A verification sample for road marking paint performance testing and preparation method thereof

Abstract

The invention discloses a verification sample for road marking paint performance detection and a preparation method thereof, wherein the verification sample is prepared from the following components: 45-55 parts by weight of petroleum resin, 15-20 parts by weight of titanium dioxide, 105-120 parts by weight of 250-mesh calcium powder, 90-100 parts by weight of 40-150-mesh mixed calcium powder, and 15-20 parts by weight of 40-70-mesh mixed quartz sand. After a large number of experimental studies, the invention finally determines that the capability verification paint sample obtained by adopting the formula of the invention can meet the requirements of the capability verification sample for uniformity and stability.

Description

Technical Field

[0001] The invention relates to the field of detection technology, and in particular to a capability verification sample for road marking paint performance detection and a preparation method thereof. Background Art

[0003] There is no similar method for reference in the study of hot-melt powder road marking paint as a proficiency test sample. Hot-melt powder road marking paint mainly includes film-forming materials (petroleum resin, rosin resin, etc.), pigments (titanium dioxide, chrome yellow, molybdenum cadmium red, etc.), fillers (heavy calcium carbonate, light calcium carbonate, quartz powder, etc.), dispersion media, additives, glass beads, etc. Due to its complex composition and uncertain ratio, there are currently no relevant standard samples available, and it is quite difficult to study and prepare uniform, stable, and consistent proficiency test samples. Summary of the invention

[0004] In view of this, the present invention provides a verification sample for road marking paint performance testing and a preparation method thereof. To achieve the above-mentioned purpose, the present invention mainly provides the following technical solutions:

[0005] One aspect of the present invention relates to a verification sample for testing the performance of road marking paint, which is prepared from the following components:

[0006] 45-55 parts by weight of petroleum resin, 15-20 parts by weight of titanium dioxide, 105-120 parts by weight of 250 mesh calcium powder, 90-100 parts by weight of 40-150 mesh mixed calcium powder, and 15-20 parts by weight of 40-70 mesh mixed quartz sand. The present invention adopts the above formula to ensure the uniformity and stability requirements of the verification sample. On the contrary, if any of the above components is missing, it is difficult to ensure the uniformity and stability requirements.

[0007] In a preferred embodiment of the present invention, the verification sample is prepared from the following components:

[0008] 45 parts by weight of petroleum resin, 15 parts by weight of titanium dioxide, 105 parts by weight of 250 mesh calcium powder, 90 parts by weight of 40-150 mesh mixed calcium powder, and 15 parts by weight of 40-70 mesh mixed quartz sand.

[0009] Another aspect of the present invention also relates to a method for preparing the above verification sample, comprising the following steps:

[0010] First place the sample can on the balance with a diameter no larger than the balance pan, close the side door, press the tare key, the balance will automatically calibrate the zero point, then add the raw material samples to be weighed item by item according to the formula until the required mass is reached, and record the mass of the raw materials on the record sheet; press the tare key and continue to weigh the raw materials according to the formula until the preparation is completed. The relative error of the amount of each raw material added is controlled within 1%.

[0011] In a preferred embodiment of the present invention, the preparation method further comprises the following steps: after no significant difference is found between the samples after homogeneity test, the samples are double-packaged first in a plastic sealed bag and then in a plastic sealed bottle, and stored in a dry and ventilated room.

[0012] Compared with the prior art, the present invention has the following beneficial effects:

[0013] After a large number of experimental studies, the present invention finally determined that the proficiency testing coating sample obtained by adopting the formula of the present invention can meet the requirements of the proficiency testing sample for uniformity and stability. DETAILED DESCRIPTION

[0014] In order to further explain the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the specific implementation methods, technical solutions, features and effects of the present invention application are described in detail below with preferred embodiments.

[0015] Example 1

[0016] 1. Sample preparation

[0017] The formula of the verification sample of the embodiment of the present invention is: 45 parts by weight of C5 petroleum resin, 15 parts by weight of titanium dioxide, 105 parts by weight of 250 mesh calcium powder, 90 parts by weight of 40-150 mesh mixed calcium powder (mixed calcium powder is a mixed calcium powder of various particle sizes between 40 and 150 mesh), and 15 parts by weight of 40-70 mesh mixed quartz sand (mixed quartz sand is a mixed quartz sand of various particle sizes between 40 and 70 mesh).

[0018] Specific process: first place the sample can on the balance, the diameter of the sample can is not larger than the balance pan, close the side door, press the tare key, the balance will automatically calibrate the zero point, and then add the raw material samples to be weighed item by item according to the formula until the required mass is reached, and record the mass of the raw materials on the record sheet; press the tare key, continue to weigh the raw materials according to the formula until the preparation is completed, and the relative error of each raw material addition is controlled within 1%; prepare a total of 65 samples according to the above preparation method, each 270±2.7g. After the uniformity test shows that there is no significant difference between the samples, the samples are first double-packed in plastic sealed bags and then in plastic sealed bottles, and stored in a dry and ventilated room; after the transportation stability test, the samples have no significant difference during transportation and are sent to the participating laboratories by express companies at the same time. Each participating laboratory will be issued 1 sample, and the samples will be randomly distributed according to the registration of the participating laboratories.

[0019] 2. Uniformity Test

[0020] 1. Inspection items

[0021] Density, compressive strength (23±1)℃.

[0022] 2. Sampling plan

[0023] Ten samples were randomly selected from the 65 samples to be dispatched and tested for uniformity in a random order.

[0024] 3. Inspection methods

[0025] The same test personnel shall use the same set of equipment to complete the test of all samples at one time within a continuous period of time in accordance with "Road Marking Paint" JT / T 280-2022. Before the test, the sample blocks shall be conditioned in an environment of ((23±2)℃, ((50±5)%RH) for 24h.

[0026] 4. Uniformity test results

[0027] Since the density and compressive strength tests of the coatings need to be prepared into cubic specimens, and the compressive strength is a destructive test, before the results of the participating laboratories are fed back, the standard deviation of the capability assessment of the previous proficiency verification program project is used for preliminary judgment. Its value refers to the standard deviation of the laboratory comparison project assessment of 32 institutions organized in 2019. This project cannot be tested repeatedly, and the standard deviation of the measurement results S is used as S s According to the Statistical Methods for Proficiency Testing Using Inter-laboratory Comparisons CB / T28043-2019 S ≤0.3σ criterion for judgment,

[0028] After the results of the participating laboratories are returned and statistically analyzed, the S S The uniformity of the sample is tested at ≤0.3σ, and the test result is the final judgment of the uniformity test.

[0029]

[0030] Conclusion: The uniformity test of the verification sample in this embodiment is S≤0.3σ, and the sample meets the uniformity requirement.

[0031] 3. Stability Test

[0032] Stability test includes transportation stability test and time stability test. The test method is the same as uniformity test.

[0033] (I) Test results of transport stability and time stability during the sample verification phase

[0034] The detection method of the sample transportation stability verification stage is based on "Road Marking Paint" JT / T 280-2004, which was issued and implemented on June 9, 2022. It has been confirmed by the method that there is no change in the density and compressive strength test methods of hot-melt road marking paints. Therefore, in Example 1, the transportation stability test results refer to the results of the sample verification stage.

[0035] During the sample verification phase, the sample transportation stability and 3-month stability tests were conducted. The test results can fully prove that the sample is sufficiently stable during the transportation process of the proficiency testing plan. Therefore, the transportation stability test is no longer performed during the implementation of Example 1 and the subsequent proficiency testing plan. The specific test results are as follows:

[0036] The samples are drawn from the samples that have been configured and packaged in the sample library. The total number of samples is 50. The configuration time is May 6-7, 2022. They are transported after being wrapped in special anti-collision paper and special cartons for express delivery.

[0037] 1. Inspection items

[0038] Density, compressive strength (23±1)℃.

[0039] 2. Check sample quantity and transportation conditions

[0040] On May 10, 2022, 10 samples were randomly selected from 50 samples for the first inspection. The randomly selected samples were 33, 28, 1, 32, 7, 2, 4, 3, 9, and 23.

[0041] On July 19, 2022, 10 samples were randomly selected for transportability inspection, and the randomly selected samples were 50, 47, 24, 5, 12, 45, 20, 29, 11, and 10. The time from the delivery of the samples to the return of the express delivery was 8 days in total. The specific transportation details are shown in the table below.

[0042]

[0043] 3. Inspection time

[0044] First inspection date: May 10, 2022

[0045] Second inspection date: August 1, 2022

[0046] 4. Inspection methods

[0047] In accordance with "Road Marking Paint" JT / T 280-2004 and "Road Marking Paint Density, Compressive Strength Determination Capability Verification Implementation Details" JKJC-P-ZY-02, the first and second inspection personnel and equipment are the same, and the same person and the same set of equipment will complete the inspection of all samples in the most continuous time possible.

[0048] 5. Stability test evaluation

[0049] The t-test method in CNAS-GL003:2018 "Guidelines for the Evaluation of Homogeneity and Stability of Proficiency Testing Samples" was used to evaluate whether there was a significant difference between the two mean values ​​of the samples, and then the statistical method in Appendix B5.1 of GB / T 28043-2019 "Statistical Methods for Proficiency Testing Using Inter-laboratory Comparisons" was used to Further verification. The test results are shown in the following table:

[0050]

[0051] (2) Criteria Verification

[0052] The samples used in this stability test are consistent with the sample formula used in the laboratory comparison project organized by 32 institutions in 2019. They are all configured in accordance with JKJC-P-ZY-01 "Preparation Rules for Proficiency Testing Items". When the criteria are further validated, reference is made to the standard deviation of the assessment items using laboratory comparisons.

[0053]

[0054] Conclusion: The road marking paint samples were stable over a period of 80 days and during express transportation.

[0055] (II) Stability test during proficiency testing

[0056] 1. Inspection items

[0057] Density, compressive strength (23±1)℃.

[0058] 2. Sampling plan

[0059] After the results of the participating laboratories are returned, 6 samples are randomly selected from the remaining 19 samples that have not been issued in the sample library of this batch and stability tests are carried out in random order.

[0060] 3. Inspection methods

[0061] The same test personnel shall use the same set of equipment to complete the test of all samples at one time within a continuous period of time in accordance with "Road Marking Paint" JT / T 280-2022. Before the test, the sample blocks shall be conditioned at (23±2)℃, ((50±5)%RH) for 24h.

[0062] 4. Stability test results

[0063] The total average difference of the uniformity test and stability test of the samples in this comparison test It was verified that the samples in this comparison test were stable enough.

[0064]

[0065] in conclusion: , the road marking paint samples met the requirements in terms of sample stability.

[0066] The above disclosure is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the above claims.

Claims

1. A verification sample for road marking paint performance testing, characterized in that: Formulated from the following components: 45-55 parts by weight of petroleum resin, 15-20 parts by weight of titanium dioxide, 105-120 parts by weight of 250 mesh calcium powder, 90-100 parts by weight of 40-150 mesh mixed calcium powder, and 15-20 parts by weight of 40-70 mesh mixed quartz sand.

2. The verification sample according to claim 1, characterized in that: The verification sample was prepared from the following components: 45 parts by weight of petroleum resin, 15 parts by weight of titanium dioxide, 105 parts by weight of 250 mesh calcium powder, 90 parts by weight of 40-150 mesh mixed calcium powder, and 15 parts by weight of 40-70 mesh mixed quartz sand.

3. The method for preparing a verification sample according to claim 1 or 2, characterized in that: The steps include: First place the sample can on the balance with a diameter no larger than the balance pan, close the side door, press the tare key, the balance will automatically calibrate the zero point, then add the raw material samples to be weighed item by item according to the formula until the required mass is reached, and record the mass of the raw materials on the record sheet; press the tare key and continue to weigh the raw materials according to the formula until the preparation is completed. The relative error of the amount of each raw material added is controlled within 1%.

4. The method for preparing a verification sample according to claim 3, characterized in that: The preparation method further comprises the following steps: after the samples are tested for uniformity and no significant difference is found between the samples, they are firstly double-packed in a plastic sealed bag and then in a plastic sealed bottle, and stored in a dry and ventilated room.

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