as an external reference substance (standard sample) to correct the element content and isotope ratio of an unknown sample. The reproducibility of the analysis data of the external reference substance can be predicted under the condition that the state of the instrument is normal, the state of the instrument can be randomly changed sometimes, and the reproducibility of the standard substance is deteriorated, so that the instrument needs to be debugged again. Therefore, the specific analysis result of the external reference substance is monitored in real time, so that the change of the state of the instrument is interfered as early as possible, and the condition that the instrument cannot obtain the data with the analysis precision meeting the requirement when the instrument is wasted is avoided. In addition, the reasonability of the analysis data can be monitored in real time, and useless analysis can be eliminated in time, such as overhigh ordinary Pb of the zircon in definite years caused by disqualification of the zircon target, deviation of an analysis point, the fact that a secondary ion signal exceeds the analysis range of a detector and the like.

Therefore, by developing a software and hardware monitoring device, the temperature and humidity of the laboratory room, an instrument cooling system, the ion current intensity of the instrument, a specific analysis result and the like are monitored in real time, and an engineer is informed in time so as to intervene in environmental changes, instrument faults, instrument state changes and invalid analysis time in time, improve the normal operation time of the instrument, create a high-efficiency intelligent ion probe laboratory and enable the secondary ion mass spectrometer to have higher application efficiency.

Based on the above self-research, the following examples were obtained with modifications.