Device for reproduction and transmission of mass concentration units of oxygen and hydrogen in liquid media

FIELD: measurement equipment.

SUBSTANCE: device for reproduction and transmission of mass concentration units of oxygen and hydrogen in liquid media is based on subsequent preparation of standard liquid solutions and determination in them of content of dissolved oxygen or hydrogen. The device includes a working chamber, a temperature control system including a thermostat and a heat exchange circuit, a standard barometer, a standard thermometer with a sensor submerged into the medium of the working chamber, and a mixer. Besides, the device is provided with oxygen and hydrogen analysers; the working chamber is designed for high gas pressure and provided with an inspection hole and mounting seats for electrochemical and optical sensors of oxygen or hydrogen analysers, to which mass concentration units of oxygen and hydrogen are transmitted. Besides, the device is provided with a supply system of gas mixtures, which consists of bottles with control gas mixtures, an inert gas bottle and a control system of flow and flow rate of control gas mixtures, which includes a gas line, a bubbler for pumping of gas mixtures to the working chamber, fine adjustment valves installed at the inlet and outlet of the working chamber.

EFFECT: enlarging functional capabilities and improving calibration accuracy of analysers.

3 cl, 1 dwg

 

The invention relates to the field of measuring technique, namely the measurement of the concentration of oxygen and hydrogen that are designed for verification, calibration of analyzers dissolved oxygen and hydrogen used at the enterprises of thermal and nuclear power engineering, metallurgy, food, chemical and refining industries, in biotechnology and medicine, housing, fish farms and sewage treatment plants.

It is known device [RF Patent for the invention №2365948, G01W 1/18, 2009] for calibration and verification of gas analyzers containing temperature gauges and pressure, output, communication, liquid thermostat, nautical, stabilizer high pressure used liquid thermostat - passive, with nautical is a steel vessel, designed for high pressure gas, 30-60% of the volume filled with liquid dosing component, through which is passed a carrier gas supplied through the bubbler.

The disadvantage of this device is relatively narrow functionality. The device eliminates the possibility to measure the mass concentration of dissolved gas in a liquid medium.

As the closest analogue of the selected device for calibration and verification of analyzers, dissolved oxygen, based on the last�consistently in the preparation of sample solutions of distilled water and the determination of dissolved oxygen graded or checked by the analyzer amperometric sensor, closed permeable to oxygen membrane containing working chamber with the gaseous phase receiver and immersed in distilled water, the oxygen sensor, coupled with a graded or checked by the analyzer, the sample measuring absolute pressure, compressor, control unit, a mixer for mixing distilled water in the working chamber, a bubbler for pumping the gas mixture through the gas and liquid phase of the working chamber, a thermometer, a unit of automatic stabilization of the temperature in the working chamber, a spout for manual introduction liquid or gas additives in obeskislorozhennuju nitrogen distilled water, standalone receiver, pneumatically connected to a measuring absolute pressure, the control unit and the gaseous phase of the working chamber, an additional compressor in a stand-alone receiver, the cylinder with nitrogen, the vessel with nitrogen, equipped with a removable oxygen absorbers. [RF patent for useful model No. 133936, G01N 27/00, 2013].

Closest to the proposed device is intended for use with amperometric sensors analyzers dissolved oxygen from the environment.

The disadvantages of this device are the inability to measure oxygen in microgramos" area concentrations (less than 10 mg/DM3), narrow functional who�agnosti for verification and calibration of instruments and low accuracy of measurements, use as the basis of a solution of distilled water.

In order to extend the range of measurements of the concentration of oxygen dissolved in water and increase the accuracy of its reproduction, use dissolved in distilled water and other liquid media in which at a temperature of from 0 to 50°C is observed Henry's law-Dalton with the introduction of the correction factor, calibration gas mixture (ASG) and the working chamber to withstand high gas pressure. These technical improvements also allow you to play and transfer unit concentration of dissolved hydrogen. In addition, the device allows for calibration and verification only with amperometric sensors.

The object of the invention is to expand the functional capabilities of the device to implement with high fidelity and transfer of the units of mass concentration of dissolved oxygen and hydrogen on the basis of Henry's law-Dalton with the use of calibration gas.

The technical result is to increase functionality and improve the accuracy of testing and calibration of analyzers by changing the method of preparation of sample solution using the calibration gas.

The problem is solved, and the required technical result is achieved due �Chet, device for playback and transfer of the units of mass concentration of oxygen and hydrogen in liquid media based on the sequential preparation of sample solutions of liquids and the determination of dissolved oxygen or hydrogen containing working chamber, a thermal control system comprising a thermostat and a heat exchanger circuit, the reference barometer, reference thermometer with the sensor immersed in the environment of the working chamber, the stirrer, the device is equipped with analyzers of oxygen and hydrogen with enhanced metrological characteristics in comparison with commercially available, the working chamber is designed for high pressure gas and is made provided with an observation window and seats for electrochemical and optical sensors, analyzers, oxygen or hydrogen, which are transmitted in units of mass concentration of oxygen and hydrogen, the apparatus is provided with a supply system of gas mixtures consisting of cylinders of calibration gas mixtures, gas cylinder with inert gas system and flow control and flow of calibration gas mixtures, comprising a gas line, bubbler for pumping a gas mixture into the working chamber, the fine adjustment valves installed on the inlet and outlet of the working chamber. The working chamber can be made of stainless Stalis thickness of the cover and the wall with a viewing window 20 mm and a thickness of the other walls 10 mm, that allows you to create inside pressure of 1200 kPa. Valves, fine adjustment can be made in the form of acicular netcetera.

Between the set of essential features of the claimed object and achievable technical result there is a causal relationship, namely the design features of the working chamber allows to make measurements in the pressure range from atmospheric to 1200 kPa, which in turn expands the range of reproducible analyzers with electrochemical and optical sensors of oxygen concentrations from 0 to 100000 mg/DM3(compared with the device is analogous to the range of reproducible concentrations of oxygen 200-45000 mg/DM3and contributes to the reproduction of analyzers with electrochemical sensors for hydrogen concentration from 0 to 20,000 mg/DM3; the application of ice, flowing method of filing, the control of the gas flow and mixing of water through the viewing window reduce the systematic component of error in the reproduction units of concentration; the application of high-precision oxygen analyzers and hydrogen reduce the random component of error, the needle nakatali fine adjustment of the flow ASG realize high precision of maintaining the necessary pressure at continuous duct ASG; inspection door on�allows to control the ingress of gas bubbles on the sensor analyzers which are formed by vigorous stirring of the liquid phase in the chamber and lead to sharp spikes in concentration and, as a result, incorrect results of measurement of mass concentration of oxygen and hydrogen in a liquid medium.

Unlike the prototype of this device allows to reproduce the unit of the concentration of oxygen in water and other liquid media in which at a temperature of from 0 to 50°C is observed Henry's law-Dalton with the introduction of the correction factor, in the extended range from 0 to 100000 mg/DM3and unit the hydrogen concentration in the range from 0 to 20,000 mg/DM3.

The invention is illustrated by Fig. 1, which shows a diagram of the device for calibration and verification of oxygen analyzers.

The working chamber (1) made of stainless steel with the thickness of the lid and the wall with a viewing window (not digitized) 20 mm (10 mm due to the necessary groove for installation of inspection Windows and 10 mm for fixing screws M6 cap) and the thickness of the remaining walls of 10 mm, which allows you to create inside pressure of 1200 kPa. The viewing window has a rectangular shape and made of glass with a thickness of 8 mm. placed On the lid of the seat (18) for connection of sensors analyzers. The working chamber (1) equipped with a stirrer (4). The gas supply system consists of a calibration gas cylinders (16), the cylinder (17) with inert gas you�the eye of purity and system flow control and flow of calibration gas mixtures, includes gas line (15) with pressure reducing valves (not digitized), bubbler (6), the fine adjustment valves on the inlet (7) and outlet (8) of the working chamber. Thermal control system includes a thermostat (2) and the heat exchange circuit (3). Composition of the device also includes the following measurement tools: the hydrogen analyzer (10) with a sensor (9), the oxygen analyzer (12) with a sensor (11), the reference thermometer (14) with a sensor (13) and a reference barometer (5).

The device for playback and transfer of the units of mass concentration of oxygen and hydrogen is as follows.

The working chamber (1) filled with distilled water or other solvent (liquid) 70% of the total volume, then the injection of oxygen or hydrogen from cylinders of calibration gas (16) through a gas line (15) and bubbler (6) in the working chamber (1) where is the saturation gas to the values of the equilibrium concentrations, and the mixer is turned on (4), providing uniform distribution of the gas in the liquid. Control of the mixing is done through the observation window are not labeled and provided in the working chamber (1). The constancy of temperature of distilled water in the chamber is achieved by circulation of thermostated water through an external thermostat (2) by heat exchange circuit (3). The temperature control is made� reference thermometer (14). Excess pressure is adjusted by the fine adjustment valves on the inlet (7) and outlet (8). Pressure is controlled using reference barometer (5). To create a "zero" concentration oxygen using an inert gas of high purity (17). To control the concentration of oxygen and hydrogen by using the hydrogen analyzers (10) and oxygen (12) having advanced metrological characteristics relative to commercially available. Seats (18) are designed for connection of sensors which are in units of mass concentration of oxygen and hydrogen.

The device involves the following approach, characterizing measured by the analyzer, the value of dissolved oxygen concentration or hydrogen concentration of dissolved oxygen in the range from 0 to 100000 mg/DL3or hydrogen in the range from 0 to 20000 mg/DL3measured by the analyzer, which are transmitted in units of mass concentration of oxygen or hydrogen, corresponds to their solubility (equilibrium concentration) in a particular exemplary solution of distilled water at a constant temperature in the pressure range from atmospheric to 1200 kPa prepared by saturation by sparging system from cylinders of calibration gas at a constant temperature and a predetermined absolute pressure p�working camera 1. The method is suitable for calibration of analyzers, including electrochemical and optical oxygen sensors, allowing measurements under working conditions of high pressure of the working medium in the range of from atmospheric to 1200 kPa.

The basis of the method of preparation of solutions with a given concentration of a solute in a liquid medium of oxygen and hydrogen in a closed volume of the working chamber based on the mathematical dependence of Henry's law-Dalton characterizing linear change in the equilibrium concentrations of dissolved oxygen and hydrogen, obtained as by changing the oxygen content and hydrogen calibration gas mixtures - state standard samples (ASG-GSO) and absolute pressure of gases in the working chamber, as well as the dependence of the solubility of oxygen and hydrogen in distilled water temperature. The value of the concentration C at a pressure P, the relative volumetric gas content X (%) in the calibration gas mixture and the water temperature T is calculated by the formula:

where A is the solubility (equilibrium concentration) of oxygen or hydrogen in water (mg/l or %) at normal pressure and a temperature T (°C) (for oxygen according to ISO 5814: 2012); P is the current pressure (kPa), P0- normal atmospheric pressure of 101.3 kPa, X - �relative volume content of oxygen or hydrogen in ice, X0- the constant in the case of oxygen equal 20,94%, and for hydrogen - 100%, k - correction factor characterizing the type of liquid used as the liquid medium of the working chamber.

From (1) that changes the equilibrium concentration of solute in the liquid environment of oxygen or hydrogen at a constant temperature is directly proportional to the change in the magnitude of the absolute pressure in the working chamber.

Consequently, the linearity transformation of the analyzer under calibration can be estimated on the linearity of the change of the absolute pressure in the working chamber, characterized by exemplary readings of gauges absolute pressure (barometer, pressure gauge, vacuum gauge).

For the verification of the analyzer demand the value of the concentrations of dissolved oxygen and hydrogen calculated by the formula (1) is achieved by changing the absolute pressure in the gas phase of the working chamber and the application of calibration gas with different gas contents.

Basic absolute ∆ δ and relative errors are calculated by the formulas(2), (3):

where C is the concentration of dissolved oxygen was calculated by the formula (1), mg/DM3; CISM- the concentration of dissolved oxygen measured by the analyzer at an absolute pressure�research Institute P mg/DM3.

To assess the linearity of the calibration characteristics of the analyzer determines the error of the measurements at three points of the graded measurement range of the analyzer: the fixed points in the beginning, in the middle and at the end of the measuring range. The errors are calculated by relations (2) and (3).

Thus, in the proposed device is achieved the required technical result consists in expanding the functionality because it allows you to play and transfer units of mass concentration of oxygen in the extended range, and hydrogen in a wide range with high precision in water and other liquid media in which at a temperature of from 0 to 50°C is observed Henry's law-Dalton with the introduction of the correction factor.

1. The device for playback and transfer of the units of mass concentration of oxygen and hydrogen in liquid media based on the sequential preparation of sample solutions of liquids and the determination of dissolved oxygen or hydrogen containing working chamber, a thermal control system comprising a thermostat and a heat exchanger circuit, the reference barometer, reference thermometer with the sensor immersed in the environment of the working chamber, the agitator, characterized in that the device is equipped with analyzers of oxygen and hydrogen, slave�tea Luggage designed for high pressure gas and is made provided with an observation window and seats for electrochemical and optical sensors, analyzers, oxygen or hydrogen, which are transmitted in units of mass concentration of oxygen and hydrogen, the apparatus is provided with a supply system of gas mixtures consisting of cylinders of calibration gas mixtures, gas cylinder with inert gas system and flow control and flow of calibration gas mixtures, comprising a gas line, bubbler for pumping a gas mixture into the working chamber, the fine adjustment valves installed on the inlet and outlet of the working chamber.

2. The device according to claim 1, characterized in that the working chamber is made of stainless steel with the thickness of the lid and sides with an observation window of 20 mm and a thickness of the remaining walls of 10 mm, which allows you to create inside pressure of 1200 kPa.

3. The device according to claim 1, characterized in that the fine adjustment valves can be made in the form of acicular netcetera.



 

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