CN114184445A - Method for measuring content of residual metal elements in OLED material - Google Patents
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Abstract
The invention discloses a method for measuring the content of residual metal elements in an OLED material, which is a pretreatment method of extracting a sample by using an organic solvent and carrying out acidification ultrasonic extraction, and a single-quadrupole inductively coupled plasma mass spectrometer provided with an organic sample introduction system is used for detection. Compared with the conventional dry digestion and acid digestion pretreatment method, the method has the characteristics of rapid pretreatment, less process interference, low detection limit, small background blank, good precision, high accuracy and friendly operation environment.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a method for determining the content of residual metal elements in an OLED material.
Background
The organic light emitting diode display is widely applied to daily life, such as smart phones, flat panels, televisions, vehicle-mounted displays and the like, by virtue of the advantages of self luminescence, low power consumption, wide viewing angle, high contrast, high response speed, mild to human eyes and the like.
The residual metal element refers to an inorganic substance which cannot be completely removed in the production process, the content of the residual metal element is an important control index in the quality standard of the OLED material, and the residual metal forms a non-radiative transition recombination center in a light-emitting region, namely a light-emitting trap, so that the stability of a device is influenced, even the device is failed, and the industrial application of the material is influenced.
For the detection method of residual metal elements, the existing national standards and documents are commonly found in the fields of medicines, foods, toys and the like, and the used method mainly adopts devices such as atomic absorption spectroscopy, an inductively coupled plasma spectrometer, an inductively coupled plasma mass spectrometer and the like for detection through a pretreatment mode of dry method and acid digestion.
For the determination of the metal elements in the OLED material, the cited standard is only the general rule of the inductively coupled plasma mass spectrometry of SJ/T11637-2016 electronic chemicals, and the method is also the only reference standard method for testing the content of the metal elements in the OLED material so far. However, in practical applications, it is found that the description of the aspects of reagent selection, sample preparation and processing is ambiguous, and the OLED material can be tested by completely complying with the standard method, and an inaccurate or low-reproducibility detection result can be given. The detection is the eye of raw material management, product research and development, production control and final product quality control, a detection result capable of reflecting the objective fact of things plays a positive role in research and development and production activities, and a detection result with a problem can make wrong judgment, so that the brought consequences are disastrous.
Disclosure of Invention
In view of the above-mentioned needs in the art, the present invention provides a method for determining the content of residual metal elements in an OLED material; the detection method disclosed by the invention is simple to operate, the detected result reflects the objective essence of the object, and the detection method has a positive effect on the quality evaluation of the material and better guides the production activity.
A method for determining the content of residual metal elements in an OLED material comprises the following steps:
(1) and preparing a standard solution:
1) the mixed multi-element standard solution mother liquor with gradient concentration is prepared by using a nitric acid solution as a solvent for 24 multi-element standard solutions 1 and 9 multi-element standard solutions 2,
2) preparing an internal standard solution from a multi-element standard solution 3 containing Ge, In, Re, Rh, Sc and Y by using a nitric acid solution as a solvent;
3) respectively taking X mul from mixed multi-element standard solution mother liquor with gradient concentration, adding the X mul into different PFA sample tanks, and respectively adding Y mul of internal standard solution; finally NMP was added to the PFA sample tank to bring the mass of the solution to m1Preparing mixed multi-element standard solution with gradient concentration;
(2) preparation of sample solution to be measured
a) Weighing sample m0g into a PFA sample canister;
b) adding Y mu l of the internal standard solution obtained in the step 2);
c) quantitatively preparing a sample: adding NMP into a PFA sample tank weighed with a sample and added with an internal standard until the total solid-liquid mass is m1g, screwing a thread sealing cover for sealing;
d) extracting metal elements: placing the sealed PFA sample tank in a water bath for ultrasonic extraction for 30min, and taking out the sample liquid to be detected after the sample liquid is clarified and transparent through visual observation;
(3) preparation of blank solution
Except that the step of weighing the sample is reduced, the steps are consistent with the step (2).
(4) And sample detection
An inductively coupled plasma mass spectrometer using an organic sampling system adopts an organic sampling mode, uses argon as carrier gas, oxygen as reaction gas and helium as collision gas, is matched with the organic sampling system, sequentially samples and analyzes mixed multi-element standard solution with gradient concentration from low to high, corrects the response value of an element to be detected according to the ratio of an internal standard value of an internal standard element to be actually measured to an expected value, obtains a standard curve by a least square method, obtains the standard curve, and obtains a linear R2Respectively testing blank and sample to-be-tested solutions, wherein the number of the blank and the sample to-be-tested solutions is more than or equal to 0.999; calculating the concentration of the metal element in the sample liquid to be detected according to the standard curve of the metal element to be detected;
(5) and the calculation formula of the metal element content is as follows:
Xi: metal element content of OLED Material, μ g/kg
Ci: the concentration of the element i in the sample solution to be tested, mu g/kg
C0: the concentration of the element i in the blank solution to be tested is mu g/kg
m0: weighed mass of solid sample, g
m1: the weighed mass of the solution to be tested, g.
The concentrations of the multi-element standard solutions 1, 2 and 3 are 1000 mug/ml, the solvent is a 10% nitric acid solution, the concentration of the internal standard solution is 2 mug/ml, the multi-standard solution 1 and the multi-element standard solution 2 in the step 1) are the most identical, and the concentrations of the mixed multi-element standard solutions with gradient concentrations are respectively as follows: 0.1, 0.5, 1, 5, 10, 50 mug/kg.
The X mu l is 100 mu l, and the Y mu l is 100 mu l; m is0g is 0.1g, m1g is 10g, to the nearest 0.0001 g.
The preparation method of the internal standard solution comprises the following steps: sucking 1ml to 50ml of PFA volumetric flask from the Ge, In, Re, Rh, Sc and Y multi-element standard solution, and using 10% nitric acid to fix the volume to obtain 2 mu g/ml of Ge, In, Re, Rh, Sc and Y multi-element standard solution mother liquor as an internal standard solution.
The preparation method of the gradient concentration mixed multi-element standard solution comprises the following steps: respectively sucking 0.5ml to 50ml of PFA volumetric flasks from the multi-element standard solution 1 and the multi-element standard solution 2, fixing the volume with 10% nitric acid to obtain 10 mu g/ml mixed multi-element standard solution, respectively sucking 0.5ml, 2.5ml, 5ml and 25ml to 4 different 50ml PFA volumetric flasks from the 10 mu g/ml mixed multi-element standard solution, fixing the volume with 10% nitric acid to obtain 0.1 mu g/ml, 0.5 mu g/ml, 1 mu g/ml and 5 mu g/ml mixed multi-element standard solution mother liquor, respectively sucking 0.5ml to 2 different 50ml PFA volumetric flasks from 1 mu g/ml and 5 mu g/ml mixed multi-element standard solution mother liquor, fixing the volume with 10% nitric acid to obtain 0.01 mu g/ml and 0.05 mu g/ml mixed multi-element standard solution mother liquor; from the mixed multi-element standard solution mother liquor of 0.01 mu g/ml, 0.05 mu g/ml, 0.1 mu g/ml, 0.5 mu g/ml, 1 mu g/ml and 5 mu g/ml, 100 mu l of each of the mixed multi-element standard solution mother liquor is taken to different PFA sample tanks, meanwhile, 100 mu l of the mixed multi-element standard solution mother liquor of 2 mu g/ml of Ge, In, Re, Rh, Sc and Y is added to each PFA sample tank, and finally NMP is added to the PFA sample tank to reach 10g, so as to prepare the mixed multi-element standard solution with 6 gradient concentrations of 0.1, 0.5, 1, 5, 10 and 50 mu g/kg.
The multi-element standard solution 1 contains metal elements such As Al, As, B, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, Se, Sr, V and Zn.
The metal elements contained in the multielement standard solution 2: mo, Pd, Re, S, Sb, Si, Sn, Ti and W.
The PFA sample canister must be subjected to a cleaning step before use, the cleaning step being: soaking the PFA sample tank in a 30% nitric acid cylinder for not less than 24 h; after soaking, repeatedly washing the container by ultrapure water with the volume not less than 10 times of the container, and eluting residual metal elements on the surface of the container.
According to the invention, the OLED material main body is extracted by adopting an organic solvent to form a homogeneous solution, the metal elements remained in the material are further fully extracted in an acidic environment and an ultrasonic condition, and are directly subjected to sample injection detection by matching with an organic sample injection system. In the selection of the pretreatment reagent, the organic solvent selected by the invention is N-methylpyrrolidone (marked by NMP in the text), and the advantages are that:
1) the commercial product has high purity and has metal element concentration of less than 1ppb
1) The saturated vapor pressure is about 0.04kPa at 20 ℃, the volatilization is slow, the loss is less and the quantification is accurate in the liquid adding quantification process;
2) the relative density is close to that of water, the water-soluble trace metal complex can be mutually dissolved in any proportion, even in the presence of an acidic medium, a sample obtained by pretreatment is uniform, the layering phenomenon cannot occur, the trace metal elements are further ensured to be fully extracted in an acidic environment, the toxicity is low, a large amount of concentrated acid tail gas is not generated, and the operation environment is relatively friendly.
The invention adopts a pretreatment method of extracting a sample by an organic solvent NMP and nitric acid acidification ultrasonic extraction, and uses a single quadrupole inductively coupled plasma mass spectrometer with an organic sample introduction system for detection. Compared with the conventional dry digestion and acid digestion pretreatment method, the method has the characteristics of rapid pretreatment, less process interference, low detection limit, small background blank, good precision, high accuracy and friendly operation environment.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying specific embodiments, in which some, but not all embodiments of the invention are shown. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention.
The standard solutions used are all commercially available
24 kinds of multi-element standard solutions 1 (brand: SPEX Certiprep, number: XNEF-54, concentration: 1000. mu.g/ml) containing metal elements of Al, As, B, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, Se, Sr, V, Zn.
9 kinds of multielement standard solution 2 (brand: SPEX Certiprep, number: XNEF-55C, concentration: 1000. mu.g/ml) multielement standard solution 2 contains metal elements: mo, Pd, Re, S, Sb, Si, Sn, Ti and W.
Ge, In, Re, Rh, Sc and Y multi-element standard solution 3 (brand: national nonferrous metals and electronic materials analysis and test center, number: GNM-M062079-2013, concentration: 1000. mu.g/ml), the multi-element standard solution 3 contains metal elements: ge, In, Re, Rh, Sc, Y, are used as internal standard elements In this application.
Example 1
The first step is as follows: preparation of standard solution:
sucking 1ml to 50ml of PFA volumetric flask from the Ge, In, Re, Rh, Sc and Y multi-element standard solution 3, and using 10% nitric acid to fix the volume to obtain 2 mu g/ml of Ge, In, Re, Rh, Sc and Y multi-element standard solution mother liquor as an internal standard solution;
respectively sucking 0.5ml to 50ml of PFA volumetric flasks from the multi-element standard solution 1 and the multi-element standard solution 2, fixing the volume with 10% nitric acid to obtain 10 mu g/ml mixed multi-element standard solution, respectively sucking 0.5ml, 2.5ml, 5ml and 25ml to 4 different 50ml PFA volumetric flasks from the 10 mu g/ml mixed multi-element standard solution, fixing the volume with 10% nitric acid to obtain 0.1 mu g/ml, 0.5 mu g/ml, 1 mu g/ml and 5 mu g/ml mixed multi-element standard solution mother liquor, respectively sucking 0.5ml to 2 different 50ml PFA volumetric flasks from 1 mu g/ml and 5 mu g/ml mixed multi-element standard solution mother liquor, fixing the volume with 10% nitric acid to obtain 0.01 mu g/ml and 0.05 mu g/ml mixed multi-element standard solution mother liquor;
taking 100 mu l of mixed multi-element standard solution mother liquor of 0.01 mu g/ml, 0.05 mu g/ml, 0.1 mu g/ml, 0.5 mu g/ml, 1 mu g/ml and 5 mu g/ml into different PFA sample tanks, simultaneously adding 100 mu l of mixed multi-element standard solution mother liquor of 2 mu g/ml Ge, In, Re, Rh, Sc and Y into each PFA sample tank, finally adding NMP into the PFA sample tank until the mass of the solution reaches 10g to prepare mixed multi-element standard solution with 6 gradient concentrations of 0.1, 0.5, 1, 5, 10 and 50 mu g/kg, and after the preparation, carrying out sample injection analysis from low to high In sequence, obtaining a standard curve by a least square method, R2≥0.999；
The second step is that: the sample pretreatment method comprises the following steps:
1) the PFA sample tank is soaked in a 30% nitric acid cylinder in advance, and the soaking time is not less than 24 hours; after soaking, repeatedly washing the container by ultrapure water with the volume not less than 10 times that of the container, and eluting residual metal elements on the surface of the container;
2) weighing: weigh sample 0.1g (to the nearest 0.0001g) into a PFA sample canister and record the weighed mass m0；
3) Adding an internal standard: sucking 100 mul from 2 mug/ml internal standard solution and adding into a PFA sample tank weighed with samples;
4) quantitatively preparing a sample: adding NMP into a PFA sample tank weighed with a sample and added with an internal standard until the total solid-liquid mass is 10g, and recording the weighed mass m1Screwing a thread sealing cover for sealing;
5) extracting metal elements: and (3) placing the PFA sample tank which is prepared quantitatively and sealed in a water bath for ultrasonic extraction for 30min, and taking out the PFA sample tank to be detected after the sample liquid is clarified and transparent through visual observation.
The third step: the preparation and treatment links of the blank solution are only reduced by the link 2) of sample weighing, and the rest is consistent with the second step.
The fourth step: sample detection
An inductively coupled plasma mass spectrometer using an organic sampling system adopts an organic sampling mode, uses argon as carrier gas, oxygen as reaction gas and helium as collision gas, is matched with the organic sampling system, sequentially samples and analyzes 6 gradient concentration mixed multi-element standard solutions of 0.1, 0.5, 1, 5, 10 and 50 mu g/kg, corrects the response value of an element to be detected according to the ratio of an internal standard value of an actually measured internal standard element to an expected value, obtains a standard curve through a least square method, and obtains a standard curve linear R2Respectively testing blank and sample to-be-tested solutions, wherein the number of the blank and the sample to-be-tested solutions is more than or equal to 0.999; calculating the concentration of the metal elements in the sample liquid to be detected according to the standard curve of the metal elements to be detected; .
The fifth step: the calculation formula of the content of the metal elements is as follows:
Xi: metal element content of OLED Material, μ g/kg
Ci: the concentration of the element i in the sample solution to be tested, mu g/kg
C0: the concentration of the element i in the blank solution to be tested is mu g/kg
m0: weighed mass of solid sample, g
m1: weight of liquid to be measured, g
Through calculation, the sample to be tested in the embodiment contains 9 metal elements, the content of which is shown in table 1 below, meets the requirement of appendix B.1 in GB/T27417 and 2017 qualification chemical analysis method confirmation and verification guideline on the variation coefficient of the laboratory, and shows that the result is accurate.
TABLE 1 test results of the content of metallic elements (μ g/kg) of the samples
The blank test of 11 samples was carried out consecutively, and the detection limit of the test method was 2ppm below the conventional detection limit of international standard IEC-62321-5 by calculating the 3-fold standard deviation of the test results, as shown in table 2 below:
TABLE 211 detection limits (μ g/kg) obtained from blank test results
And simultaneously preparing 6 sample blanks, preparing blank samples, and respectively testing the metal element concentrations of the blank samples under the condition of the same standard curve to obtain blank test results shown in the table 3, wherein the blank results are all less than 1 mu g/kg, and the range difference between the blanks is less than 1 mu g/kg, which shows that no difference exists among different PFA sample tanks after being cleaned, and the blank background is stable.
TABLE 36 sample blank test results (μ g/kg)
15 parallel OLED material samples are prepared from batch samples, wherein one sample is used as an original sample, and the other 14 samples are subjected to 7 parallel results of parallel standard adding tests (standard adding concentrations are 2000 mug/kg and 1000 mug/kg), the relative standard deviation and the standard adding recovery rate of the test results are calculated, as shown in Table 4, the average recovery rate of each element standard adding sample is 86-102%, the method is high in accuracy, the relative standard deviation RSD is 0.4-4.5%, the metal elements are high in precision, and the precision and the accuracy simultaneously indicate that the sample pretreatment method is reliable, the method is accurate, and the result consistency is good.
TABLE 4 relative standard deviation and recovery of spiked samples
3 gradient standard-adding samples are prepared from batch samples, the concentrations are respectively 100 mug/kg, 200 mug/kg and 500 mug/kg, the test is carried out once every 3 hours, the test result is shown in the following table 5, the average recovery rate is 92% -111% as seen from the table, the stability change of the same gradient sample at the interval of 9 hours is recorded, the RSD is less than 5%, the sample is considered to be basically not changed after being placed for 9 hours, and the long-term stability of the sample is considered to be good.
TABLE 53 results of variation of the gradient-labeled samples over 9 hours (3 h intervals)
Compared with the conventional dry digestion and acid digestion pretreatment method, the method has the characteristics of rapid pretreatment, less process interference, low detection limit, small background blank, good precision, high accuracy and environment-friendly operation.
Claims (8)
1. A method for determining the content of residual metal elements in an OLED material comprises the following steps:
(1) and preparing a standard solution:
1) the mixed multi-element standard solution mother liquor with gradient concentration is prepared by using a nitric acid solution as a solvent for 24 multi-element standard solutions 1 and 9 multi-element standard solutions 2,
2) preparing an internal standard solution from a multi-element standard solution 3 containing Ge, In, Re, Rh, Sc and Y by using a nitric acid solution as a solvent;
3) adding X mu l of mixed multi-element standard solution mother liquor with gradient concentration into different PFA sample tanks respectively, and adding into the PFA sample tanksRespectively adding Y mul of internal standard solution; finally NMP was added to the PFA sample tank to bring the mass of the solution to m1Preparing mixed multi-element standard solution with gradient concentration;
(2) preparation of sample solution to be measured
a) Weighing sample m0g into a PFA sample canister;
b) adding Y mu l of the internal standard solution obtained in the step 2);
c) quantitatively preparing a sample: adding NMP into a PFA sample tank weighed with a sample and added with an internal standard until the total solid-liquid mass is m1g, screwing a thread sealing cover for sealing;
d) extracting metal elements: placing the sealed PFA sample tank in a water bath for ultrasonic extraction for 30min, and taking out the sample liquid to be detected after the sample liquid is clarified and transparent through visual observation;
(3) preparation of blank solution
Except that the step of weighing the sample is reduced, the steps are consistent with the step (2);
(4) and sample detection
An inductively coupled plasma mass spectrometer using an organic sampling system adopts an organic sampling mode, uses argon as carrier gas, oxygen as reaction gas and helium as collision gas, is matched with the organic sampling system, sequentially samples and analyzes mixed multi-element standard solution with gradient concentration from low to high, corrects the response value of an element to be detected according to the ratio of an internal standard value of an internal standard element to be actually measured to an expected value, obtains a standard curve by a least square method, obtains the standard curve, and obtains a linear R2Respectively testing blank and sample to-be-tested solutions, wherein the number of the blank and the sample to-be-tested solutions is more than or equal to 0.999; calculating the concentration of the metal element in the sample liquid to be detected according to the standard curve of the metal element to be detected;
(5) and the calculation formula of the metal element content is as follows:
Xi: metal element content of OLED Material, μ g/kg
Ci: the concentration of the element i in the sample solution to be tested, mu g/kg
C0: the concentration of the element i in the blank solution to be tested is mu g/kg
m0: weighed mass of solid sample, g
m1: the weighed mass of the solution to be tested, g.
2. The method according to claim 1, wherein the multi-element standard solution 1, 2, 3 has a concentration of 1000 μ g/ml, the solvent is 10% nitric acid solution, the internal standard solution has a concentration of 2 μ g/ml, the multi-standard solution 1 in step 1) and the multi-element standard solution 2 are the most identical, and the concentrations of the mixed multi-element standard solution with gradient concentration are respectively as follows: 0.1, 0.5, 1, 5, 10, 50 mug/kg.
3. The method of claim 2, wherein said X μ Ι is 100 μ Ι and said Y μ Ι is 100 μ Ι; m is0g is 0.1g, m1g is 10g, to the nearest 0.0001 g.
4. The method of claim 3, wherein the internal standard solution is prepared by the following steps: sucking 1ml to 50ml of PFA volumetric flask from the Ge, In, Re, Rh, Sc and Y multi-element standard solution, and using 10% nitric acid to fix the volume to obtain 2 mu g/ml of Ge, In, Re, Rh, Sc and Y multi-element standard solution mother liquor as an internal standard solution.
5. The method of claim 4, wherein the gradient concentration mixed multi-element standard solution is prepared by the following method: respectively sucking 0.5ml to 50ml of PFA volumetric flasks from the multi-element standard solution 1 and the multi-element standard solution 2, fixing the volume with 10% nitric acid to obtain 10 mu g/ml mixed multi-element standard solution, respectively sucking 0.5ml, 2.5ml, 5ml and 25ml to 4 different 50ml PFA volumetric flasks from the 10 mu g/ml mixed multi-element standard solution, fixing the volume with 10% nitric acid to obtain 0.1 mu g/ml, 0.5 mu g/ml, 1 mu g/ml and 5 mu g/ml mixed multi-element standard solution mother liquor, respectively sucking 0.5ml to 2 different 50ml PFA volumetric flasks from 1 mu g/ml and 5 mu g/ml mixed multi-element standard solution mother liquor, fixing the volume with 10% nitric acid to obtain 0.01 mu g/ml and 0.05 mu g/ml mixed multi-element standard solution mother liquor; from the mixed multi-element standard solution mother liquor of 0.01 mu g/ml, 0.05 mu g/ml, 0.1 mu g/ml, 0.5 mu g/ml, 1 mu g/ml and 5 mu g/ml, 100 mu l of each of the mixed multi-element standard solution mother liquor is taken to different PFA sample tanks, meanwhile, 100 mu l of the mixed multi-element standard solution mother liquor of 2 mu g/ml of Ge, In, Re, Rh, Sc and Y is added to each PFA sample tank, and finally NMP is added to the PFA sample tank to reach 10g, so as to prepare the mixed multi-element standard solution with 6 gradient concentrations of 0.1, 0.5, 1, 5, 10 and 50 mu g/kg.
6. The method according to claim 1, wherein the multi-element standard solution 1 contains metal elements selected from the group consisting of Al, As, B, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, Se, Sr, V, and Zn.
7. The method according to claim 1, wherein the metallic elements contained in the multielement standard solution 2 are: mo, Pd, Re, S, Sb, Si, Sn, Ti and W.
8. The method of any of claims 1-7, wherein the PFA sample canister must be subjected to a purging step prior to use, the purging step comprising: soaking the PFA sample tank in a 30% nitric acid cylinder for not less than 24 h; after soaking, repeatedly washing the container by ultrapure water with the volume not less than 10 times of the container, and eluting residual metal elements on the surface of the container.
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