CN105021674A - Verification method of gas humidity detector - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000012795 verification Methods 0.000 title claims description 25
- 238000001514 detection method Methods 0.000 claims abstract description 73
- 239000007789 gas Substances 0.000 claims abstract description 36
- 238000005070 sampling Methods 0.000 claims abstract description 34
- 239000000344 soap Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000002347 injection Methods 0.000 claims abstract description 8
- 239000007924 injection Substances 0.000 claims abstract description 8
- 238000005259 measurement Methods 0.000 claims abstract description 6
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- 238000003869 coulometry Methods 0.000 description 1
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- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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Abstract
本发明涉及一种气体湿度检测仪的校验方法，气体湿度检测仪包括进样系统、检测系统和数据处理与控制系统，校验方法包括以下步骤，进样系统校验：采用皂膜流计测量进样系统进样量，通过比较皂膜流计测量值和检测仪检测值，校验进样系统流量大小和计量准确性；检测系统校验：将已知量的蒸馏水或除盐水注入检测仪的电解池，通过比较蒸馏水的理论值和检测仪检测值，或除盐水的理论值和检测仪检测值，校验检测系统的准确性；气体湿度检测仪检测准确性校验：采用已知湿度的氮气，通过比较氮气湿度的理论值和检测仪检测值，校验检测仪检测准确性；本发明通过同时对进样系统、检测系统和检测仪整体进行校验，可以更加有效的评价检测仪检测性能。
The invention relates to a calibration method of a gas humidity detector. The gas humidity detector includes a sampling system, a detection system, and a data processing and control system. The calibration method includes the following steps. The calibration of the sampling system: using a soap film flow meter Measure the injection volume of the sampling system, and verify the flow rate and measurement accuracy of the sampling system by comparing the measured value of the soap film flow meter with the detection value of the detector; check the detection system: inject a known amount of distilled water or desalted water into the detection The electrolytic cell of the instrument is used to verify the accuracy of the detection system by comparing the theoretical value of distilled water with the detection value of the detector, or the theoretical value of desalted water and the detection value of the detector; the detection accuracy of the gas humidity detector is verified: use known Humid nitrogen, by comparing the theoretical value of the nitrogen humidity with the detection value of the detector, the detection accuracy of the detector is verified; the present invention can more effectively evaluate the detection by simultaneously verifying the sampling system, the detection system and the detector as a whole Instrument detection performance.
Description
技术领域technical field
本发明涉及校验方法，具体涉及一种气体湿度检测仪的校验方法。The invention relates to a calibration method, in particular to a calibration method for a gas humidity detector.
背景技术Background technique
卡尔·费休库仑法利用电化学反应原理测定水分含量的测定方法，是一种成熟、经典的微量水分检测方法并且测定结果最为准确的化学方法，常被作为水分特别是ppm痕量水分的标准分析方法，用以校正其它的测定方法，基于该方法研制出SF6气体湿度的检测仪；该检测仪不同于露点法和阻容法SF6气体湿度检测仪，因其是一种绝对测量方法，它可有效、真实的检测出SF6气体的湿度；因此，检测仪器性能的好坏直接关系到检测结果的准确性，对该种方法仪器的校验至关重要的。The Karl Fischer Coulomb method uses the principle of electrochemical reaction to determine the moisture content. It is a mature and classic trace moisture detection method with the most accurate chemical method. It is often used as the standard for moisture, especially ppm trace moisture. Analytical method, used to correct other determination methods, based on this method, a detector for SF 6 gas humidity was developed; this detector is different from the dew point method and resistance capacitance method SF 6 gas humidity detector, because it is an absolute measurement method , it can effectively and truly detect the humidity of SF 6 gas; therefore, the performance of the detection instrument is directly related to the accuracy of the detection results, which is very important for the calibration of this method.
现有的校验方法一般只能从整体上校验其检测的准确性，不能检测具体各个部分的准确性，并且很难找到具体的原因。Existing verification methods generally can only verify the accuracy of its detection as a whole, but cannot detect the accuracy of specific parts, and it is difficult to find specific reasons.
发明内容Contents of the invention
本发明提供一种可以分别校验进样系统、检测系统和整体检测的准确性的校验方法。The invention provides a verification method capable of separately verifying the accuracy of the sampling system, the detection system and the overall detection.
本发明采用的技术方案是：气体湿度检测仪包括进样系统、检测系统和数据处理与控制系统，其校验方法包括以下步骤：The technical scheme adopted in the present invention is: the gas humidity detector includes a sampling system, a detection system, and a data processing and control system, and its verification method includes the following steps:
进样系统校验：采用皂膜流计测量进样系统进样量，通过比较皂膜流计测量值和检测仪检测值，校验进样系统流量大小和计量准确性；Sampling system verification: use soap film flow meter to measure the sample injection volume of the sampling system, and verify the flow rate and measurement accuracy of the sampling system by comparing the measured value of the soap film flow meter with the detection value of the detector;
检测系统校验：将已知量的蒸馏水或除盐水注入检测仪的电解池，通过比较蒸馏水的理论值和检测仪检测值，或除盐水的理论值和检测仪检测值，校验检测系统的准确性；Detection system calibration: inject a known amount of distilled water or desalted water into the electrolytic cell of the detector, and verify the detection system by comparing the theoretical value of distilled water with the detection value of the detector, or the theoretical value of desalted water and the detection value of the detector. accuracy;
气体湿度检测仪检测准确性校验：采用已知湿度的氮气，通过比较氮气湿度的理论值和检测仪检测值，校验检测仪检测准确性。Calibration of the detection accuracy of the gas humidity detector: use nitrogen with known humidity, and verify the detection accuracy of the detector by comparing the theoretical value of the nitrogen humidity with the detection value of the detector.
作为优选，所述进样系统校验中根据环境温度和大气压将皂膜流计测量得到的气体进样量大小换算成标准状况下体积，与检测仪检测值比较。Preferably, in the calibration of the sampling system, the gas injection volume measured by the soap film flow meter is converted into the volume under standard conditions according to the ambient temperature and atmospheric pressure, and compared with the detection value of the detector.
作为优选，所述进样系统校验中测量至少2次皂膜流计的进样量，取平均值，计算相对误差，满足设定的相对误差范围，则判定检测仪进样系统准确。As a preference, in the calibration of the sampling system, measure the injection volume of the soap film flow meter at least twice, take the average value, calculate the relative error, and if the set relative error range is satisfied, then it is judged that the sampling system of the detector is accurate.
作为优选，所述相对误差值不大于皂膜流计满量程的0.8％，判定检测仪进样系统准确。As a preference, the relative error value is not more than 0.8% of the full scale of the soap film flow meter, and it is judged that the sampling system of the detector is accurate.
作为优选，所述检测系统校验过程将已知含水量的标样注入检测仪电解池，通过比较含水量的理论值和检测仪检测值，校验检测系统的准确性。Preferably, in the detection system verification process, a standard sample with known water content is injected into the electrolytic cell of the detector, and the accuracy of the detection system is verified by comparing the theoretical value of water content with the detection value of the detector.
作为优选，所述检测系统校验中进行至少两次平行试验。Preferably, at least two parallel experiments are performed in the detection system calibration.
作为优选，所述检测值和理论值的相对误差不超过±5％，判定检测仪检测系统准确。Preferably, the relative error between the detected value and the theoretical value does not exceed ±5%, which means that the detection system of the detector is accurate.
作为优选，所述气体湿度检测仪检测准确性校验过程中至少测定10个样本，计算其标准偏差，，满足设定的标准偏差范围，则判定检测仪准确。。Preferably, at least 10 samples are measured during the detection accuracy verification process of the gas humidity detector, and the standard deviation is calculated. If the set standard deviation range is met, the detector is determined to be accurate. .
作为优选，所述标准偏差为7.14-1.10％，判定检测仪准确。Preferably, the standard deviation is 7.14-1.10%, which means the detector is accurate.
作为优选，所述皂膜流计为经校准的标准数字皂膜流计。Preferably, the soap film flow meter is a calibrated standard digital soap film flow meter.
本发明的有益效果是：The beneficial effects of the present invention are:
(1)本发明可以对进样系统、检测系统和检测仪整体进行校验，能够更加有效的评价检测仪器检测性能的好坏；(1) The present invention can calibrate the sampling system, the detection system and the detector as a whole, and can more effectively evaluate the detection performance of the detection instrument;
(2)本发明校验准确性更高、更有针对性。(2) The verification accuracy of the present invention is higher and more targeted.
附图说明Description of drawings
图1为本发明中气体湿度检测仪结构示意图。Fig. 1 is a schematic structural diagram of a gas humidity detector in the present invention.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明做进一步说明。The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.
气体湿度检测仪包括进样系统、检测系统和数据处理与控制系统，其校验方法包括以下步骤：The gas humidity detector includes a sampling system, a detection system, and a data processing and control system, and its verification method includes the following steps:
进样系统校验：采用皂膜流计测量进样系统进样量，通过比较皂膜流计测量值和检测仪检测值，校验进样系统流量大小和计量准确性；Sampling system verification: use soap film flow meter to measure the sample injection volume of the sampling system, and verify the flow rate and measurement accuracy of the sampling system by comparing the measured value of the soap film flow meter with the detection value of the detector;
检测系统校验：将已知量的蒸馏水或除盐水注入检测仪的电解池，通过比较蒸馏水的理论值和检测仪检测值，或除盐水的理论值和检测仪检测值，校验检测系统的准确性；Detection system calibration: inject a known amount of distilled water or desalted water into the electrolytic cell of the detector, and verify the detection system by comparing the theoretical value of distilled water with the detection value of the detector, or the theoretical value of desalted water and the detection value of the detector. accuracy;
气体湿度检测仪检测准确性校验：采用已知湿度的氮气，通过比较氮气湿度的理论值和检测仪检测值，校验检测仪检测准确性。Calibration of the detection accuracy of the gas humidity detector: use nitrogen with known humidity, and verify the detection accuracy of the detector by comparing the theoretical value of the nitrogen humidity with the detection value of the detector.
进样系统校验中将皂膜流计测量得到的气体进样量大小换算成标准状况下体积，与检测仪检测值比较；进样系统校验中测量至少2次皂膜流计的进样量，取平均值，计算相对误差；相对误差值不大于皂膜流计满量程的0.8％，判定检测仪进样系统准确。In the calibration of the sampling system, the gas injection volume measured by the soap film flow meter is converted into the volume under standard conditions, and compared with the detection value of the detector; in the calibration of the sampling system, the injection of the soap film flow meter is measured at least twice measure, take the average value, and calculate the relative error; the relative error value is not greater than 0.8% of the full scale of the soap film flow meter, and it is determined that the sampling system of the detector is accurate.
校验时，采用经校准的标准数字皂膜流计的进样口与气体湿度检测仪放空口处相连接；向皂膜流计添加肥皂水，检测仪开始进样同时开始进样同时开启皂膜流计量按钮，分别记下气体湿度检测仪和皂膜流计的流量大小；记录下环境温度、大气压，然后将气体湿度检测仪气体进样量的大小换算成标准状况下体积大小，以皂膜流计三次计量结果的平均值，计算相对误差，其值不大于满量程的0.8％，则判定检测仪检测准确性，如果相对误差值大于满量程的0.8％，则需要对检测仪进行校准。When calibrating, connect the sampling port of the calibrated standard digital soap film flow meter to the vent port of the gas humidity detector; add soapy water to the soap film flow meter, and the detector starts to inject samples at the same time and open the soap at the same time. Press the membrane flow measurement button to record the flow rate of the gas humidity detector and the soap film flow meter respectively; record the ambient temperature and atmospheric pressure, and then convert the gas sample volume of the gas humidity detector into the volume under standard conditions, and use soap The average value of the three measurement results of the membrane flow meter is used to calculate the relative error. If the value is not greater than 0.8% of the full scale, the detection accuracy of the detector can be judged. If the relative error value is greater than 0.8% of the full scale, the detector needs to be calibrated .
检测系统校验过程将已知含水量的标样注入检测仪电解池，通过比较含水量的理论值和检测仪检测值，校验检测系统的准确性，至少进行两次平行试验；检测值和理论值的相对误差不超过±5％，判定检测仪检测系统准确。During the verification process of the detection system, the standard sample with known water content is injected into the electrolytic cell of the detector, and the accuracy of the detection system is verified by comparing the theoretical value of the water content with the detection value of the detector, and at least two parallel tests are carried out; The relative error of the theoretical value is not more than ±5%, and it is determined that the detection system of the detector is accurate.
校验时，用0.5μL注射器量取0.1μL蒸馏水、除盐水或已知含水量的标样，开启检测仪手动进样模式，通过电解池上部的手动进样口注入电解池，进行三次平行试验；检测仪的显示值即其检测值与理论值的相对误差不超过±5％，则判定检测仪准确，若检测仪的显示值即其检测值与理论值的相对误差超过±5％，则需要对检测仪进行校准。During calibration, use a 0.5 μL syringe to measure 0.1 μL of distilled water, demineralized water or a standard sample with known water content, turn on the manual sampling mode of the detector, inject the electrolytic cell through the manual sampling port on the upper part of the electrolytic cell, and perform three parallel tests ; The display value of the detector, that is, the relative error between the detected value and the theoretical value does not exceed ±5%, then it is judged that the detector is accurate; if the displayed value of the detector, that is, the relative error between the detected value and the theoretical value exceeds ±5%, then Calibration of the detector is required.
气体湿度检测仪检测准确性校验过程中至少测定10个样本，计算其标准偏差；标准偏差为7.14-1.10％，判定检测仪准确。During the verification process of the detection accuracy of the gas humidity detector, at least 10 samples are measured, and the standard deviation is calculated; the standard deviation is 7.14-1.10%, and the detector is judged to be accurate.
校验时，选取4种不同湿度的氮气进行检测，每个样品测定5次后，对检测结果计算其标准偏差，其标准偏差为7.14-1.10％，则判定检测仪准确；若标准偏差不在此范围内，则需要对检测仪进行校准。When calibrating, select 4 kinds of nitrogen with different humidity for testing, and after measuring each sample 5 times, calculate the standard deviation of the test results, and if the standard deviation is 7.14-1.10%, it is judged that the detector is accurate; if the standard deviation is not in this Within the range, the detector needs to be calibrated.
本发明主要针对于基于卡尔·费休库仑法SF6气体湿度检测仪的校验，因为这种气体湿度检测仪对于准确性要求更高，所以其校验更加重要；本发明采用校验进样系统、校验检测系统和整体的检测准确性同时进行，可以有效评价检测仪检测性能的好坏。The present invention is mainly aimed at the verification of the SF 6 gas humidity detector based on the Karl Fischer coulometric method, because this gas humidity detector has higher requirements for accuracy, so its verification is more important; The system, calibration and detection system and the overall detection accuracy are carried out at the same time, which can effectively evaluate the detection performance of the detector.
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention should be included in the protection of the present invention. within range.
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Application publication date: 20151104 |