Prediction method for maximum migration quantity of metal ions in photosensitive material storage container

Abstract

The invention discloses a method for predicting the maximum migration amount of metal ions in a photosensitive material storage container, and belongs to the field of photosensitive material storage containers. The prediction method comprises the following steps: adding an extracting agent into a storage container to be detected; placing the storage container to be detected at a set temperature, and carrying out mechanical and / or ultrasonic oscillation extraction; sucking a set amount of extracting solution from the storage container to be detected according to a set time interval; obtaining the concentration of metal ions in the extracting solution, and establishing a metal ion concentration-time curve; calculating the first-order differential of the concentration of the metal ions to the time, taking the maximum value of the result, and calculating the maximum migration rate of the metal ions in the storage container to be detected; and calculating the maximum migration quantity of the metal ions in the process of storing the photosensitive material in the storage container. According to the method, the maximum migration quantity of the metal ions of the photosensitive material storage container under different extracting agents, different temperatures and different oscillation modes can be rapidly evaluated, and guidance is provided for selecting a proper storage container for the photosensitive material.

Description

Technical Field

[0001] The present invention relates to the field of storage containers for photosensitive materials, and particularly to a method for predicting the maximum migration amount of metal ions in a storage container for photosensitive materials. Background Art

[0002] During the storage of photosensitive materials, metal ions in storage containers made of glass or plastic are likely to migrate to the photosensitive materials, resulting in excessive metal ion content. Therefore, the industry attaches great importance to the migration amount of metal ions in storage containers for photosensitive materials.

[0003] The existing conventional method is to inject a suitable organic solvent or photosensitive material into the storage container, extract the metal ions in the container by long-term soaking (not less than 6 months), and then measure the concentration of metal ions in the extractant to evaluate whether the storage container is compatible with the stored photosensitive materials. The main problems of this method are as follows: (1) The evaluation period is too long, which is very different from the requirements for test efficiency in the actual application process; (2) It can only evaluate the migration amount under static conditions and cannot evaluate the influence of handling on the migration of metal ions; (3) The influence of the contact area between the extractant and the storage container is not considered, while in fact, the contact area is an important factor affecting the migration of metal ions; (4) The test result is the concentration of metal ions, and the migration rate cannot be calculated, so the migration amount of metal ions in storage containers of the same material but different specifications and sizes cannot be predicted and evaluated through the migration rate. Currently, there is still a blank in using the dynamic method to simulate the transportation process and quickly evaluate the migration rate and migration amount of metal ions in storage containers for photosensitive materials through accelerated experiments.

[0004] In summary, it is necessary to propose a reasonable, simple, scientific, and fast and accurate method for predicting the migration amount of metal ions in a storage container for photosensitive materials, reducing the error of human factors, ensuring the health of test personnel, and guaranteeing the scientificity and rigor of the experiment. Summary of the Invention

[0005] In view of this, the present invention provides a method for predicting the maximum migration amount of metal ions in a storage container for photosensitive materials. The main purpose is to select appropriate temperature, extractant, oscillation mode, and oscillation frequency according to the actual application scenarios (properties of photosensitive materials, transportation conditions, storage environment), quickly simulate and evaluate the migration amount of metal ions in a storage container for photosensitive materials, provide a scientific basis for evaluating the compatibility between the storage container and the photosensitive material to be filled, and provide guidance for selecting a suitable storage container for the photosensitive material.

[0006] The technical solution provided by the present invention is as follows:

[0007] A method for predicting the maximum migration amount of metal ions in a storage container for photosensitive materials, comprising the following steps:

[0008] S1. Add a certain volume of extraction agent to the storage container to be tested, seal the mouth of the storage container to be tested, and calculate the contact ratio K. The contact ratio K is the ratio of the contact area S between the extraction agent and the storage container to be tested to the volume V of the extraction agent. The unit of the contact ratio K is square decimeters per liter.

[0009] S2. Place the storage container to be tested filled with the extraction agent at a set temperature, and perform mechanical oscillation and / or ultrasonic oscillation extraction on the storage container to be tested filled with the extraction agent; the temperature is -25 to 60 °C. The mechanical oscillation includes one of the ways of swinging and rotating. The mechanical oscillation frequency is 0 to 100 times per minute, and the ultrasonic frequency is 0 to 80 kHz.

[0010] S3. Absorb a set amount of extraction liquid from the storage container to be tested at set time intervals, and add an equal amount of extraction agent to the storage container to be tested after each absorption of the extraction liquid.

[0011] S4. Obtain the concentration of metal ions in each absorbed extraction liquid and establish a curve of metal ion concentration - time; the specific metal ions include sodium ions, potassium ions, calcium ions, magnesium ions, aluminum ions, chromium ions, manganese ions, iron ions, cobalt ions, nickel ions, copper ions, and zinc ions.

[0012] S5. For the concentration of metal ions and the corresponding time in each measured extraction liquid, calculate the first - order differential of the metal ion concentration with respect to time, that is, dc i / dt; take the maximum value in the first - order differential calculation result, that is, (dc i / dt) max ;

[0013] S6. Calculate the maximum migration rate of metal ions in the storage container to be tested under this extraction condition according to the following formula:

[0014] ;

[0015] In the formula:

[0016] MR i(max) is the maximum migration rate of metal ion i, and the unit is micrograms per square decimeter per day.

[0017] S7. Calculate the maximum migration amount of metal ions in storage containers of the same material and different specifications and sizes during the storage of photosensitive materials under the same extraction condition according to the following formula:

[0018] MR i(max) ×A×t;

[0019] In the formula:

[0020] Q i(max)$Q_{max}$ is the maximum migration amount of metal ion $i$, in micrograms;

[0021] $A$ is the contact area between the photosensitive material and the inner wall of the storage container, in square decimeters;

[0022] $t$ is the storage time, in days.

[0023] According to the prediction method for the maximum migration amount of metal ions in the photosensitive material storage container described above, in step S1, the extractant is propylene glycol methyl ether acetate or a specific type of photosensitive material, and the specific type of photosensitive material is the material planned to be filled in the storage container.

[0024] Further, in step S2, the storage container to be tested filled with the extractant is placed in the medium tank, and the storage container to be tested is fixed with a fixture; the medium tank is filled with the medium; under the combined action of the heater, cooler, temperature sensor and circulation pump, the medium in the medium tank and the extractant in the storage container to be tested are maintained at the set temperature; the storage container to be tested is mechanically oscillated under the action of the mechanical oscillator; the ultrasonic generator performs ultrasonic oscillation on the storage container and the extractant inside it; the control system is respectively connected to the heater, cooler, mechanical oscillator, ultrasonic generator, temperature sensor and circulation pump, and is used for setting temperature, oscillation mode, oscillation frequency, extraction time parameters and the opening and closing control of the device.

[0025] Further, the medium is one of water, ethylene glycol, and water / ethylene glycol mixture.

[0026] According to the prediction method for the maximum migration amount of metal ions in the photosensitive material storage container described above, in step S3, the set time interval is 1 day, or 5 days, or 7 days, and the set amount of the extraction solution aspirated each time is 1 - 5 mL.

[0027] According to the prediction method for the maximum migration amount of metal ions in the photosensitive material storage container described above, the concentration of metal ions in the extractant aspirated each time is analyzed and obtained by using an inductively coupled plasma - mass spectrometer; it specifically includes the following steps:

[0028] S41. Preparation of a series of standard solutions: Take 5.0 mL of a 1.0 mg / L mixed standard solution of metal ions (including sodium ions, potassium ions, calcium ions, magnesium ions, aluminum ions, chromium ions, manganese ions, iron ions, cobalt ions, nickel ions, copper ions, and zinc ions), place it in a volumetric flask, and dilute it to 100 mL with a 2% (v / v) nitric acid solution to prepare a mixed standard solution A with a mass concentration of 50.00 μg / L; take 10.0 mL of mixed standard solution A and dilute it to 100 mL with a 2% (v / v) nitric acid solution to prepare a mixed standard solution B with a mass concentration of 5.00 μg / L; respectively take 0, 1.0 mL, 2.0 mL, 4.0 mL, and 10.0 mL of mixed standard solution B and place them in 5 volumetric flasks, and dilute them to 100 mL with N-methylpyrrolidone to prepare a series of mixed standard solutions with concentrations of 0, 50.0 ng / L, 100.0 ng / L, 200.0 ng / L, and 500.0 ng / L; the volumetric flasks are made of tetrafluoroethylene perfluoroalkoxy copolymer;

[0029] S42. Calibration curve plotting: Using an inductively coupled plasma-mass spectrometer, measure the signal intensities of each metal ion in the mixed standard solutions of metal ions with different concentrations, and plot a standard curve with the concentration as the abscissa and the response value as the ordinate;

[0030] S43. Use an inductively coupled plasma-mass spectrometer to measure the extract, obtain the signal intensity of the metal ions to be measured in the extract, and substitute it into the standard curve of the metal ion to obtain the concentration of the metal ions to be measured.

[0031] Furthermore, use an inductively coupled plasma-mass spectrometer to analyze and obtain the concentration of metal ions in each aliquot of the extract taken. The specific analysis conditions are as follows:

[0032] The RF power is 1400 - 1600 W, the plasma gas flow rate is 15 - 20 L / min, the argon auxiliary gas flow rate is 1.0 - 1.4 L / min; the argon carrier gas flow rate is 0.7 - 0.8 L / min, and the vacuum degree of the analysis chamber is 0.9×10 -6 ~1.1×10 -6 , and the pulsed voltage is 800 - 1000 V; the conditions of the organic injection system are: the oxygen flow rate is 7 - 9 mL / min, and the temperature is 2 - 4 °C.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] (1)The prediction method provided by the present invention can select appropriate temperature, extractant, oscillation mode and oscillation frequency according to the actual application scenarios (properties of photosensitive materials, transportation conditions, storage environment), quickly simulate and evaluate the migration amount of metal ions in the storage container of photosensitive materials, and provide a scientific basis for evaluating the compatibility between the storage container and the photosensitive materials to be filled;

[0035] (2)The prediction method provided by the present invention comprehensively considers the influence of the contact area between the extractant and the storage container and the volume of the extractant. The test results are accurate and have good repeatability, the evaluation period is short, the labor and time costs are greatly saved, and it can be widely used for the quality control of storage containers for photosensitive materials, and can provide a reference basis for formulating standards in the future;

[0036] (3)The prediction method provided by the present invention uses an inductively coupled plasma-mass spectrometer as an analytical instrument to detect the concentration of metal ions, and establishes a method for determining the maximum migration amount of various common metal ions in the storage container of photosensitive materials. This method is fast, accurate and highly sensitive;

[0037] (4)The prediction method provided by this patent can provide guidance for the selection of storage containers corresponding to photosensitive materials to reduce the migration of metal ions to photosensitive materials. Description of the Drawings

[0038] Figure 1 Schematic diagram of the implementation process of the prediction method for the maximum migration amount of metal ions in the storage container of photosensitive materials;

[0039] Figure 2 Schematic diagram of the principle of the device for providing temperature, ultrasound and oscillation to the storage container to be tested filled with extractant;

[0040] Figure 3 For the K migrated by storage container A in Example 1 + Concentration-time curve and dc i / dt-time curve data diagram;

[0041] Figure 4 For the Na migrated by storage container A in Example 1 + Concentration-time curve and dc i / dt-time curve data diagram.

[0042] Description of the reference numerals:

[0043] 1. Medium tank; 2. Fixture; 3. Medium; 4. Heater; 5. Cooler; 6. Temperature sensor; 7. Circulation pump; 8. Mechanical oscillator; 9. Ultrasonic generator; 10. Control system. Detailed Embodiments

[0044] To make the technical problems, technical solutions, and advantages to be solved by the present invention clearer, the technical solutions of the present invention will be clearly and completely described below in conjunction with the drawings Figures 1 to 4 and specific embodiments.

[0045] The present invention provides a method for predicting the maximum migration amount of metal ions in a photosensitive material storage container, which is used to evaluate the migration performance of metal ions in the photosensitive material storage container. This method can analyze the compatibility between the storage container and the photosensitive material, helping to select a storage container that meets the storage requirements of the photosensitive material and improving the quality of the photosensitive material.

[0046] The present invention provides a method for predicting the maximum migration amount of metal ions in a photosensitive material storage container, which specifically includes the following steps:

[0047] S1. Add a certain volume of extractant to the storage container to be tested, and seal the mouth of the storage container to be tested. Calculate the contact ratio K. The contact ratio K is the ratio of the contact area S between the extractant and the storage container to be tested to the volume V of the extractant. The unit of the contact ratio K is square decimeters per liter.

[0048] Preferably, the extractant is propylene glycol methyl ether acetate or a specific type of photosensitive material, and the specific type of photosensitive material is the material planned to be contained in the storage container. In actual use, a storage container is only used to store the photosensitive material compatible with it; if incompatible photosensitive materials are stored, it will cause pollution to the photosensitive material and have an adverse effect.

[0049] S2. Place the storage container to be tested filled with the extractant at a set temperature, and perform mechanical oscillation and / or ultrasonic oscillation on the storage container to be tested filled with the extractant.

[0050] Preferably, the temperature is -25 to 60 °C. The mechanical oscillation includes one of the ways of swinging and rotating, the oscillation frequency is 0 to 100 times per minute, and the ultrasonic frequency is 0 to 80 kHz. More preferably, the mechanical oscillation frequency is 10 to 100 times per minute; when there is ultrasonic action, the ultrasonic frequency is 10 to 80 kHz.

[0051] In step S2, specifically, a device for providing temperature and oscillation to the storage container to be tested filled with the extractant is provided. The device used includes a medium tank 1, a heater 4, a cooler 5, a mechanical oscillator 8, an ultrasonic generator 9, a temperature sensor 6, a circulation pump 7, and a control system 10. The medium tank 1 is made of stainless steel and wrapped with a heat-insulating layer, and is used to contain the medium 3 and install the storage container to be tested. The medium 3 is added into the medium tank 1, and a fixing fixture 2 is arranged in the medium tank 1, and the fixing fixture 2 fixes the storage container to be tested in the medium tank 1. The heater 4 consists of electric heating coils with different powers and quickly heats the medium 3. The cooler 5 consists of components such as a compressor, a condenser, a capillary tube, and an evaporator, and cools the medium 3. The circulation pump 7 circulates the medium 3 to ensure uniform temperature of the medium 3. The temperature range of the temperature sensor 6 is -30°C to 100°C, and it is water- and oil-resistant. The heater 4, the cooler 5, the temperature sensor 6, and the circulation pump 7 work together, and the medium 3 in the medium tank 1 and the extractant in the container to be tested are maintained at the set temperature. The mechanical oscillator 8 performs mechanical oscillation on the container to be tested, and the oscillation frequency is 0 to 100 times per minute, simulating the oscillation effect on the container to be tested during transportation. The ultrasonic generator 9 performs ultrasonic oscillation on the storage container to be tested and the extractant therein, and the oscillation frequency is 0 to 80 kHz to accelerate the migration of metal ions in the storage container to be tested and shorten the experimental period. The control system 10 is respectively connected to the heater 4, the cooler 5, the mechanical oscillator 8, the ultrasonic generator 9, the temperature sensor 6, and the circulation pump 7, and is used to set parameters such as temperature, oscillation mode, oscillation frequency, extraction time, etc. and control the opening and closing of the device. In the present invention, the storage container to be tested filled with the extractant is placed in the medium tank 1, and the storage container to be tested is fixed by the fixture 2; the medium 3 is injected into the medium tank 1; under the combined action of the heater 4, the cooler 5, the temperature sensor 6, and the circulation pump 7, the medium 3 in the medium tank 1 and the extractant in the container to be tested are maintained at the set temperature; the container to be tested performs mechanical oscillation under the action of the mechanical oscillator 8; the ultrasonic generator 9 performs ultrasonic oscillation on the container to be tested and the extractant therein.

[0052] Further, the medium 3 is one of water, ethylene glycol, and a water / ethylene glycol mixture. The freezing point of pure ethylene glycol is usually -11.5°C. However, when ethylene glycol is mixed with water, the freezing point will be significantly reduced. When the temperature is above 0°C, water is used as the medium 3; when the temperature is between -10°C and 0°C, ethylene glycol is used as the medium 3; when the temperature is between -25°C and -10°C, a water / ethylene glycol mixture is used as the medium 3, and the ratio of water and ethylene glycol is adjusted according to the actual temperature requirement.

[0053] S3. Draw a set amount of extraction solution from the storage container to be measured at set time intervals. After each draw of the extraction solution, add an equal amount of extractant to the storage container to be measured. The set time intervals are 1 day, or 5 days, or 7 days, and the set amount of extraction solution drawn each time is 1 - 5 mL. Drawing the extraction solution from the storage container to be measured and adding an equal amount of extractant ensures that each draw of the extractant is done at the same contact ratio, ensuring the accuracy of the experimental results. The extractant is a metal - ion - free liquid, and the extraction solution is a mixed liquid of metal ions and the extractant.

[0054] S4. Obtain the concentration of metal ions in the extraction solution drawn each time, and establish a metal - ion concentration - time curve.

[0055] Specifically, use an inductively coupled plasma - mass spectrometer to analyze and obtain the concentration of metal ions in the extraction solution drawn each time. It specifically includes the following steps:

[0056] S41. Preparation of a series of standard solutions: Take 5.0 mL of a 1.0 mg / L mixed standard solution of metal ions (including sodium ions, potassium ions, calcium ions, magnesium ions, aluminum ions, chromium ions, manganese ions, iron ions, cobalt ions, nickel ions, copper ions, and zinc ions), place it in a volumetric flask, and dilute it to 100 mL with a 2% (by volume) nitric acid solution to prepare a mixed standard solution A with a mass concentration of 50.00 μg / L; take 10.0 mL of mixed standard solution A and dilute it to 100 mL with a 2% (by volume) nitric acid solution to prepare a mixed standard solution B with a mass concentration of 5.00 μg / L; respectively take 0, 1.0 mL, 2.0 mL, 4.0 mL, and 10.0 mL of mixed standard solution B and place them in 5 volumetric flasks, and dilute them to 100 mL with N - methylpyrrolidone to prepare a series of mixed standard solutions with concentrations of 0, 50.0 ng / L, 100.0 ng / L, 200.0 ng / L, and 500.0 ng / L; the volumetric flasks are made of tetrafluoroethylene perfluoroalkoxy copolymer material;

[0057] S42. Plotting the calibration curve: Use an inductively coupled plasma mass spectrometer to measure the signal intensity of each metal ion in the metal - ion mixed standard solutions with different concentrations, and plot a standard curve with the concentration as the abscissa and the response value as the ordinate;

[0058] S43. Use an inductively coupled plasma mass spectrometer to measure the extraction solution to obtain the signal intensity of the metal ions to be measured in the extraction solution, and substitute it into the standard curve of this metal ion to obtain the concentration of the metal ions to be measured.

[0059] The mass numbers and plasma ionization modes of the elements to be measured in S42 and S43 are shown in Table 1.

[0060] Table 1

[0061]

[0062] When analyzing and obtaining the concentration of metal ions in each aspirated extract using an inductively coupled plasma mass spectrometer, the specific analysis conditions are as follows: the RF power is 1400 - 1600 W, the plasma gas flow rate is 15 - 20 L / min, the argon auxiliary gas flow rate is 1.0 - 1.4 L / min; the argon carrier gas flow rate is 0.7 - 0.8 L / min, and the analysis chamber vacuum degree is 0.9×10 -6 ~1.1×10 -6 , the pulse voltage is 800 - 1000 V; the conditions of the organic injection system are: the oxygen flow rate is 7 - 9 mL / min, and the temperature is 2 - 4 °C.

[0063] S5. For the concentration of metal ions in each measured extract and the corresponding time, calculate the first-order differential of the metal ion concentration with respect to time, that is, dc i / dt; take the maximum value in the first-order differential calculation result, that is, (dc i / dt) max ;

[0064] S6. Calculate the maximum migration rate of metal ions in the storage container to be measured under this extraction condition (this extraction condition refers to the extraction condition in S2) according to the following formula:

[0065] ;

[0066] In the formula:

[0067] MR i(max) is the maximum migration rate of metal ion i, with the unit of micrograms per square decimeter per day;

[0068] S7. Calculate the maximum migration amount of metal ions in storage containers of the same material and different specifications and sizes during the storage of photosensitive materials under the same extraction condition (that is, the same as the extraction condition in S2, and the extraction condition includes temperature, mechanical oscillation, and ultrasonic oscillation conditions) according to the following formula:

[0069] MR i(max) ×A×t;

[0070] In the formula:

[0071] Q i(max) is the maximum migration amount of metal ion i, with the unit of micrograms;

[0072] A is the contact area between the photosensitive material and the inner wall of the storage container, with the unit of square decimeters;

[0073] t is the storage time, with the unit of days.

[0074] The photosensitive material storage container of the present invention may be in the shape of a cylindrical bottle or a rectangular shell. The prediction method provided by the present invention may meet the requirements of inspection and testing of storage containers of different shapes and sizes.

[0075] Metal ions include but are not limited to sodium ions, potassium ions, calcium ions and magnesium ions. Other metal ions present in the photosensitive material storage container such as aluminum ions, chromium ions, manganese ions, iron ions, cobalt ions, nickel ions, copper ions, zinc ions, etc. can be detected and analyzed using the method provided by the present invention.

[0076] Compared with the prior art, the present invention has the following beneficial effects:

[0077] (1) The prediction method provided by the present invention can select appropriate temperature, extractant, oscillation mode and oscillation frequency according to the actual application scenario (properties of photosensitive materials, transportation conditions, storage environment), quickly simulate and evaluate the migration amount of metal ions in the photosensitive material storage container, and provide a scientific basis for evaluating the compatibility between the storage container and the photosensitive material to be contained.

[0078] (2) The prediction method provided by the present invention comprehensively considers the influence of the contact area between the extractant and the storage container and the volume of the extractant. The test results are accurate and repeatable, the evaluation cycle is short, and the manpower and time costs are greatly saved. It can be widely used in the quality control of photosensitive material storage containers and provide a reference for the formulation of standards in the future.

[0079] (3) The prediction method provided by the present invention uses an inductively coupled plasma-mass spectrometer to detect the concentration of metal ions and establishes a method for determining the maximum migration amount of multiple metal ions commonly found in photosensitive material storage containers. This method is rapid, accurate, and highly sensitive.

[0080] The following is a specific example of a method for predicting the maximum migration amount of metal ions in a photosensitive material storage container.

[0081] Embodiment 1:

[0082] A company produces two cylindrical glass storage containers A and B of the same shape and size but different materials. The outer diameter and wall thickness of the two containers to be tested are measured respectively. The inner diameter is calculated to be 0.86dm, the height of the cylindrical part is measured to be 2.12dm, and the volume is calculated to be 1.23L. The following steps are included:

[0083] Propylene glycol methyl ether acetate was selected as the extractant, and 0.75 L of propylene glycol methyl ether acetate was added to storage container A and storage container B respectively, and the mouths of storage container A and storage container B were sealed. The calculated extraction contact ratio K was 5.42 dm 2 / L.

[0084] Place the storage containers A and B containing the extractant at the set temperatures respectively, and ultrasonically vibrate and oscillate the storage containers to be tested containing the extractant. Place the storage containers to be tested containing the extractant in the aforementioned device.

[0085] Set the temperature to 20 °C, the mechanical oscillation mode to swing, the oscillation frequency to 1 time / min, and the ultrasonic oscillation frequency to 0 kHz.

[0086] Draw a set amount of extract from storage containers A and B respectively at the set time intervals, and add an equal amount of extractant to storage containers A and B each time after drawing the extractant.

[0087] Every 7 days, use a microsyringe to draw 2 mL of extract from the container to be tested, and immediately supplement 2 mL of propylene glycol methyl ether acetate to the container to be tested.

[0088] Obtain the concentration of metal ions in the extract drawn each time, and establish a curve of metal ion concentration - time. Use an inductively coupled plasma - mass spectrometer to measure the concentration of metal ions therein. The results are shown in Tables 2 and 3, where Table 2 is the concentration of metal ions migrated from storage container A, and Table 3 is the concentration of metal ions migrated from storage container B.

[0089] Table 2

[0090]

[0091] Table 3

[0092]

[0093] Using time as the abscissa and the concentration of metal ions as the ordinate to plot a graph, obtain a curve of metal ion concentration - time. For the concentration of metal ions and the corresponding time in each measured extract, calculate the first - order differential of the metal ion concentration with respect to time, i.e., dc i / dt; Figure 3 is the concentration - time curve and dc + / dt - time curve data graph of K i migrated from storage container A, Figure 4 is the concentration - time curve and dc + / dt - time curve data graph of Na i migrated from storage container A (the unit of time on the abscissa in the figure is "d", which means "day"). Take the maximum value in the first - order differential calculation results to obtain the maximum migration slope (dc i / dt) max , according to the maximum migration slope (dc i / dt) maxAnd the contact ratio K, calculate the maximum migration rate MR of metal ions in storage container A and storage container B under this extraction condition i(max) , as shown in Table 4

[0094] Table 4

[0095]

[0096] It can be found by comparison that for K + , Na + , Mg 2+ in storage container B, the migration rate is much greater than that in storage container A, and for Ca 2+ , the migration rate is slightly greater than that in storage container A

[0097] Calculate the maximum migration amount Q of metal ions in storage containers of the same material and different specifications and sizes during the storage of photosensitive materials under the same temperature and extraction conditions i(max) :

[0098] Prepare storage container A' and storage container B' with a volume of 4L respectively using the same raw materials as storage container A and storage container B, and predict the maximum migration amount Q of metal ions in photosensitive materials with PGMEA as the diluent after 180 days of storage in storage container A' and storage container B' respectively i(max) .

[0099] First, it is measured that the inner radii of storage container A' and storage container B' are both 1.62 dm, and the cylindrical heights are both 1.91 dm. When fully filled, the contact areas of the photosensitive materials with the inner walls of storage container A' and storage container B' are 11.78 dm 2 , and the predicted results of the maximum migration amounts of metal ions in storage container A' and storage container B' are shown in Table 5

[0100] Table 5

[0101]

[0102] Example 2

[0103] Using a certain type of photosensitive material (PM-X) as the extractant, and also using storage container A and storage container B as storage containers, with other conditions (temperature, extraction method) being exactly the same as in Example 1. Table 6 shows the concentrations of metal ions migrated by storage container A, and Table 7 shows the concentrations of metal ions migrated by storage container B

[0104] Table 6

[0105]

[0106] Table 7

[0107]

[0108] Taking time as the abscissa and the concentration of metal ions as the ordinate to plot a graph, a curve of metal ion concentration - time is obtained. For the concentration of metal ions and the corresponding time measured in each extraction solution, the first - order differential of the metal ion concentration with respect to time is calculated, that is, dc i / dt; take the maximum value in the calculation results of the first - order differential, and obtain the maximum migration slope (dc i / dt) max , according to the maximum migration slope (dc i / dt) max and the contact ratio K, calculate the maximum migration rate MR of metal ions in storage container A and storage container B under this extraction condition i(max) , as shown in Table 8

[0109] Table 8

[0110]

[0111] Calculate the maximum migration amount Q of metal ions in storage containers of the same material but different specifications and sizes during the storage of photosensitive materials under the same temperature and extraction conditions i(max) :

[0112] Use the same raw materials as storage container A and storage container B to prepare 4L storage container A' and storage container B' respectively, and predict the maximum migration amount Q of metal ions in photosensitive material (PM - X) after storing in storage container A' and storage container B' for 180 days i(max) .

[0113] First, it is measured that the inner radii of storage container A' and storage container B' are both 1.62 dm, the cylindrical heights are both 1.91 dm, and the contact areas of the photosensitive material with the inner walls of storage container A' and storage container B' during full - capacity storage are 11.78 dm 2 , and the prediction results of the maximum migration amounts of metal ions in storage container A' and storage container B' are shown in Table 9

[0114] Table 9

[0115]

[0116] There are differences in the maximum migration amounts obtained by storing different extractants in the same storage containers in Example 1 and Example 2. In actual use, different photosensitive materials should be stored in storage containers that meet the compatibility requirements. The method provided by this patent can provide a guiding role for selecting suitable storage containers for photosensitive materials to reduce the migration of metal ions to photosensitive materials

[0117] Finally, it should be noted that the above-described embodiments are only specific embodiments of the present invention, used to illustrate the technical solutions of the present invention, rather than limiting it. The protection scope of the present invention is not limited thereto. Although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that any person skilled in the art within the technical scope disclosed by the present invention can still modify the technical solutions described in the foregoing embodiments, or can easily think of changes, or perform equivalent replacements on some of the technical features; and these modifications, changes or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention, and should all be covered within the protection scope of the present invention.

Claims

1. A method for predicting the maximum migration amount of metal ions in a photosensitive material storage container, characterized in that: The following steps are involved: S1. Add a certain volume of extractant to the storage container to be tested, seal the mouth of the storage container to be tested, and calculate the contact ratio K, which is the ratio of the contact area S between the extractant and the storage container to be tested to the volume V of the extractant; S2, placing the storage container to be tested containing the extractant at a set temperature, and subjecting the storage container to be tested containing the extractant to mechanical vibration and / or ultrasonic vibration extraction; S3, drawing a set amount of extract from the storage container to be tested at a set time interval, and adding an equal amount of extractant to the storage container to be tested after drawing the extract each time; S4, obtaining the concentration of metal ions in the extract each time, and establishing a metal ion concentration-time curve; S5. Calculate the first-order differential of the concentration of metal ions with respect to time for each measured concentration of metal ions in the extract and the corresponding time, i.e., dc i / dt; take the maximum value from the first-order differential calculation result, that is, (dc i / dt) max ; S6. Calculate the maximum migration rate of metal ions in the storage container under the extraction conditions according to the following formula: ； Where: MR i(max) is the maximum migration rate of metal ion i; S7. Calculate the maximum migration amount of metal ions in storage containers of the same material and different specifications and sizes during storage of photosensitive materials under the same extraction conditions according to the following formula: MR i(max) ×A×t; Where: Q i(max) is the maximum migration amount of metal ion i; A is the contact area between the photosensitive material and the inner wall of the storage container; t is the storage time.

2. The method for predicting the maximum migration amount of metal ions in a photosensitive material storage container according to claim 1, characterized in that: In step S1, the extractant is propylene glycol methyl ether acetate or a specific type of photosensitive material, and the specific type of photosensitive material is the material planned to be contained in the storage container.

3. The method for predicting the maximum migration amount of metal ions in a photosensitive material storage container according to claim 1, characterized in that: In step S2, a storage container to be tested containing an extractant is placed in a medium tank (1), and the storage container to be tested is fixed by a fixture (2); a medium (3) is injected into the medium tank (1); under the joint action of a heater (4), a cooler (5), a temperature sensor (6) and a circulation pump (7), the medium (3) in the medium tank (1) and the extractant in the container to be tested are maintained at a set temperature; under the action of a mechanical oscillator (8), the container to be tested is subjected to mechanical oscillation; an ultrasonic generator (9) performs ultrasonic oscillation on the container to be tested and the extractant therein; and a control system (10) is respectively connected to the heater (4), the cooler (5), the mechanical oscillator (8), the ultrasonic generator (9), the temperature sensor (6) and the circulation pump (7) for setting temperature, oscillation mode, oscillation frequency, extraction time parameters and on / off control of the device.

4. The method for predicting the maximum migration amount of metal ions in a photosensitive material storage container according to claim 3, characterized in that: The medium (3) is one of water, ethylene glycol, and a water / ethylene glycol mixture.

5. The method for predicting the maximum migration amount of metal ions in a photosensitive material storage container according to claim 1, characterized in that: In step S3, the time interval is set to 1 day, or 5 days, or 7 days, and the set amount of the extract to be absorbed each time is 1-5 mL.

6. The method for predicting the maximum migration amount of metal ions in a photosensitive material storage container according to claim 1, characterized in that: The concentration of metal ions in the extracted solution each time is obtained by inductively coupled plasma-mass spectrometry analysis; specifically, the following steps are included: S41. Preparation of a series of standard solutions: Take 5.0 mL of 1.0 mg / L metal ion mixed standard solution, place it in a volumetric flask, dilute to 100 mL with 2% nitric acid solution, and prepare a mixed standard solution A with a mass concentration of 50.00 μg / L; take 10.0 mL of mixed standard solution A and dilute to 100 mL with 2% nitric acid solution, and prepare a mixed standard solution B with a mass concentration of 5.00 μg / L; take 0, 1.0 mL, 2.0 mL, 4.0 mL, and 10.0 mL of mixed standard solution B, place them in 5 volumetric flasks, dilute to 100 mL with N-methylpyrrolidone, and prepare a series of mixed standard solutions with concentrations of 0, 50.0 ng / L, 100.0 ng / L, 200.0 ng / L, and 500.0 ng / L, respectively; the volumetric flask is made of tetrafluoroethylene perfluoroalkoxy copolymer; S42, drawing a calibration curve: using an inductively coupled plasma-mass spectrometer, measuring the signal intensity of each metal ion in a mixed standard solution of metal ions with different concentrations, and drawing a standard curve with the concentration as the abscissa and the response value as the ordinate; S43. Using an inductively coupled plasma-mass spectrometer to measure the extract, obtain the signal intensity of the metal ion to be measured in the extract, substitute it into the standard curve of the metal ion, and obtain the concentration of the metal ion to be measured.

7. The method for predicting the maximum migration amount of metal ions in a photosensitive material storage container according to claim 6, characterized in that: The concentration of metal ions in each extracted solution was obtained by inductively coupled plasma-mass spectrometry analysis. The specific analysis conditions were as follows: The RF power was 1400-1600 W, the plasma gas flow rate was 15-20 L / min, the argon auxiliary gas flow rate was 1.0-1.4 L / min, the argon carrier gas flow rate was 0.7-0.8 L / min, and the vacuum degree of the analysis chamber was 0.9×10 -6 ~1.1×10 -6 , the pulse voltage is 800~1000V; The conditions of the organic injection system are: oxygen flow rate of 7-9 mL / min and temperature of 2-4 °C.

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