Detection method of anhydrous potassium pyrophosphate
By drying anhydrous potassium pyrophosphate standard samples and using a plating solution analyzer to detect the concentration of the potassium pyrophosphate test solution, the problems of complex detection process and low results in the prior art are solved, and fast and accurate batch detection is achieved to meet the requirements of high purity.
Patent Information
- Application Number
- CN202510239335.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-28
- Publication Date
- 2025-04-25
AI Technical Summary
In the prior art, the detection process of anhydrous potassium pyrophosphate is complicated and takes a long time, and is not suitable for batch inspection, and the detection results are relatively low, which cannot meet the detection requirements of anhydrous potassium pyrophosphate with a purity of more than 98%.
By drying anhydrous potassium pyrophosphate standard sample to remove moisture, a potassium pyrophosphate test solution is prepared, and the concentration of the potassium pyrophosphate test solution is directly detected using a plating solution analyzer, which simplifies the operation process and is suitable for batch testing.
It realizes fast, simple and accurate detection of anhydrous potassium pyrophosphate, is suitable for batch testing, and the detection results are accurate and meets the requirements of high purity.
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Figure CN119880832A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of copper foil electroplating, and in particular to a method for detecting anhydrous potassium pyrophosphate. Background Art
[0002] In the heat resistance treatment process of copper foil surface, electroplating is generally used to plate a layer of metal on the surface of copper foil to improve the heat resistance of copper foil. In addition, these coatings can not only block the attack of amine substances in the prepreg resin on copper foil, but also help to improve the chemical affinity between copper foil and substrate, thereby improving the bonding strength between copper foil and substrate; and potassium pyrophosphate in the electroplating solution plays a complexing role, which helps to improve the dispersibility and covering ability of the electroplating solution during the electroplating process, making the coating more uniform and delicate.
[0003] In common electroplating solution inspection, it is necessary to analyze the content of anhydrous potassium pyrophosphate in the potassium pyrophosphate solution. Currently, the content of anhydrous potassium pyrophosphate is usually detected by adjusting the pH value and titration. However, this process is relatively complicated and not conducive to operation, and batch inspection is also impossible. Summary of the invention
[0004] The purpose of the embodiments of the present application is to provide a method for detecting anhydrous potassium pyrophosphate that is simple to operate and suitable for batch detection.
[0005] The present application embodiment discloses a method for detecting anhydrous potassium pyrophosphate, comprising the steps of:
[0006] Prepare anhydrous potassium pyrophosphate standards and anhydrous potassium pyrophosphate samples;
[0007] The anhydrous potassium pyrophosphate standard sample is dried;
[0008] preparing the anhydrous potassium pyrophosphate standard sample and the anhydrous potassium pyrophosphate sample into corresponding potassium pyrophosphate test solutions respectively; and
[0009] A plating solution analyzer is used to detect the concentration of the potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample, the detection result is displayed, and the detection result is analyzed and tested. If the detection result meets the preset conditions, it is judged that the detection result meets the requirements.
[0010] Optionally, the preset conditions include a test standard curve comparison analysis, in which the concentration of the potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample is detected by using a plating solution analyzer, the test result is displayed, and the test result is analyzed and tested. If the test result meets the preset conditions, the step of judging whether the test result meets the requirements includes:
[0011] preparing a plurality of first test solution samples based on the dried anhydrous potassium pyrophosphate standard sample;
[0012] Respectively detecting the concentrations of a plurality of the first test solution samples;
[0013] Establishing a test standard curve according to the concentrations and response intensities of the plurality of first test solution samples;
[0014] Substituting the test results into the test standard curve for comparative analysis; and
[0015] If the test result is consistent with the test standard curve, it is judged that the test result meets the requirements.
[0016] Optionally, the linear equation of the test standard curve is Y=0.0008X+0.0007; wherein X is the concentration of the potassium pyrophosphate test solution, and Y is the detection response intensity of the potassium pyrophosphate test solution.
[0017] Optionally, the preset conditions include performing method detection limit analysis, using a plating solution analyzer to detect the concentration of a potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample, displaying the test results, and analyzing and testing the test results. If the test results meet the preset conditions, the step of judging whether the test results meet the requirements includes:
[0018] Prepare multiple blank spiked test solutions by spiking potassium pyrophosphate based on blank reagents;
[0019] respectively detecting the concentrations of the plurality of blank spiked test solutions;
[0020] Calculating the average and standard deviation of the detection concentrations of the plurality of blank spiked test solutions;
[0021] calculating the method detection limit of the plurality of blank spiked test solutions; and
[0022] If the detection limit of the method is less than or equal to the preset value, the test result is judged to meet the requirements.
[0023] Optionally, the preset value is 0.02g / L.
[0024] Optionally, the preset conditions include spike recovery analysis, and the concentration of the potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample is detected by using a plating solution analyzer, the detection result is displayed, and the detection result is analyzed and tested. If the detection result meets the preset conditions, the step of judging whether the detection result meets the requirements includes:
[0025] preparing a plurality of second test solution samples based on the anhydrous potassium pyrophosphate sample;
[0026] Dividing the plurality of second test solution samples into a low-concentration sample group, a medium-concentration sample group, and a high-concentration sample group, wherein the low-concentration sample group, the medium-concentration sample group, and the high-concentration sample group each contain a plurality of second test solution samples;
[0027] Adding a low concentration to each second test solution sample in the low-concentration sample group, adding a medium concentration to each second test solution sample in the medium-concentration sample group, and adding a high concentration to each second test solution sample in the high-concentration sample group;
[0028] Respectively detecting the concentration of each second test solution sample in the low-concentration sample group, the concentration of each second test solution sample in the medium-concentration sample group, and the concentration of each second test solution sample in the high-concentration sample group;
[0029] Calculating the average value and standard deviation of the concentrations of the plurality of second test solution samples in the low-concentration sample group, the average value and standard deviation of the concentrations of the plurality of second test solution samples in the medium-concentration sample group, and the average value and standard deviation of the concentrations of the plurality of second test solution samples in the high-concentration sample group; and
[0030] The spiked recovery rates of the low-concentration sample group, the spiked recovery rates of the medium-concentration sample group, and the spiked recovery rates of the high-concentration sample group are calculated. If the spiked recovery rates of the low-concentration sample group, the spiked recovery rates of the medium-concentration sample group, and the spiked recovery rates of the high-concentration sample group are all within the preset standards, it is determined that the test result meets the requirements.
[0031] Optionally, the preset standard is that the spiked recovery rate is between 80% and 110%.
[0032] Optionally, the step of preparing the anhydrous potassium pyrophosphate standard sample and the anhydrous potassium pyrophosphate sample into corresponding potassium pyrophosphate test solutions comprises:
[0033] Weigh 10 g of anhydrous potassium pyrophosphate sample;
[0034] Dissolve the anhydrous potassium pyrophosphate sample in a 500 mL volumetric flask with water;
[0035] Pipette 20 ml of the solution in the 500 ml volumetric flask into a 100 ml volumetric flask to prepare a potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample.
[0036] Optionally, in the step of drying the anhydrous potassium pyrophosphate standard sample, the anhydrous potassium pyrophosphate standard sample is placed in an electric heated air drying oven and dried at 103°C±2°C.
[0037] Optionally, the plating solution analyzer is of model DPX6600.
[0038] The beneficial effects of the embodiments of the present application are as follows: in the embodiments of the present application, the moisture of the anhydrous potassium pyrophosphate standard sample is dried before use, while the test sample does not need to be dried, which can reflect the influence of moisture absorption of the anhydrous potassium pyrophosphate sample on the purity; moreover, the embodiments of the present application directly use a plating solution analyzer to detect the concentration of the potassium pyrophosphate test solution, and the concentration of the potassium pyrophosphate test solution can be directly read without complex operations such as adjusting the pH value and titration, which is simple to operate, short in time, and suitable for batch detection; finally, the embodiments of the present application analyze and test the test results to ensure the accuracy of the test results. BRIEF DESCRIPTION OF THE DRAWINGS
[0039] The included drawings are used to provide a further understanding of the embodiments of the present application, which constitute a part of the specification, are used to illustrate the implementation methods of the present application, and together with the text description, explain the principles of the present application. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work. In the drawings:
[0040] Figure 1 It is a schematic flow chart of a method for detecting anhydrous potassium pyrophosphate provided in an embodiment of the present application;
[0041] Figure 2 This embodiment of the present application provides a method based on Figure 1 Schematic diagram of the process;
[0042] Figure 3 This is another embodiment of the present application based on Figure 1 Schematic diagram of the process;
[0043] Figure 4 This is another embodiment of the present application based on Figure 1 Schematic diagram of the process;
[0044] Figure 5 This is another embodiment of the present application based on Figure 1 Schematic diagram of the process. DETAILED DESCRIPTION
[0045] It should be understood that the terms used herein, the specific structures and functional details disclosed are only for describing specific embodiments and are representative, but the present application can be implemented in many alternative forms and should not be construed as being limited to only the embodiments described herein.
[0046] In addition, unless otherwise clearly specified or limited, "connected" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be internally connected between two elements. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to specific circumstances.
[0047] At present, in the industry standard "Potassium Pyrophosphate for Electroplating", the detection of anhydrous potassium pyrophosphate requires two steps. The first step is to adjust the pH value of the solution; the second step is to titrate with a sodium hydroxide standard solution to pH = 3.80 ± 0.02, and use anhydrous sodium pyrophosphate as a standard sample and test sample for comparison, so as to calculate the potassium pyrophosphate content. However, in the document "Improvements in the Method for Determining the Content of Potassium Pyrophosphate", no standard sample is used for comparison, and titration is performed directly according to the method in "Potassium Pyrophosphate for Electroplating", and calculation is performed based on the amount of sodium hydroxide consumed.
[0048] However, in the industry standard "Potassium Pyrophosphate for Electroplating", the detection of anhydrous potassium pyrophosphate requires adjusting the pH value first and then titrating. The pH value needs to be strictly controlled during the process, which makes the pre-treatment process complicated, time-consuming, and not conducive to operation. In the document "Improvement of the Method for Determining the Content of Potassium Pyrophosphate", no standard sample was used for comparison, and titration was directly carried out according to the national standard method. The titration process also needs to strictly control the pH value. The result calculated based on the amount of sodium hydroxide consumed was found to be lower than the national standard value, which could not meet the detection requirement of anhydrous potassium pyrophosphate purity of more than 98%.
[0049] Based on the above problems, the embodiments of the present application provide a method for detecting anhydrous potassium pyrophosphate to solve the technical problem that the pH value needs to be adjusted and titrated during detection in potassium pyrophosphate, the detection process is complicated and time-consuming, and is not conducive to batch inspection; and the measured value obtained according to the document "Improvement in the Method for Determining the Content of Potassium Pyrophosphate" is lower than the actual measured value of the industry standard, and cannot meet the detection requirement of anhydrous potassium pyrophosphate with a purity of more than 98%.
[0050] like Figure 1 As shown, the detection method of anhydrous potassium pyrophosphate comprises the steps of:
[0051] S1: prepare anhydrous potassium pyrophosphate standard and anhydrous potassium pyrophosphate sample;
[0052] S2: drying the anhydrous potassium pyrophosphate standard sample;
[0053] S3: preparing the anhydrous potassium pyrophosphate standard sample and the anhydrous potassium pyrophosphate sample into corresponding potassium pyrophosphate test solutions respectively;
[0054] S4: using a plating solution analyzer to detect the concentration of the potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample, displaying the detection result, and analyzing and testing the detection result; if the detection result meets a preset condition, it is determined that the detection result meets the requirement.
[0055] In the embodiment of the present application, there is no need to dry the anhydrous potassium pyrophosphate sample before use, which can reflect the influence of the anhydrous potassium pyrophosphate sample on the purity after absorbing moisture; moreover, the embodiment of the present application directly uses a plating solution analyzer to detect the concentration of the potassium pyrophosphate test solution, and the concentration of the potassium pyrophosphate test solution can be directly read without complex operations such as adjusting the pH value and titration. The operation is simple, the time consumption is short, and it is suitable for batch detection; finally, the embodiment of the present application analyzes and tests the test results to ensure the accuracy of the test results.
[0056] In the embodiment of the present application, the anhydrous potassium pyrophosphate sample is a white powder or granular compound. Unlike potassium pyrophosphate, the anhydrous potassium pyrophosphate sample does not contain crystal water and has higher purity. In order to accurately reflect the effect of moisture absorption of the anhydrous potassium pyrophosphate sample on purity, before preparing the test solution with the anhydrous potassium pyrophosphate standard sample, the embodiment of the present application also puts the anhydrous potassium pyrophosphate standard sample into an electric blast drying oven and dries it at 103°C ± 2°C; wherein, the model of the electric blast drying oven can be specifically WGL-125B, and the anhydrous potassium pyrophosphate sample does not need to be dried and is directly prepared for testing.
[0057] It should be noted that the anhydrous potassium pyrophosphate standard is a standard part calibrated with a specific concentration, and the anhydrous potassium pyrophosphate sample is the object to be measured in the embodiments of the present application.
[0058] In order to prevent unstable readings, a sufficient amount of anhydrous potassium pyrophosphate sample was weighed in the present embodiment to prepare a potassium pyrophosphate test solution. In order to avoid excessive dilution, 10 g of anhydrous potassium pyrophosphate sample was weighed, the volume was fixed to 500 mL, and the sample was diluted 5 times before testing on the machine.
[0059] Specifically, Figure 2 As shown, in step S3, the following steps are also included:
[0060] S31: weigh 10 g of anhydrous potassium pyrophosphate sample;
[0061] S32: dissolving the anhydrous potassium pyrophosphate sample into a 500 mL volumetric flask with water;
[0062] S33: Pipette 20 ml of the solution in the 500 ml volumetric flask into a 100 ml volumetric flask to prepare a potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample.
[0063] Among them, an electronic balance with a sensitivity of 0.1 mg can be used to weigh the anhydrous potassium pyrophosphate sample, and deionized water can be used to dissolve the anhydrous potassium pyrophosphate sample to further improve the detection effect.
[0064] In step S4, the plating solution analyzer is also an electroplating plating solution analyzer, and its model is DPX6600, which specifically includes a cuvette for holding the plating solution to be tested, a light source and a photoelectric conversion unit located on both sides of the cuvette, an MCU unit connected to the photoelectric conversion unit, and an analysis result output display unit connected to the MCU unit. The plating solution analyzer used in the embodiment of the present application is implemented based on optical principles, selects a corresponding light source for ion in the plating solution, analyzes the concentration of the ion in the plating solution according to the degree of absorption of light by the plating solution, and displays the analysis result.
[0065] The result output by the analysis result output display unit is the machine-readable concentration C of the anhydrous potassium pyrophosphate sample to be tested, and its mass fraction W, the value is expressed in %, and the formula is calculated as follows:
[0066]
[0067] Where c is the machine-readable concentration of potassium pyrophosphate test solution, v is the constant volume of potassium pyrophosphate test solution, f is the dilution multiple of potassium pyrophosphate test solution, M is the mass of anhydrous potassium pyrophosphate sample, W 标 is the mass fraction of anhydrous potassium pyrophosphate standard.
[0068] Through the above design, the mass fraction of the anhydrous potassium pyrophosphate sample to be tested can be directly obtained through the plating solution analyzer, which is simple and fast to operate and easy to detect in large quantities. Of course, in some embodiments, the plating solution analyzer can also directly display the concentration of the potassium pyrophosphate test solution, and then manually calculate the mass fraction of the anhydrous potassium pyrophosphate sample.
[0069] like Figure 3 As shown, in some embodiments, the preset conditions include test standard curve comparison analysis, and correspondingly, in step S4, it also includes:
[0070] S411: preparing a plurality of first test solution samples based on the dried anhydrous potassium pyrophosphate standard sample;
[0071] S412: Detecting the concentrations of a plurality of the first test solution samples respectively;
[0072] S413: establishing a test standard curve according to the concentrations and response intensities of the plurality of first test solution samples;
[0073] S414: Substituting the test result into the test standard curve for comparison and analysis;
[0074] S415: If the test result is consistent with the test standard curve, it is determined that the test result meets the requirements.
[0075] Combined with the results shown in Table 1, specifically, 10.0000g of anhydrous potassium pyrophosphate standard sample (purity example is 98.254%) that has been dried to a constant mass in a drying oven at 103°C ± 2°C is quickly and accurately weighed by the reduction method, and the volume is adjusted to a 500mL volumetric flask with water to obtain liquid A; then 0, 5.00, 10.00, 20.00, and 25.00mL of the anhydrous potassium pyrophosphate solution of the above-mentioned liquid A are accurately transferred to a 100mL volumetric flask, and the volume is adjusted to the scale with water, and shaken. Prepare potassium pyrophosphate standard solutions with concentrations of 0, 1, 2, 4, and 5g / L, that is, five first test solution samples with concentrations of 0, 1, 2, 4, and 5g / L are obtained in S411. Finally, the machine test is carried out to obtain the response intensity of the five first test solution samples, and the five groups of data are combined to obtain the linear equation and linear correlation coefficient of the test standard curve.
[0076]
[0077] Table 1: Test standard curve parameter table
[0078] Through the above verification, the linear correlation coefficient R of the calibration curve (test standard curve) is equal to 1, and the calibration curve meets the requirements for linearity and calibration in the "Requirements for Validation and Internal Quality Control of Chemical Analysis Methods" (GB / T 32465-2015), and also meets the method requirements. The test results can be verified by substituting the test results of the potassium pyrophosphate test solution into the test standard curve for comparative analysis. Specifically, the linear equation of the test standard curve is Y=0.0008X+0.0007; wherein X is the concentration of the potassium pyrophosphate test solution, and Y is the response intensity of the potassium pyrophosphate test solution.
[0079] like Figure 4 As shown, in some embodiments, the preset conditions include method detection limit analysis, and correspondingly, in step S4, it also includes:
[0080] S421: Prepare multiple blank spiked test solutions by spiking potassium pyrophosphate based on blank reagents;
[0081] S422: Detecting the concentrations of the plurality of blank spiked test solutions respectively;
[0082] S423: Calculate the average value and standard deviation of the detection concentrations of the plurality of blank spiked test solutions;
[0083] S424: Calculate the method detection limits of the plurality of blank spiked test solutions;
[0084] S425: If the detection limit of the method is less than or equal to a preset value, it is determined that the detection result meets the requirements.
[0085] It should be noted that the blank reagent is pure water or deionized water. In S421, an anhydrous potassium pyrophosphate standard sample may be added to the blank reagent, or an anhydrous potassium pyrophosphate sample may be added to the blank reagent.
[0086] Specifically, refer to the method specified in A.1 Method Detection Limit and A.2 Determination Lower Limit in Appendix A of the Technical Guidelines for the Development of Environmental Monitoring Analytical Methods (HJ 168-2020), and perform n (n ≥ 7) parallel determinations on the blank spiked test solution of potassium pyrophosphate according to the detection method in A.1.1a in the blank test. Calculate the standard deviation of n parallel determinations, and calculate the method detection limit according to formula (A.1): MDL = t (n-1,0.99) ×S, where t is the t distribution value when the degrees of freedom are n-1 and the confidence level is 99%, t(n-1,0.99) is 3.143, and s is the standard deviation.
[0087]
[0088] Table 2: Method detection limit and determination lower limit test results
[0089] According to the full sample analysis procedure, the detection limit and determination limit of the blank spiked test solution of potassium pyrophosphate were tested. The test results are shown in Table 2. Through experimental verification, the method detection limit of anhydrous potassium pyrophosphate is 0.02g / L, which is less than or equal to the preset value of the method detection limit of 0.02g / L; the determination limit is 0.08g / L, which is less than or equal to the preset value of the determination limit of 0.08g / L, making the method detection limit and determination limit both low, and the test results meet the requirements.
[0090] It should be noted that, in some embodiments, only the method detection limit of the anhydrous potassium pyrophosphate sample may be analyzed, only the determination lower limit of the anhydrous potassium pyrophosphate sample may be analyzed, or both the method detection limit and the determination lower limit of the anhydrous potassium pyrophosphate sample may be analyzed simultaneously. The specific selection is made according to the actual situation and is not limited here.
[0091] like Figure 5 As shown, in some embodiments, the preset conditions include spike recovery analysis, and correspondingly, in step S4, it also includes:
[0092] S431: preparing a plurality of second test solution samples based on the anhydrous potassium pyrophosphate sample;
[0093] S432: Dividing the plurality of second test solution samples into a low concentration sample group, a medium concentration sample group and a high concentration sample group, wherein the low concentration sample group, the medium concentration sample group and the high concentration sample group respectively include a plurality of second test solution samples;
[0094] S433: adding a low concentration to each second test solution sample in the low concentration sample group, adding a medium concentration to each second test solution sample in the medium concentration sample group, and adding a high concentration to each second test solution sample in the high concentration sample group;
[0095] S434: respectively detecting the concentration of each second test solution sample in the low-concentration sample group, the concentration of each second test solution sample in the medium-concentration sample group, and the concentration of each second test solution sample in the high-concentration sample group;
[0096] S435: Calculate the average value and standard deviation of the concentrations of the second test solution samples in the low-concentration sample group, the average value and standard deviation of the concentrations of the second test solution samples in the medium-concentration sample group, and the average value and standard deviation of the concentrations of the second test solution samples in the high-concentration sample group;
[0097] S436: Calculate the spiked recovery rate of the low-concentration sample group, the spiked recovery rate of the medium-concentration sample group, and the spiked recovery rate of the high-concentration sample group. If the spiked recovery rate of the low-concentration sample group, the spiked recovery rate of the medium-concentration sample group, and the spiked recovery rate of the high-concentration sample group are all within the preset standard, then it is determined that the test result meets the requirements.
[0098] Specifically, weigh 10g of anhydrous potassium pyrophosphate sample, accurate to 0.0001g, dissolve it in water to 500mL; accurately transfer 10.00mL and dilute it to a 100mL volumetric flask. Use the above-mentioned A solution to spike low, medium and high concentrations (i.e., add 5.00mL, 12.50mL, and 20.00mL, respectively) according to the full sample analysis procedure, parallel determination six times, and the sample spike determination value and the recovery rate are shown in Table 3.
[0099]
[0100] Table 3: Spike recovery determination results (unit: g)
[0101] The results show that the recovery rate of the anhydrous potassium pyrophosphate solution sample spiked is in the range of 97.2% to 102.1%, which meets the accuracy requirement of 80% to 110%. The standard deviations of the low, medium and high spiked determinations of the anhydrous potassium pyrophosphate solution sample are 0.0013g / L, 0.0023g / L and 0.0052g / L respectively; the relative standard deviations are 0.43%, 0.51% and 0.86% respectively, and the precision meets the quality control and related quality management requirements of the method.
[0102] The embodiment of the present application improves the accuracy of the final test result by performing correctness and precision analysis on anhydrous potassium pyrophosphate samples.
[0103] In addition, in some embodiments, the actual anhydrous potassium pyrophosphate sample was also analyzed. Specifically, 10 g of the anhydrous potassium pyrophosphate sample was weighed, with an accuracy of 0.0001 g, and dissolved in water to 500 mL; 20.00 mL was accurately transferred and diluted to a 100 mL volumetric flask, and the sample corresponding to Table 3 was spiked and measured simultaneously. The measurement results are shown in Table 4.
[0104]
[0105] Table 4: Test results of actual potassium pyrophosphate samples (unit: g)
[0106] Through the above tests, the average purity of the anhydrous potassium pyrophosphate solution samples was 99.9%; the standard deviation and relative standard deviation were 1.09% and 1.09% respectively, which met the accuracy and precision of the method and related quality control and management requirements, thereby judging that the anhydrous potassium pyrophosphate samples met the requirements and the test results also met the requirements.
[0107] It should be noted that, in the present application embodiment, the preset conditions may include only the test standard curve comparison analysis, or only the detection limit analysis, or only the determination lower limit analysis, or only the spiked recovery analysis, or simultaneously include at least two of the test standard curve comparison analysis, the detection limit analysis, the determination lower limit analysis and the spiked recovery analysis. It can be specifically selected according to the actual situation, and is not limited here. Of course, preferably, the preset conditions simultaneously include the four of the test standard curve comparison analysis, the detection limit analysis, the determination lower limit analysis and the spiked recovery analysis, so that the detection limit of the test result is low, the accuracy is high, the reading is stable, the operation is simple, the time consumption is short, and it is suitable for batch detection.
[0108] It should be noted that the limitations on the various steps involved in this solution are not considered to limit the order of the steps without affecting the implementation of the specific solution. The steps written in front can be executed first, or later, or even simultaneously. The solutions of different implementation embodiments can be combined and applied without conflict. As long as this solution can be implemented, it should be regarded as belonging to the scope of protection of this application.
[0109] The above content is a further detailed description of the present application in combination with specific optional implementation methods, and it cannot be determined that the specific implementation of the present application is limited to these descriptions. For ordinary technicians in the technical field to which the present application belongs, several simple deductions or substitutions can be made without departing from the concept of the present application, which should be deemed to fall within the scope of protection of the present application.
Claims
1. A method for detecting anhydrous potassium pyrophosphate, characterized in that: Includes steps: Prepare anhydrous potassium pyrophosphate standards and anhydrous potassium pyrophosphate samples; The anhydrous potassium pyrophosphate standard sample is dried; The anhydrous potassium pyrophosphate standard sample and the anhydrous potassium pyrophosphate sample are respectively prepared into corresponding potassium pyrophosphate test solutions; as well as A plating solution analyzer is used to detect the concentration of the potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample, the detection result is displayed, and the detection result is analyzed and tested. If the detection result meets the preset conditions, it is judged that the detection result meets the requirements.
2. The detection method of anhydrous potassium pyrophosphate as claimed in claim 1, characterized in that, The preset conditions include a test standard curve comparison analysis, using a plating solution analyzer to detect the concentration of the potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample, displaying the test results, and analyzing and testing the test results. If the test results meet the preset conditions, the step of judging whether the test results meet the requirements includes: preparing a plurality of first test solution samples based on the dried anhydrous potassium pyrophosphate standard sample; Respectively detecting the concentrations of a plurality of the first test solution samples; Establishing a test standard curve according to the concentrations and response intensities of the plurality of first test solution samples; Substituting the test results into the test standard curve for comparative analysis; and If the test result is consistent with the test standard curve, it is judged that the test result meets the requirements.
3. The detection method of anhydrous potassium pyrophosphate as claimed in claim 2, characterized in that, The linear equation of the test standard curve is Y=0.0008X+0.0007; Wherein, X is the concentration of potassium pyrophosphate test solution, and Y is the response intensity of potassium pyrophosphate test solution.
4. The detection method of anhydrous potassium pyrophosphate as claimed in claim 1, characterized in that, The preset conditions include performing method detection limit analysis, using a plating solution analyzer to detect the concentration of the potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample, displaying the test results, and analyzing and testing the test results. If the test results meet the preset conditions, the step of judging whether the test results meet the requirements includes: Prepare multiple blank spiked test solutions by spiking potassium pyrophosphate based on blank reagents; respectively detecting the concentrations of the plurality of blank spiked test solutions; Calculating the average and standard deviation of the detection concentrations of the plurality of blank spiked test solutions; calculating the method detection limit of the plurality of blank spiked test solutions; and If the detection limit of the method is less than or equal to the preset value, the test result is judged to meet the requirements.
5. The detection method of anhydrous potassium pyrophosphate as claimed in claim 4, characterized in that, The preset value is 0.02 g / L.
6. The method for detecting anhydrous potassium pyrophosphate according to claim 1, wherein The preset conditions include spike recovery analysis, using a plating solution analyzer to detect the concentration of the potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample, displaying the test results, and analyzing and testing the test results. If the test results meet the preset conditions, the step of judging whether the test results meet the requirements includes: preparing a plurality of second test solution samples based on the anhydrous potassium pyrophosphate sample; Dividing the plurality of second test solution samples into a low-concentration sample group, a medium-concentration sample group, and a high-concentration sample group, wherein the low-concentration sample group, the medium-concentration sample group, and the high-concentration sample group each contain a plurality of second test solution samples; Adding a low concentration to each second test solution sample in the low-concentration sample group, adding a medium concentration to each second test solution sample in the medium-concentration sample group, and adding a high concentration to each second test solution sample in the high-concentration sample group; Respectively detecting the concentration of each second test solution sample in the low-concentration sample group, the concentration of each second test solution sample in the medium-concentration sample group, and the concentration of each second test solution sample in the high-concentration sample group; Calculating the average value and standard deviation of the concentrations of the plurality of second test solution samples in the low-concentration sample group, the average value and standard deviation of the concentrations of the plurality of second test solution samples in the medium-concentration sample group, and the average value and standard deviation of the concentrations of the plurality of second test solution samples in the high-concentration sample group; and The spiked recovery rates of the low-concentration sample group, the spiked recovery rates of the medium-concentration sample group, and the spiked recovery rates of the high-concentration sample group are calculated. If the spiked recovery rates of the low-concentration sample group, the spiked recovery rates of the medium-concentration sample group, and the spiked recovery rates of the high-concentration sample group are all within the preset standards, it is determined that the test result meets the requirements.
7. The method for detecting anhydrous potassium pyrophosphate according to claim 6, wherein: The preset standard is that the spiked recovery rate is between 80% and 110%.
8. The method for detecting anhydrous potassium pyrophosphate according to claim 1, wherein The step of preparing the anhydrous potassium pyrophosphate standard sample and the anhydrous potassium pyrophosphate sample into corresponding potassium pyrophosphate test solutions comprises: Weigh 10 g of anhydrous potassium pyrophosphate sample; Dissolve the anhydrous potassium pyrophosphate sample in a 500 mL volumetric flask with water; and Pipette 20 ml of the solution in the 500 ml volumetric flask into a 100 ml volumetric flask to prepare a potassium pyrophosphate test solution corresponding to the anhydrous potassium pyrophosphate sample.
9. The method for detecting anhydrous potassium pyrophosphate according to claim 1, wherein In the step of drying the anhydrous potassium pyrophosphate standard sample, the anhydrous potassium pyrophosphate standard sample is placed in an electric heated air drying oven and dried at 103° C.±2° C.
10. The method for detecting anhydrous potassium pyrophosphate according to claim 1, wherein The model of the plating solution analyzer is DPX6600.