CN114755270A - Method and device for measuring pH temperature compensation of ammonia-containing pure water medium - Google Patents
Method and device for measuring pH temperature compensation of ammonia-containing pure water medium Download PDFInfo
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Abstract
The invention belongs to the technical field of calibration of detection instruments, and relates to a method and a device for measuring pH temperature compensation of an ammonia-containing pure water medium, wherein the method comprises the following steps: 1) and regulating the temperature of the ammonia-containing pure water to be constant Tn; 2) measuring the conductivity of pure ammonia-containing water at Tn, and calculating a standard pH value An (n is 1, 2, 3, … i, …) at 25 ℃; 3) measuring the actual pH value Bn of the ammonia-containing pure water under Tn; 4) collecting data; for each group of data values, the temperature is taken as an abscissa, and the difference between the standard pH value and the actual pH value is taken as an ordinate, so as to obtain a temperature compensation fitting curve; 5) and (4) bringing the temperature value t of the ammonia-containing water sample into the fitting curve to obtain a corresponding pH temperature compensation value, and performing compensation calibration on the measured value of the ammonia-containing water sample. The invention can realize the calibration of the pH meter, and has small error and high precision; the online calibration is realized, the smooth operation of the system is ensured, and the operation is simple and convenient.
Description
Technical Field
The invention belongs to the technical field of calibration of detection instruments, and relates to a method and a device for measuring pH temperature compensation of an ammonia-containing pure water medium.
Background
The pH meter consists of two parts, namely a sensor and a secondary meter, can be matched with three composite electrodes or two composite electrodes to meet various use places, is matched with pure water and an ultrapure water electrode, and can be suitable for measuring the pH value of water with the conductivity of less than 3 mu s/cm (such as chemical make-up water, saturated steam, condensed water and the like).
However, in the measurement process, the temperature of the water sample often deviates from 25 ℃, and in order to ensure the accuracy of the measurement result, the pH meter needs to be subjected to temperature compensation, so that the measurement accuracy is improved, but the following problems occur in the measurement of the pH in the actual production: (1) in the production process, the temperature of a water sample, the ion concentration in the water and the impurities are variable and fluctuant, particularly, the temperature compensation of a pH meter has great difference along with the change of a medium, and the inaccurate temperature compensation in pure water, particularly in an ammonia-containing pure water medium can cause great deviation of a pH measured value, so that the meter is calibrated only by a buffer solution without considering the change of the medium condition of the water sample, and the measured result has serious deviation; (2) when the pH value of the ammonia-containing pure water medium is measured, temperature compensation of a buffer solution medium is used in many production plants, and a large error occurs in a final result, so that the key for improving the pH measurement accuracy is to determine the temperature compensation of the ammonia-containing pure water medium and perform effective compensation.
Disclosure of Invention
Aiming at the problems in the background technology, the invention provides a method and a device for measuring the pH value of an ammonia-containing pure water medium by means of temperature compensation, wherein the standard pH value under the condition of 25 ℃ is calculated through the accurate measurement of the conductivity under the specific temperature condition of pure water, and then is compared with the actually measured pH value under the temperature, so that a nonlinear temperature compensation curve of the pH value under the ammonia-containing pure water medium condition is fitted, the pH compensation calibration in the measurement is realized, the measurement deviation of an instrument is greatly reduced, the measurement accuracy is improved, and the application is wide.
In order to achieve the purpose, the invention adopts the technical scheme that:
a pH temperature compensation measurement method for an ammonia-containing pure water medium comprises the following steps:
1) adding ammonia with different concentrations into the pure water to form ammonia-containing pure water, and adjusting the temperature of the ammonia-containing pure water to keep a constant value Tn;
2) measuring the conductivity of the ammonia-containing pure water at a constant temperature Tn, and calculating a standard pH value An (n is 1, 2, 3, … i, …) at 25 ℃ by a nonlinear temperature compensation model;
3) measuring the actual pH value Bn of the ammonia-containing pure water under a constant temperature Tn by using a pH meter;
4) collecting Tn, An and Bn data of the ammonia-containing pure water under different ammonia concentrations; for each group of data values, taking the temperature as an abscissa and the difference between the standard pH value and the actual pH value as an ordinate to obtain a temperature compensation fitting curve;
5) and (3) bringing temperature values t of ammonia-containing water samples with different concentrations into a fitting curve during measurement to obtain corresponding pH temperature compensation values, and performing compensation calibration on the measured values of the ammonia-containing water samples according to the pH table according to the temperature compensation values.
The process of the standard pH value An in the step 2) is,
2.1) measuring the conductivity value Kn (t) corresponding to the ammonia-containing pure water at the temperature Tn, and substituting the conductivity value Kn (t) into a nonlinear temperature compensation coefficient model formula to obtain a temperature compensation coefficient value sigma n of the ammonia-containing pure water;
2.2) substituting the temperature compensation coefficient value sigma n obtained in the step 2.1) into the following formula to obtain a conductivity value Kn (25) ═ Kn (t) x sigma n x (25-t) + Kn (t) at 25 ℃ of the ammonia-containing pure water;
2.3) substituting the conductivity value Kn (25) of the step 2.2) into the formula An of 8.57+ lg Kn (25) to obtain the standard pH value An of the ammonia-containing pure water at 25 ℃.
The temperature compensation coefficient model formula is as follows:
F(x，y)＝C+a1·x+a2·y+a3·xy+a4·x2+a5·y2+a6·x2 y+a7·xy2+a8·x3+a9·y3+a10·x3y+a11·x2y2+a12·xy3+al3·x4+a14·y4
wherein: f (x, y) represents a temperature compensation coefficient at the current temperature y; x represents conductivity, y represents temperature; c and a1 to a14 represent constants.
A measuring device for realizing the pH temperature compensation measuring method of an ammonia-containing pure water medium comprises a closed shell, a conductivity meter, a control unit, a temperature sensor and a pH meter; the closed shell is provided with a water inlet and a water outlet communicated with the water inlet; the water outlet is respectively communicated with the conductivity meter and the pH meter; the control unit is electrically connected with the conductivity meter and the temperature sensor respectively; the temperature sensor is arranged on a pipeline between the water outlet and the pH meter; a heat insulation sleeve is arranged outside the closed shell; and a dosing pipeline communicated with the water inlet is arranged on the water inlet.
The measuring device further comprises a heating device and a refrigerating device which are electrically connected with the closed shell.
The measuring device also comprises an EDI device connected with the water inlet; the dosing pipeline is located between the EDI device and the water inlet.
The measuring device further comprises a display unit; the display unit is electrically connected with the control unit and the pH meter respectively.
The beneficial effects of the invention are:
1. according to the invention, the standard conductivity and the standard pH value at 25 ℃ are obtained through the conductivity and temperature compensation model in the control unit, the actual pH value at the temperature is obtained through the pH meter, so that the standard value and the actual value are compared to obtain the ammonia-containing pure water with different concentrations and the pH temperature compensation values under different temperature conditions, a fitting temperature curve is drawn, and the measured values of the ammonia-containing water samples with different concentrations are compensated and calibrated through the pH meter in actual production according to the fitting temperature curve, so that the measurement precision is improved, and the measurement error is reduced.
2. According to the invention, a series of standard pH values and uncompensated actual pH values of the ammonia-containing pure water at different temperatures are obtained by changing the temperature value of the ammonia-containing pure water, and a temperature compensation curve of a temperature-pH difference value is drawn, so that the medium condition pH measurement value can be subjected to accurate nonlinear temperature compensation, the pH measurement accuracy is greatly improved, the deviation influence of the temperature on the pH measurement result is greatly reduced, and the accuracy of the measurement result and the safe operation of thermal equipment are ensured.
3. The pH temperature compensation measuring method and the device provided by the invention have the advantages of simple structure and simplicity and convenience in operation, and are suitable for detection of various ammonia-containing water qualities.
Drawings
FIG. 1 is a schematic view of a measuring device according to the present invention;
wherein:
1, sealing a shell; 2-a conductivity meter; 3-a control unit; 4-a temperature sensor; 5-pH meter; 6-a display unit; 7-EDI device; 8, a heat preservation sleeve.
Detailed Description
The present invention will now be described in detail with reference to the accompanying drawings and examples.
Example 1
Referring to fig. 1, the measurement device provided in this embodiment includes a sealed housing 1, a conductivity meter 2, a control unit 3, a temperature sensor 4, and a pH meter 5; the closed shell 1 is provided with a water inlet and a water outlet communicated with the water inlet; the water outlet is respectively communicated with the conductivity meter 2 and the pH meter 5; the control unit 3 is respectively electrically connected with the conductivity meter 2 and the temperature sensor 4; the temperature sensor 4 is arranged on a pipeline between the water outlet and the pH meter 5; the outside of the closed shell 1 is provided with a heat preservation sleeve 8.
The measuring device provided by the embodiment further comprises an EDI device 7 connected with the water inlet; and a dosing pipeline is also arranged between the EDI device 7 and the water inlet.
In this embodiment, the EDI device 7 is an existing device, and mainly functions to obtain ultrapure water, thereby ensuring that the obtained temperature compensation curve has high accuracy. Ammonia with different concentrations is added into the ultrapure water through a dosing pipeline.
The measuring device provided by the embodiment further comprises a heating device and a cooling device which are electrically connected with the closed shell 1. The heating device and the refrigerating device are temperature control equipment commonly used in the existing industrial production, and the main purpose is to heat or cool a water sample in the closed shell 1 to enable the water sample to be at a certain temperature value and keep the temperature constant through the heat insulation sleeve 8.
The measuring device provided by the embodiment further comprises a display unit 6; the display unit 6 is electrically connected to the control unit 3 and the pH meter 5, respectively. The display unit 6 can be a display screen or a computer display, and is mainly used for displaying detection data so as to be convenient for observation and monitoring.
In this embodiment, the conductivity meter 2 and the temperature sensor 4 are both commercially available conductivity detectors; the pH meter 5 is a commercially available product. During implementation, different types of pH instruments can be selected, and the device is adopted to carry out temperature compensation calibration on the measured value of the pH instrument.
In this embodiment, the sealed housing 1 is a cylindrical can made of 316L stainless steel. The outer wall is provided with a layer of heat insulation sleeve 7 for insulating the water sample in the closed shell 1 and keeping the temperature constant.
Example 2
The pH temperature compensation measuring method provided in this embodiment includes the following steps:
1) Adding ammonia with different concentrations into the pure water to form ammonia-containing pure water, and adjusting the temperature of the ammonia-containing pure water to keep a constant value Tn;
2) measuring the conductivity of the ammonia-containing pure water at a constant temperature Tn, and calculating a standard pH value An (n is 1, 2, 3, … i, …) at 25 ℃ by a nonlinear temperature compensation model;
3) measuring the actual pH value Bn of the ammonia-containing pure water under a constant temperature Tn by using a pH meter;
4) collecting Tn, An and Bn data of the ammonia-containing pure water under different ammonia concentrations; for each group of data values, taking the temperature as an abscissa and the difference between the standard pH value and the actual pH value as an ordinate to obtain a temperature compensation fitting curve;
5) and (3) bringing temperature values t of ammonia-containing water samples with different concentrations into a fitting curve during measurement to obtain corresponding pH temperature compensation values, and performing compensation calibration on the measured values of the ammonia-containing water samples according to the pH table according to the temperature compensation values.
In this embodiment, the process of calibrating the pH value An in step 2) is,
2.1) measuring the conductivity value Kn (t) corresponding to the ammonia-containing pure water at the temperature Tn, and substituting the conductivity value Kn (t) into a nonlinear temperature compensation coefficient model formula to obtain a temperature compensation coefficient value sigma n of the ammonia-containing pure water;
2.2) substituting the temperature compensation coefficient value sigma n obtained in the step 2.1) into the following formula to obtain the conductivity value Kn (25) ═ Kn (t) multiplied by sigma n x (25-t) + Kn (t) at 25 ℃ of the ammonia-containing pure water;
2.3) substituting the conductivity value Kn (25) of the step 2.2) into the formula An which is 8.57+ lg Kn (25) to obtain the standard pH value An of the ammonia-containing pure water at 25 ℃.
In this embodiment, the temperature compensation coefficient model formula is:
F(x，y)＝C+a1·x+a2·y+a3·xy+a4·x2+a5·y2+a6·x2y+a7·xy2+a8·x3+a9·y3+a10·x3y+a11·x2y2+a12·xy3+a13·x4+a14·y4
wherein: f (x, y) represents a temperature compensation coefficient at the current temperature y; x represents conductivity, y represents temperature; c and a1 to a14 represent constants.
Specifically, the measurement of pH temperature compensation of an ammonia-containing pure water medium having an ammonia concentration of 0.3mg/L is exemplified.
Firstly, a water sample generates ultrapure water after passing through an EDI device 7, and then ammonia is added into the ultrapure water through a dosing pipeline to obtain ammonia-containing pure water with the ammonia concentration of 0.3 mg/L;
secondly, ammonia-containing pure water enters the closed shell 1 through a water inlet, the temperature of the ammonia-containing pure water is controlled and adjusted to be constant at Tn through a heating device and a refrigerating device, and in the embodiment, n is 1-9;
further, 9 pieces of ammonia-containing pure water with different temperatures are discharged from the water outlet, each piece of ammonia-containing pure water enters the conductivity meter 2 and the pH meter 5 respectively, and the temperature of the outlet water T1-T9 of the ammonia-containing pure water is measured by the temperature sensor 4, wherein the temperature is 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃ and 45 ℃ in sequence.
In the conductivity meter 2, measuring the conductivity of the ammonia-containing pure water under a temperature constant value Tn, transmitting the conductivity value to the control unit 3, and obtaining a temperature compensation coefficient value sigma n of the ammonia-containing pure water by a nonlinear temperature compensation coefficient model formula built in the control unit 3; further substituting σ n into Kn (25) ═ Kn (t) × σ n × (25-t) + Kn (t) to obtain a conductivity value Kn (25) at 25 ℃ for ammonia-containing pure water; then, Kn (25) is substituted into the formula An of 8.57+ lg Kn (25) to obtain the standard pH value An of the ammonia-containing pure water at 25 ℃.
The actual pH value Bn of the ammonia-containing pure water at a constant temperature Tn is determined by a pH meter 5.
Finally, collecting the collected data, wherein Tn is T1-T9, and Tn is 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃ and 45 ℃ respectively; an is A1-A9, Bn is B1-B9; the ammonia-containing pure water at each temperature Tn corresponds to a standard pH value An and An actual pH value Bn at 25 ℃; the difference between the standard pH and the actual pH is obtained and recorded as the temperature compensation value, see table 1 for details.
TABLE 10.3 temperature compensation values of ammonia-containing pure water at different temperatures
Further, the temperature value is used as an abscissa, the temperature compensation value is used as an ordinate y, and then the curve is fitted to obtain a fitting curve equation of the temperature compensation, wherein y is 4 × 10-9T6-5×10-7T5+3×10-5T4-0.0007T3+0.0087T2-0.0128T-0.9101, linear degree of correlation R2＝0.9999。
Therefore, in actual production, when the pH meter 5 of this embodiment is used to measure the pH of ammonia-containing water with an ammonia concentration of 0.3mg/L, the pH measurement value is recorded as C, the temperature value t of the ammonia-containing water is measured at the same time, and t is substituted into the above-mentioned sextuple equation to find the corresponding temperature compensation value y, and according to the measurement value C-y, the pH value of the ammonia-containing water with a concentration of 0.3mg/L after temperature compensation is obtained, so as to implement compensation calibration of the measurement value of the ammonia-containing water sample by the pH meter 5, and ensure the accuracy of the measurement result.
Example 3
In contrast to example 2, the measurement of pH temperature compensation of an ammonia-containing pure water medium having an ammonia concentration of 2mg/L is described as an example; the temperature constant values Tn, n are 1-8, T1-T8 are 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃ and 45 ℃ respectively. The other measurement methods are the same as example 2, and the difference between the standard pH value and the actual pH value of the ammonia-containing pure water at the temperature of T1-T8 is obtained and recorded as a temperature compensation value, which is specifically shown in Table 2.
TABLE 22 temperature compensation values of ammonia-containing pure water at different temperatures
Further, the temperature value is used as an abscissa, the temperature compensation value is used as an ordinate y, and then the curve is fitted to obtain a temperature compensation fitting curve equation of which y is 2 × 10-8T6-3×10-6T5+0.0002T4-0.0058T3+0.109T2-1.0249T +3.0858, degree of linear correlation R2＝0.9999。
Therefore, in actual production, when the pH meter 5 of this embodiment is used to measure the pH of the ammonia-containing water with an ammonia concentration of 2mg/L, the pH measurement value is recorded as D, the temperature value t of the ammonia-containing water is measured at the same time, t is substituted into the above equation to obtain the corresponding temperature compensation value y, and the pH value of the 2mg/L ammonia-containing water subjected to temperature compensation is obtained according to the measurement value D-y, so that the compensation calibration of the pH meter 5 on the measurement value of the ammonia-containing water sample is realized, and the accuracy of the measurement result is ensured.
Meanwhile, by comparing the temperature compensation values in the table 1 and the table 2 at the same temperature, it is found that when the ammonia concentration in the ultrapure water is increased from 0.3mg/L to 2mg/L (by 7 times), the variation range of the corresponding temperature compensation value is small, for example, at 15 ℃, the temperature compensation value corresponding to 0.3mg/L is-0.40, the temperature compensation value corresponding to 2mg/L is-0.48, and the variation is 0.08 (less than 0.1) at the maximum; comparing the temperature compensation values under the same ammonia concentration, and finding that the change amplitude of the temperature compensation value is 0.11-0.24 (more than 0.1) when the temperature rises by 5 ℃; therefore, the pH measured values under different ammonia concentrations are compensated through a temperature compensation value curve so as to ensure accurate measurement results, and errors caused by temperature are greatly reduced, so that accurate data support is provided for industrial production.
Claims (7)
1. The method for measuring the pH temperature compensation of the ammonia-containing pure water medium is characterized by comprising the following steps of:
1) adding ammonia with different concentrations into the pure water to form ammonia-containing pure water, and adjusting the temperature of the ammonia-containing pure water to keep a constant value Tn;
2) measuring the conductivity of the ammonia-containing pure water at a constant temperature Tn, and calculating a standard pH value An (n is 1, 2, 3, … i, …) at 25 ℃ by a nonlinear temperature compensation model;
3) Measuring the actual pH value Bn of the ammonia-containing pure water under a constant temperature Tn by using a pH meter;
4) collecting Tn, An and Bn data of the ammonia-containing pure water under different ammonia concentrations; for each group of data values, the temperature is taken as an abscissa, and the difference between the standard pH value and the actual pH value is taken as an ordinate, so as to obtain a temperature compensation fitting curve;
5) and (3) bringing the temperature values t of the ammonia-containing water samples with different concentrations into a fitting curve during measurement to obtain corresponding pH temperature compensation values, and performing compensation calibration on the measured values of the ammonia-containing water samples according to the pH table by using the temperature compensation values.
2. The pH temperature compensation measurement method of ammonia-containing pure water medium according to claim 1, characterized in that the standard pH value An in the step 2) is,
2.1) measuring the conductivity value Kn (t) corresponding to the ammonia-containing pure water at the temperature Tn, and substituting the conductivity value Kn (t) into a nonlinear temperature compensation coefficient model formula to obtain a temperature compensation coefficient value sigma n of the ammonia-containing pure water;
2.2) substituting the temperature compensation coefficient value sigma n obtained in the step 2.1) into the following formula to obtain a conductivity value Kn (25) ═ Kn (t) x sigma n x (25-t) + Kn (t) at 25 ℃ of the ammonia-containing pure water;
2.3) substituting the conductivity value Kn (25) of the step 2.2) into the formula An of 8.57+ lg Kn (25) to obtain the standard pH value An of the ammonia-containing pure water at 25 ℃.
3. The method for measuring the pH temperature compensation of the ammonia-containing pure water medium according to claim 2, wherein the temperature compensation coefficient model formula is as follows:
F(x，y)＝C+a1·x+a2·y+a3·xy+a4·x2+a5·j2+a6·x2y+a7·xy2+a8·x3+a9·y3+a10·x3y+a11·x2y2+a12·xy3+a13·x4+a14·y4
wherein: f (x, y) represents a temperature compensation coefficient at the current temperature y; x represents conductivity, y represents temperature; c and a1 to a14 represent constants.
4. A measuring device for realizing the pH temperature compensation measuring method of the ammonia-containing pure water medium according to claim 3, wherein the measuring device comprises a closed shell (1), a conductivity meter (2), a control unit (3), a temperature sensor (4) and a pH meter (5); the closed shell (1) is provided with a water inlet and a water outlet communicated with the water inlet; the water outlet is respectively communicated with the conductivity meter (2) and the pH meter (5); the control unit (3) is electrically connected with the conductivity meter (2) and the temperature sensor (4) respectively; the temperature sensor (4) is arranged on a pipeline between the water outlet and the pH meter (5); a heat insulation sleeve (8) is arranged outside the closed shell (1); and a dosing pipeline communicated with the water inlet is arranged on the water inlet.
5. A measuring device as claimed in claim 4, characterized in that the measuring device further comprises heating means and cooling means electrically connected to the closed housing (1).
6. A measuring device as claimed in claim 5, characterized in that the measuring device further comprises an EDI device (7) connected to the water inlet; the dosing pipeline is positioned between the EDI device (7) and the water inlet.
7. The measuring device according to claim 6, characterized in that it further comprises a display unit (6); the display unit (6) is electrically connected with the control unit (3) and the pH meter (5) respectively.
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