阅读说明：本技术 一种多维滴定分析的信号采集方法 (Signal acquisition method for multidimensional titration analysis ) 是由 王宇曦 高飞 钟亚莉 王飞 田丰 张昂 李婧奕 郭禹 于 2019-08-29 设计创作，主要内容包括：本发明公开了一种多维滴定分析的信号采集方法,该方法通过设置由有效采集期和闲置期组成的信号采集周期、由信号采集周期和间隔期组成的测量周期将不同的测量参数的信号采集周期及测量周期相统一,实现了相同测量基质不同测量参数的同步测定,从而使相同测量基质的多维滴定分析成为可能；通过所述间隔期长度的设定,灵活调整多维滴定分析信号采集频率,实现了滴定信号突变区域的高频率采集和滴定信号平缓区域的低频率监控；通过测量序列与测量参数信号采集点的准确对应,为反应溶液中物质结构的变化与计量的研究提供丰富的信息；并通过不同测量参数对相同测量基质的同步多维滴定分析,减少了实验次数,提高工作效率。(The invention discloses a signal acquisition method for multidimensional titration analysis, which unifies signal acquisition periods and measurement periods of different measurement parameters by setting a signal acquisition period consisting of an effective acquisition period and an idle period and a measurement period consisting of a signal acquisition period and an interval period, thereby realizing synchronous measurement of different measurement parameters of the same measurement substrate and enabling multidimensional titration analysis of the same measurement substrate to be possible; the acquisition frequency of the multidimensional titration analysis signal is flexibly adjusted by setting the length of the interval period, so that the high-frequency acquisition of a titration signal mutation area and the low-frequency monitoring of a titration signal gentle area are realized; through the accurate correspondence of the measurement sequence and the measurement parameter signal acquisition point, abundant information is provided for the research of the change and the measurement of the material structure in the reaction solution; and synchronous multidimensional titration analysis is carried out on the same measurement matrix through different measurement parameters, so that the experiment times are reduced, and the working efficiency is improved.)

1. A signal acquisition method of multidimensional titration analysis is characterized in that a multidimensional titration analysis signal acquisition system is controlled to obtain at least one measurement period which takes a measurement sequence as a reference;

the measurement period comprises a signal acquisition period and an interval period, and signal acquisition is carried out once for each measurement parameter in the signal acquisition period;

the signal acquisition period comprises an effective acquisition period and an idle period of at least one measurement parameter;

the effective acquisition period is the length of a measurement sequence from an acquisition starting point to an effective signal acquisition finishing point, and the idle period is the length of the measurement sequence from the effective signal acquisition finishing point to an acquisition finishing point;

the interval period is more than or equal to 0 measurement sequence length.

2. The method of claim 1, wherein the measurement sequence comprises one or more of time T, pulse signal f, volume of reagent added V, concentration of substance in the reaction solution C, pH of the reaction solution, spectral titration parameter S, potentiometric titration parameter E, and temperature titration parameter T.

3. The method of claim 1, wherein the measurement parameters include one or more of volume of reagent added V, concentration of substance in reaction solution C, pH of reaction solution, spectral titration parameter S, potentiometric titration parameter E, and temperature titration parameter T.

4. The method of claim 3, wherein the signal collection period comprises valid collection periods and idle periods of a plurality of measurement parameters, the collection start points of the plurality of measurement parameters are unified with the signal collection period start point, the collection end points of the plurality of measurement parameters are unified with the signal collection period end point, and the valid signal collection completion points of the plurality of measurement parameters are independent from each other.

5. The method of claim 1, wherein the interval period is 0 measurement sequences in length, and the signal is acquired continuously.

6. The method of claim 1, wherein the interval period is at least 1 measurement sequence length, the interval periods of the plurality of measurement cycles are the same, and the signal is acquired at intervals.

7. The method of claim 1, wherein the interval period is greater than or equal to 0 measurement sequence lengths, the number of measurement sequence lengths in the interval periods of the measurement periods is independent according to user definition, and the signal acquisition mode is user-defined acquisition.

Technical Field

The invention belongs to the technical field of measurement, particularly relates to the technical field of analytical chemistry, and more particularly relates to a signal acquisition method for multidimensional titration analysis.

Background

In titration chemical analysis, the structural change and the measurement of a substance in a reaction solution are extremely important basic tasks in chemical analysis. Different measurement methods are adopted to obtain different measurement data aiming at the same measurement target, and through comparison between the data, analysis of different physical quantities can be provided for the change process of a substance structure in a chemical reaction, so that the method is a widely applied and important link in chemical analysis.

Currently, there are three main types of titrimetric techniques for chemical reactions, namely potentiometric titration, temperature titration, and spectroscopic titration. As an ideal titration analysis processing strategy, it has been desired by those skilled in the art to comprehensively use three different titration methods and provide measurement data of different angles for the same chemical reaction process, thereby implementing multidimensional characterization of temperature, spectrum and electrochemistry in the same chemical reaction process. However, the measurement principle and the measurement elements of different titration modes are different, and the period and the frequency of the acquired signal are different, so that for synchronous multidimensional titration of the same measurement matrix, the respective signal acquisition periods of the titration modes in which separate titrations are still adopted are obviously not suitable.

Furthermore, the existing titrimetric methods mostly use time or pulse signals as a single measurement sequence. When the measurement data is calculated and analyzed, the mapping relation between the substance structure change and the metering parameter in the target chemical reaction can be constructed only by taking the time or the pulse signal as an independent variable and the titration parameter as a dependent variable. This greatly limits the understanding of the relationship between the structural change and the measurement of the substance in the chemical reaction, and also influences the research on the mechanism of the chemical reaction process.

In order to meet the research requirements on material structure change and metering in a target chemical reaction, the prior art performs derivative calculation on collected original measurement data, for example, a value of a volume V of an added reagent is calculated by taking a pulse signal f as an independent variable, a value of a material concentration C of a reaction solution is calculated by taking the volume V of the added reagent as the independent variable, and a pH value of a reaction system is calculated by taking the value of the material concentration C of the reaction solution as the independent variable. However, calculation errors due to multiple calculations are inevitable.

In this case, an effective solution strategy is to directly use parameters such as the volume V of the added reagent, the substance concentration C of the reaction solution, and the pH of the reaction system, which can be obtained by detection, as a measurement sequence for titration analysis, and replace a calculated value with a measured value for titration measurement to avoid calculation errors. However, the measurement methods, principles and elements of different measurement parameters are different, and the periods and frequencies of the acquired signals are also different, so how to realize the synchronous detection of the measurement sequence and the titration parameters on the same substrate becomes a problem which needs to be considered by researchers.

Therefore, it is an urgent need for those skilled in the art to develop a multi-dimensional titration analysis signal collection method based on multiple measurement sequences and titration parameters and capable of implementing undifferentiated comparison analysis.

Disclosure of Invention

In view of the above, the present invention provides a method for collecting signals of multidimensional titration analysis, which is used to obtain synchronous detection signals of different measurement sequences and multiple measurement parameters for the same detection matrix.

In order to achieve the purpose, the invention adopts the following technical scheme:

a multidimensional titration analysis signal acquisition method, control multidimensional titration analysis signal acquisition system in order to obtain at least one and measure the cycle taking sequence of measurement as the benchmark;

the measurement period comprises a signal acquisition period and an interval period, and signal acquisition is carried out once for each measurement parameter in the signal acquisition period;

the signal acquisition period comprises an effective acquisition period and an idle period of at least one measurement parameter;

the effective acquisition period is the length of a measurement sequence from an acquisition starting point to an effective signal acquisition finishing point, and the idle period is the length of the measurement sequence from the effective signal acquisition finishing point to an acquisition finishing point;

the interval period is more than or equal to 0 measurement sequence length.

It is worth to be noted that, considering that the measurement methods, principles and elements of different measurement parameters are different and the periods and frequencies of the collected signals are also different, the invention unifies the signal collection periods of different measurement parameters by setting the idle period, so that different measurement parameters have the same signal collection period in the same measurement period, and simultaneously, different measurement elements are restored to the initial state by setting the idle period, so as to prepare for the next signal collection. In addition, in consideration of the complexity of the multidimensional titration analysis measuring element in actual use, the idle period can also provide certain fault-tolerant time for the recovery of the measuring element so as to avoid signal acquisition failure caused by different states of the measuring instrument.

Meanwhile, in consideration of huge data volume of titration analysis and actual titration measurement conditions, the invention assigns the signal acquisition frequency of multidimensional titration analysis according to the interval period length value set by a user, reduces the titration data volume, improves the data processing speed of multidimensional titration analysis, avoids the acquisition of invalid signals, reduces background noise, and improves the detection limit and analysis precision.

Preferably, the measurement sequence comprises one or more of time T, pulse signal f, volume of reagent added V, substance concentration C of the reaction solution, pH value of the reaction solution, spectral titration parameter S, potentiometric titration parameter E and temperature titration parameter T.

It should be noted that, in a general titration analysis test, the time t or the pulse signal f is mostly used as a measurement sequence to obtain an acquired signal, and based on this, both the processing and analysis of titration data use the time t, the pulse signal f or a calculation derivative thereof as an independent variable to construct a mapping relation, and at this time, due to the accumulation of calculation errors, the added reagent volume V, the substance concentration C of the reaction solution, and the pH value of the reaction solution inevitably deviate from the time t and the pulse signal f of the original measurement sequence. According to the invention, by expanding the types of the measurement sequences, the time T, the pulse signal f, the added reagent volume V, the reaction liquid substance concentration C, the reaction liquid pH value, the spectral titration parameter S, the potentiometric titration parameter E and the temperature titration parameter T are taken as the measurement sequences, and the calculated values are replaced by the measured values of the added reagent volume V, the reaction liquid substance concentration C, the reaction liquid pH value, the spectral titration parameter S, the potentiometric titration parameter E and the temperature titration parameter T, the calculation error caused by multiple calculations is avoided, the types of the mapping relation of titration data processing and analysis are expanded, so that the experiment times are reduced, and an important reference basis is provided for comparison analysis between different measurement parameters of the same matrix.

Preferably, the measurement parameters include one or more of the volume V of the added reagent, the substance concentration C of the reaction solution, the pH value of the reaction solution, the spectral titration parameter S, the potentiometric titration parameter E and the temperature titration parameter T.

It is worth to be noted that, considering that different measurement parameters have different measurement meanings for the chemical reaction process, in order to realize the multi-dimensional characterization of the same measurement substrate at different angles, the invention adopts various measurement parameters, so that the optimal physical quantity can be selected according to the change of the compound structure for measurement and analysis.

More preferably, the signal acquisition period includes valid acquisition periods and idle periods of a plurality of measurement parameters, the acquisition starting points of the plurality of measurement parameters are unified with the signal acquisition period starting point, the acquisition ending points of the plurality of measurement parameters are unified with the signal acquisition period ending point, and the valid signal acquisition finishing points of the plurality of measurement parameters are independent from each other.

Considering that the period lengths of the signals acquired by different measurement parameters are different, in order to realize the multi-dimensional synchronous measurement of different measurement parameters on the same detection substrate, the invention unifies the acquisition starting points of a plurality of measurement parameters with the signal acquisition period starting point, unifies the acquisition ending point with the signal acquisition period ending point, and unifies the signal acquisition periods of a plurality of measurement parameters by using an idle period, so as to ensure that different measurement parameters realize one-time signal acquisition with the same signal acquisition starting point in the same signal acquisition period, thereby ensuring the synchronism of multi-dimensional titration analysis signal acquisition to the maximum extent, really realizing the synchronous measurement of different measurement parameters of the same measurement substrate, and laying a solid foundation for the analysis and comparison of multi-dimensional titration data.

Preferably, the interval period is 0 measurement sequence length, and the signal acquisition mode is continuous acquisition.

Preferably, the interval period is at least 1 measurement sequence length, the interval periods of the plurality of measurement periods are the same, and the signal acquisition mode is interval acquisition.

Preferably, the interval period is greater than or equal to 0 measurement sequence length, the measurement sequence length number of the interval period of the multiple measurement periods is independent according to user definition, and the signal acquisition mode is user-defined acquisition.

It is worth to be noted that the signal acquisition frequency of the multidimensional titration analysis is assigned according to the interval period length value set by the user, so that the mode selection of the signal acquisition mode of the titration analysis is realized, the acquisition of invalid signals is avoided, the data volume of interference signals is reduced, the detection limit and the analysis precision are improved, and the flexibility and the pertinence of the signal acquisition of the titration analysis are improved.

When the method is applied, a user can flexibly select a multi-dimensional titration analysis signal acquisition mode according to actual analysis needs and chemical reaction conditions. For a measurement sequence region with high attention, reducing the length of an interval period to obtain dense measurement points, thereby obtaining a titration data fitting curve closer to a true value; for a measurement sequence region with low attention, the interval period length is prolonged to obtain more sparse measurement points, so that the data volume is reduced, the data processing pressure is reduced, and the energy consumption of an instrument is reduced.

Exemplarily, the multidimensional titration analysis signal acquisition system is controlled to be used in combination with the multidimensional titration analysis signal identification system, and the interval period length is assigned according to a preset titration signal value. When the titration signal value is larger than a user-defined signal response threshold value, the interval period length is 0 measurement sequence length, the signal acquisition mode of the multidimensional titration analysis signal acquisition system is changed into a continuous acquisition mode, the signal acquisition density in a section of measurement sequence is improved, and the influence of a single discrete signal point on a titration fitting curve is reduced; when the titration signal value is smaller than the signal response threshold value used for self definition, the interval period length is at least 1 measurement sequence length, and different interval period lengths are set according to the chemical reaction process, so that the total data volume of titration data is reduced, and the energy consumption of an instrument is reduced.

Compared with the prior art, the invention has the following beneficial effects:

(1) for different signal acquisition periods and acquisition frequencies of different measurement parameters, the invention realizes synchronous determination of different measurement parameters of the same measurement matrix by unifying the signal acquisition periods and the measurement periods of different measurement parameters, thereby enabling multidimensional titration analysis of the same measurement matrix to be possible;

(2) according to the invention, through the adjustment of the interval period length, on the premise that the total titration data acquisition amount is not changed, the multi-dimensional titration analysis signal acquisition frequency is flexibly adjusted, so that the high-frequency acquisition of a titration signal mutation area and the low-frequency monitoring of a titration signal gentle area are realized;

(3) according to the invention, through accurate correspondence of the measurement sequence and the measurement parameter signal acquisition point, abundant information is provided for research on the change and measurement of the material structure in the reaction solution;

(4) the invention reduces the experiment times and improves the working efficiency by synchronous multidimensional titration analysis of different measurement parameters to the same measurement matrix.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.

Fig. 1 is a schematic diagram of a signal acquisition method of multidimensional titration analysis according to embodiment 1 of the present invention.

Fig. 2 is a schematic diagram of a signal acquisition method of multidimensional titration analysis according to embodiment 2 of the present invention.

Fig. 3 is a schematic diagram of a signal acquisition method of multidimensional titration analysis according to embodiment 3 of the present invention.

Fig. 4 is a schematic diagram of a signal acquisition method of multidimensional titration analysis according to embodiment 4 of the present invention.

Fig. 5 is a schematic diagram of a signal acquisition method of multidimensional titration analysis according to embodiment 5 of the present invention.

Fig. 6 is a schematic diagram of a signal acquisition method of multidimensional titration analysis according to embodiment 6 of the present invention.

Fig. 7 is a schematic diagram of a signal acquisition method of multidimensional titration analysis according to embodiment 7 of the present invention.

Fig. 8 is a schematic diagram of a signal acquisition method of multidimensional titration analysis according to embodiment 8 of the present invention.

FIG. 9 is a comparison of the collected signals of comparative example 1 and example 3 according to the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Unless otherwise defined, technical or scientific terms used in the claims and the specification should have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The use of "first," "second," and similar terms in the claims and the description of the invention do not denote any order, quantity, or importance, but rather the terms are used to distinguish one element from another.