CN111735906A - Method for determining alkalinity of water sample and analysis system - Google Patents
Method for determining alkalinity of water sample and analysis system Download PDFInfo
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Abstract
The invention relates to a method for determining alkalinity of a water sample and an analysis system. The method comprises the steps of obtaining the voltage E corresponding to the solution with the pH value of 8.3 +/-0.051Standard voltage E corresponding to standard solution with pH value between 8.3 +/-0.05 and 4.5 +/-0.050And the voltage E corresponding to the solution with the pH value of 4.5 +/-0.052To obtain △ E1And △ E2(ii) a Dripping an acid standard solution into a water sample, and recording the voltage value and the volume of the acid standard solution to form a curve graph; real-time voltage E corresponding to binding standard solutionm、△E1And △ E2And finding the volume of the acid standard solution corresponding to the phenolphthalein alkalinity or the total alkalinity to obtain the phenolphthalein alkalinity and/or the total alkalinity. The method can obtain the phenolphthalein alkalinity and/or the total alkalinity of the water sample at one time. The invention also comprises an analysis system which comprises a sample introduction mechanism, a data processing mechanism and a detection mechanism.
Description
Technical Field
The invention relates to the field of alkalinity determination, in particular to a method and an analysis system for determining the alkalinity of a water sample.
Background
Alkalinity refers to the amount of hydrogen ion accepting species in the water, e.g., OH-、CO3 2-、HCO3 -Silicate, phosphate, hydrogen phosphate, sulfite, ammonia and the like, which are common alkaline substances in boiler water, so that the determination of the total alkalinity of the boiler water is an important item for monitoring the boiler water quality.
In most cases, the measurement of the total alkalinity of boiler water is mostly carried out by the conventional indicator titration method. The indicator titration method is characterized in that sulfuric acid is generally used as a standard solution when the total alkalinity of boiler water is measured, methyl orange and phenolphthalein indicators are used as auxiliaries, the titration end point is judged by judging the color change of a mixed solution in the titration process according to the principle of acid-base neutralization, and then the total alkalinity of the boiler water is calculated according to the volume of the consumed standard acid solution. Although these conventional manual measurement methods are relatively low in cost and simple in analysis principle, most of them require that boiler water sample is continuously removed for chemical quantitative analysis. The operations are complex and time-consuming, some artificial errors are more easily introduced in the links of titration end point judgment and the like, and the on-line real-time detection of the total alkalinity of the boiler water cannot be realized. Therefore, the total alkalinity on-line detection system has important significance for ensuring the safe operation of the boiler and improving the heat efficiency.
The existing alkalinity detection technology is mainly divided into two major types, namely colorimetric (optical) titration method and potentiometric titration method, such as British Jeep: PACON 5500 on-line total alkalinity analyzer (optical titration).
No matter which principle is adopted by an alkalinity analyzer on the market at present, only one parameter (mainly total alkalinity) can be obtained by one-time test, and full-automatic online water quality analysis capable of simultaneously testing two parameters of phenolphthalein alkalinity and total alkalinity of the same water sample does not exist. And the titration colorimetry is greatly interfered by the chromaticity and the turbidity of a water sample and is only suitable for cleaning water bodies.
Disclosure of Invention
The invention adopts a dynamic potential calibration algorithm to overcome the drift of the electrode caused by the influence of the environmental temperature and the like, the whole reaction and titration are carried out in a constant temperature environment, and the concentration of the sample can be accurately and rapidly calculated by combining a dynamic baseline algorithm. Meanwhile, in design, the instrument can simultaneously determine the phenolphthalein alkalinity and the total alkalinity, and the phenolphthalein alkalinity and the total alkalinity results of the current water sample can be given after single measurement is finished.
The technical problem to be solved by the invention is as follows: how to accurately obtain the phenolphthalein alkalinity and the total alkalinity of a sample at one time.
In order to solve the technical problems, the invention provides a method and an analysis system for measuring the alkalinity of a water sample.
A method for determining alkalinity of a water sample, comprising the steps of:
s1, obtaining the voltage E corresponding to the solution with the pH value of 8.3 +/-0.051Standard voltage E corresponding to standard solution with pH value between 8.3 +/-0.05 and 4.5 +/-0.050And the voltage E corresponding to the solution with the pH value of 4.5 +/-0.052To obtain E1And E0Voltage difference △ E1，E2And E0Voltage difference △ E2；
S2, dropwise adding an acid standard solution into a water sample, recording a voltage value and the volume of the dropwise added acid standard solution in real time, and forming a curve graph in a two-dimensional coordinate system;
s3, real-time voltage E corresponding to the standard solution with the pH value between 8.3 +/-0.05 and 4.5 +/-0.05mThe △ E1And said △ E2And finding the volume of the acid standard solution corresponding to the phenolphthalein alkalinity or the total alkalinity in the graph, and obtaining the phenolphthalein alkalinity and/or the total alkalinity of the water sample according to the volume of the acid standard solution.
Further, the acid standard solution is dripped into the water sample in the step S2 and the real-time voltage E in the step S3mThe measurements of (a) were performed at the same constant temperature.
Still further, the constant temperature is 15 ℃ to 60 ℃.
Further, the real-time voltage E is measured before or after step S2m。
The invention also provides an analysis system, which comprises a sample introduction mechanism, a data processing mechanism and a detection mechanism;
the sample introduction mechanism is connected with the detection mechanism and is used for inputting a water sample, a standard solution and an acid standard solution to the detection mechanism;
the detection mechanism is connected with the data processing mechanism and is used for detecting the real-time voltage E of the water sample and the standard solutionmAnd the corresponding volume of the acid standard solution dropped and transmitting the data to the data processing mechanism;
the sample injection mechanism is connected with the data processing mechanism and is used for recording the volume of the acid standard solution and transmitting the volume to the data processing mechanism;
the data processing mechanism stores E1And E0Voltage difference △ E1，E2And E0Voltage difference △ E2(ii) a Wherein E is1The voltage corresponding to the solution with the pH value of 8.3 +/-0.05; e0The voltage value corresponding to the standard solution with the pH value between 8.3 +/-0.05 and 4.5 +/-0.05; voltage E2The voltage value corresponding to the solution with the pH value of 4.5 +/-0.05;
the data processing mechanism is used for combining the △ E1And said △ E2And receiving the data to obtain the phenolphthalein alkalinity and/or the total alkalinity of the water sample.
Preferably, the sampling device further comprises a flow path switching valve and at least two sampling mechanisms, wherein the flow path switching valve is connected with the at least two sampling mechanisms and the detection mechanism, and is used for switching different sampling mechanisms to be connected with the detection mechanism; and the at least two sample feeding mechanisms are used for inputting the water sample, the standard solution and the acid standard solution to the detection mechanism from different sample feeding mechanisms.
Preferably, the detection mechanism comprises a detection cell, a potential probe and a potential conversion module; the detection pool is used for bearing the water sample or the standard solution; the potential probe is used for detecting analog signals of a water sample or a standard solution in the detection pool; and the potential conversion module converts the analog signal into a voltage value and transmits the voltage value to the data processing mechanism.
Preferably, the sample feeding mechanism comprises a plunger pump and a quantitative tube; the plunger pump is connected with the quantitative pipe, and the quantitative pipe is connected with the detection mechanism.
Compared with the prior art, the invention has the advantages that: obtaining the voltage E corresponding to the solution with the pH value of 8.3 +/-0.051Standard voltage E corresponding to standard solution with pH value between 8.3 +/-0.05 and 4.5 +/-0.050And the voltage E corresponding to the solution with the pH value of 4.5 +/-0.052To obtain E1And E0Voltage difference △ E1，E2And E0Voltage difference △ E2(ii) a Dripping acid standard solution into a water sample, recording a voltage value and the volume of the dripped acid standard solution in real time, and forming a curve graph in a two-dimensional coordinate system; the curve chart reflects the volume relation between the voltage value of the sample to be measured and the acid standard solution; combining the real-time voltage E corresponding to the standard solution with the pH value between 8.3 +/-0.05 and 4.5 +/-0.05mThe △ E1And said △ E2Finding the real-time voltage E in said graphmAnd △ E bond1And △ E2At a constant value, real-time voltage EmInstead of the standard voltage E0A 1 is mixing EmAnd △ E2Adding to find the volume of the acid standard solution corresponding to the voltage value of the total alkalinity from the curve, and adding EmAnd △ E1Subtracting the voltage value of the phenolphthalein alkalinity to find the volume of the acid standard solution corresponding to the voltage value of the phenolphthalein alkalinity from the curve, and obtaining the phenolphthalein alkalinity and/or the total alkalinity of the water sample at one time according to the volume of the acid standard solution.
The invention also provides an analysis system, wherein the sample introduction mechanism is used for inputting a water sample, a standard solution and an acid standard solution to the detection mechanism; the sample introduction mechanism inputs a standard solution to the detection mechanism, the detection mechanism acquires a real-time voltage value of the standard solution, the sample introduction mechanism inputs a water sample to the detection mechanism, the sample introduction mechanism slowly inputs an acid standard solution to the detection mechanism, the data processing mechanism records the volume of the input acid standard solution and a corresponding voltage value detected by the detection mechanism, and the volume and the corresponding voltage value are drawn into a curve graph; the volume of the acid standard solution corresponding to the phenolphthalein alkalinity and the total alkalinity can be obtained on the graph, and the phenolphthalein alkalinity and/or the total alkalinity of the water sample can be obtained through the volume of the acid standard solution.
Drawings
The features and advantages of the present invention will be more clearly understood by reference to the accompanying drawings, which are illustrative and not to be construed as limiting the invention in any way, and in which:
FIG. 1 is a graph showing the voltage value of a water sample and the volume of a corresponding dropwise added acid standard solution in the method for determining the alkalinity of the water sample.
Fig. 2 is a schematic structural diagram of an analysis system according to the present invention.
Fig. 3 is a standard graph of the volume of the acid standard solution and the total alkalinity of the seawater sample in example 1 of the present invention.
Description of reference numerals: 1-a sample introduction mechanism; 11-a plunger pump; 12-a dosing tube; 2-flow path switching valve; 3-a potential detecting means; 4-detection pool.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The specific embodiment provides a method for determining the alkalinity of a water sample, which comprises the following steps:
s1, obtaining the voltage E corresponding to the solution with the pH value of 8.3 +/-0.051Standard voltage E corresponding to standard solution with pH value between 8.3 +/-0.05 and 4.5 +/-0.050And the voltage E corresponding to the solution with the pH value of 4.5 +/-0.052To obtain E1And E0Voltage difference △ E1，E2And E0Voltage difference △ E2；
S2, dripping an acid standard solution into a water sample, recording a voltage value and the volume of the dripped acid standard solution in real time, and forming a curve graph shown in figure 1 in a two-dimensional coordinate system; in order to more intuitively react the concentration relation between the volume of the acid standard solution and the phenolphthalein alkalinity or the total alkalinity, a curve graph can be converted into a standard curve graph between the volume of the acid standard solution and the concentration of the phenolphthalein alkalinity or the total alkalinity; the voltage value is obtained by a nernst equation, which is described below, and will not be described repeatedly.
S3, real-time voltage E corresponding to the standard solution with the pH value between 8.3 +/-0.05 and 4.5 +/-0.05mThe △ E1And said △ E2And finding the volume of the acid standard solution corresponding to the phenolphthalein alkalinity or the total alkalinity in the graph, and obtaining the phenolphthalein alkalinity and/or the total alkalinity of the water sample according to the volume of the acid standard solution.
In the present embodiment, the dropping of the acid standard solution into the water sample in step S2 is performed at the same constant temperature as the measurement of the real-time voltage Em in step S3; further, the constant temperature is 15 ℃ to 60 ℃.
In this embodiment, the real-time voltage E is measured before or after step S2m。
It should be noted that, only one of phenolphthalein alkalinity and total alkalinity in the water sample can be measured according to the above method.
It is further noted that alkalinity is the quantitative ability of an aqueous medium to react with hydroxide, and is quantitatively determined by titrating a volume of a water sample to a certain pH with an acid standard solution. The measurement results were expressed in mg/L as the content of calcium carbonate. There are two indications of alkalinity, one is phenolphthalein alkalinity (complex alkalinity), one is total alkalinity, and the end points of both have a large difference in pH. In the acid titration process, when the pH value of a sample is titrated to 8.3 +/-0.05, the default titration acid volume corresponds to the consumption of the alkalinity of the phenolphthalein; when the solution pH is titrated to 4.5 ± 0.05, the default is that the volume of acid consumed at this time corresponds to the total alkalinity.
The voltage value is obtained according to the nernst equation:
Eindto measure the voltage value;
E0the voltage value of the standard solution is shown;
r, T, F is an ambient temperature parameter (R-gas constant 8.3143J/(K. mol)
T-Absolute temperature K
F-Faraday constant
) Can be searched according to the corresponding table.
When the pH is known, the corresponding voltage value E can be determined according to the formula. The total base and phenolphthalein basicity are defined according to standard procedures.
Defining: titrating alkali in an unknown sample by using a standard acid solution, wherein when the pH value of the solution is 8.3, the corresponding titration volume is the consumed acid volume of phenolphthalein alkalinity (composite alkalinity); and (4) continuing titration, wherein when the pH value is 4.4-4.5, the volume of the consumed acid is the total alkalinity.
According to the definition of the pH value and the pH value, the voltage value (phenolphthalein alkalinity and total alkalinity voltage value) can be calculated by the known pH value.
Similarly, the pH value corresponding to the alkalinity of phenolphthalein and the total alkalinity is a definite known value, therefore △ E1And △ E2Is a fixed and constant value.
With reference to fig. 2, the present embodiment further provides an analysis system using the above method, which includes a sample injection mechanism 1, a data processing mechanism and a detection mechanism;
the sample feeding mechanism 1 is connected with the detection mechanism, and the sample feeding mechanism 1 is used for conveying a water sample, a standard solution and an acid standard solution to the detection mechanism;
the detection mechanism is connected with the data processing mechanism and is used for detecting the real-time voltage Em of the water sample and the standard solution and the volume of the corresponding dripped acid standard solution and transmitting data to the data processing mechanism;
the sample introduction mechanism 1 is connected with the data processing mechanism, and the sample introduction mechanism 1 is used for recording the volume of the acid standard solution and transmitting the volume to the data processing mechanism;
the data processing mechanism stores E1And E0Voltage difference △ E1，E2And E0Voltage difference △ E2(ii) a Wherein E is1The voltage corresponding to the solution with the pH value of 8.3 +/-0.05; e0The voltage value corresponding to the standard solution with the pH value between 8.3 +/-0.05 and 4.5 +/-0.05; voltage E2The voltage value corresponding to the solution with the pH value of 4.5 +/-0.05;
the data processing mechanism is used for combining the △ E1And said △ E2And receiving the data to obtain the phenolphthalein alkalinity and/or the total alkalinity of the water sample.
In this embodiment, the analysis system further includes a flow path switching valve 2 and at least two sampling mechanisms 1, the flow path switching valve 2 is connected to the at least two sampling mechanisms 1 and the detection mechanism, and the flow path switching valve 2 is used for switching different sampling mechanisms 1 to connect to the detection mechanism; the sample feeding mechanisms 1 are used for inputting the water sample, the standard solution and the acid standard solution from different sample feeding mechanisms to the detection mechanism. The solution is input through a plurality of sampling mechanisms, so that the speed of detecting different samples is accelerated, and the cross contamination is avoided. The sample injection mechanism can obtain phenolphthalein alkalinity and/or total alkalinity step by step through one-time sample injection.
In the present embodiment, the detection mechanism includes a detection cell 4 and a potential detection unit 3; the detection pool 3 is used for bearing the water sample or the standard solution; the potential detection component 3 comprises a potential probe and a potential conversion module, the potential probe is connected with the potential conversion module, and the potential probe is used for detecting analog signals of a water sample or a standard solution in the detection pool; and the potential conversion module converts the analog signal into a voltage value and transmits the voltage value to the data processing mechanism.
In this embodiment, the sample injection mechanism 1 includes a plunger pump 11 and a quantitative tube 12; the plunger pump 11 is connected with the quantitative pipe 12, and the quantitative pipe 12 is connected with the detection mechanism; the plunger pump is used for injecting the solution into the quantitative tube for accurate quantification and then sending the solution into the detection mechanism; in a more preferred embodiment, the plunger pump 11 is connected to the fixed amount tube 12, the fixed amount tube 12 is connected to the flow path switching valve 2, the flow path switching valve 2 is connected to the detection means, and different solutions are input to the detection means through the flow path switching valve.
To further illustrate the method for determining the alkalinity of a water sample according to this embodiment, the following examples are given by way of illustration. In the following examples, the standard graph has been obtained by steps S1 and S2 in the method of the present embodiment. In the following examples, 6000 drops were 1 mL.
Example 1
The total alkalinity of the seawater sample was measured, and the volume of the titrant corresponding to the voltage difference between the total alkalinity and the standard solution was 9000 drops (6000 drops to 1 mL).
And (3) extracting 15mL of the standard solution to the detection cell, obtaining a standard voltage value, finding out the volume of the corresponding titrant (acid standard solution) from the curve chart according to the standard voltage value to be 33238 drops, recording, and cleaning the detection cell. And (3) pumping 15ml of seawater sample into a potential detection pool, starting stirring, dropwise adding the titrant, and recording the number of consumed drops of the titrant at the moment as 17248 when the dropping volume of the titrant reaches 24238 drops.
The titration result 17248 is dropped into the standard curve shown in FIG. 3, and the total alkalinity of the seawater sample is calculated to be 281.4 mg/L.
Example 2
Measuring the phenolphthalein alkalinity of the standard solution, wherein the volume of a titrant corresponding to the potential difference of the standard solution and the phenolphthalein alkalinity is 5000 drops, and the concentration of the standard solution is 50.0 mg/L;
and (3) extracting 15mL of the standard solution to a detection cell, obtaining a standard voltage value, finding out the corresponding volume of the titrant 32338 drops from the graph according to the standard voltage value, recording, and cleaning the detection cell. 15ml of the standard sample is taken into a potential detection pool, stirring is started, the titrant is added dropwise, and when the volume of the titrant reaches 27338 drops, the number of consumed drops of the titrant at the moment is recorded as 6881 drops.
Substituting the titration result 6881 into the standard curve to calculate the phenolphthalein alkalinity of the standard sample to be 52.6 mg/L.
Example 3
Phenolphthalein alkalinity and total alkalinity measurements: actual samples of a river.
And (3) extracting 15mL of the standard solution to the detection cell, acquiring a standard voltage value, finding out the corresponding volume of 33738 drops of the titrant from the graph according to the standard voltage value, recording, and cleaning the detection cell. Extracting 15ml of an actual sample into a potential detection pool, starting stirring, reading and dropwise adding a titrant, and recording the number of drops consumed by the titrant at the moment as 4201 when the volume difference corresponding to the voltage difference value between the sample and a standard solution reaches 5000 drops, namely the volume of the titrant corresponding to the voltage value of the sample reaches 28738 drops, wherein the titration volume corresponding to the titrant at the moment is the phenolphthalein alkalinity; and continuously dropwise adding the titrant, and recording the number of drops consumed by the titrant at the moment when the volume difference corresponding to the voltage difference value between the sample and the standard solution reaches 9000 drops, namely the volume of the titrant corresponding to the voltage value of the product reaches 24738 drops, wherein the corresponding titration volume is the total alkalinity.
And substituting the titration result into a standard curve, and calculating the alkalinity of phenolphthalein in the actual sample to be 5.5mg/L and the total alkalinity to be 105.2 mg/L.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
Claims (8)
1. A method for measuring the alkalinity of a water sample is characterized by comprising the following steps:
s1, obtaining the voltage E corresponding to the solution with the pH value of 8.3 +/-0.051Standard voltage E corresponding to standard solution with pH value between 8.3 +/-0.05 and 4.5 +/-0.050And the voltage E corresponding to the solution with the pH value of 4.5 +/-0.052To obtain E1And E0Voltage difference △ E1，E2And E0Voltage difference △ E2；
S2, dripping an acid standard solution into a water sample, recording a voltage value and the volume of the dripped acid standard solution in real time, and forming a curve graph in a two-dimensional coordinate system;
s3, real-time voltage E corresponding to the standard solution with the pH value between 8.3 +/-0.05 and 4.5 +/-0.05mThe △ E1And said △ E2And finding the volume of the acid standard solution corresponding to the phenolphthalein alkalinity or the total alkalinity in the graph, and obtaining the phenolphthalein alkalinity and/or the total alkalinity of the water sample according to the volume of the acid standard solution.
2. The method of claim 1, wherein the dropping of the acid standard solution into the water sample in step S2 is different from the real-time voltage E in step S3mThe measurements of (a) were performed at the same constant temperature.
3. The method according to claim 2, wherein the constant temperature is 15 ℃ to 60 ℃.
4. The method of claim 1, wherein the real-time voltage E is measured before or after step S2m。
5. An analysis system is characterized by comprising a sample introduction mechanism, a data processing mechanism and a detection mechanism;
the sample feeding mechanism is connected with the detection mechanism and is used for inputting a sample, a standard solution and an acid standard solution to the detection mechanism;
the detection mechanism is connected with the data processing mechanism and is used for detecting the real-time voltage E of the water sample and the standard solutionmAnd the corresponding volume of the acid standard solution dropped and transmits the data to the data processorStructuring;
the sample injection mechanism is connected with the data processing mechanism and is used for recording the volume of the acid standard solution and transmitting the volume to the data processing mechanism;
the data processing mechanism stores E1And E0Voltage difference △ E1，E2And E0Voltage difference △ E2(ii) a Wherein E is1The voltage corresponding to the solution with the pH value of 8.3 +/-0.05; e0The voltage value corresponding to the standard solution with the pH value between 8.3 +/-0.05 and 4.5 +/-0.05; voltage E2The voltage value corresponding to the solution with the pH value of 4.5 +/-0.05;
the data processing mechanism is used for combining the △ E1And said △ E2And receiving the data to obtain the phenolphthalein alkalinity and/or the total alkalinity of the water sample.
6. The analytical system of claim 5, further comprising a flow path switching valve and at least two sample injection mechanisms, wherein the flow path switching valve is connected to the at least two sample injection mechanisms and the detection mechanism, and the flow path switching valve is used for switching different sample injection mechanisms to be connected to the detection mechanism; and the at least two sample feeding mechanisms are used for inputting the water sample, the standard solution and the acid standard solution to the detection mechanism from different sample feeding mechanisms.
7. The analytical system of claim 5, wherein the detection mechanism comprises a detection cell and a potential detection component; the detection pool is used for bearing the water sample or the standard solution; the potential detection component comprises a potential probe and a potential conversion module, the potential probe is connected with the potential conversion module, and the potential probe is used for detecting analog signals of a water sample or a standard solution in the detection pool; and the potential conversion module converts the analog signal into a voltage value and transmits the voltage value to the data processing mechanism.
8. The analytical system of claim 5, wherein the sample introduction mechanism comprises a plunger pump and a dosing tube; the plunger pump is connected with the quantitative pipe, and the quantitative pipe is connected with the detection mechanism.
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| CN113777219A (en) * | 2021-08-12 | 2021-12-10 | 北京华科仪科技股份有限公司 | Water sample alkalinity measuring device and method |
| WO2023010806A1 (en) * | 2021-08-03 | 2023-02-09 | 佛山市云米电器科技有限公司 | Method for measuring alkalinity of water sample |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023010806A1 (en) * | 2021-08-03 | 2023-02-09 | 佛山市云米电器科技有限公司 | Method for measuring alkalinity of water sample |
| CN113777219A (en) * | 2021-08-12 | 2021-12-10 | 北京华科仪科技股份有限公司 | Water sample alkalinity measuring device and method |
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