CN114184445B - Method for measuring content of residual metal element in OLED material - Google Patents
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Abstract
The application discloses a method for measuring the content of residual metal elements in an OLED material, in particular to a pretreatment method for extracting a sample by adopting an organic solvent and acidizing ultrasonic extraction, and a single four-stage rod inductively coupled plasma mass spectrometer equipped with an organic sample injection system is used for detection. Compared with the conventional dry digestion and acid digestion pretreatment method, the pretreatment method has the characteristics of rapid pretreatment, less process interference, low detection limit, small background blank, good precision, high accuracy and environment-friendly operation.
Description
Technical Field
The application belongs to the technical field of detection, and particularly relates to a method for measuring the content of residual metal elements in an OLED material.
Background
The organic light emitting diode display is widely applied in daily life, such as smart phones, flat panel, 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 is an inorganic substance which cannot be completely removed in the production process, and in the quality standard of the OLED material, the content of the residual metal element is an important control index, and the residual metal forms a non-radiative transition recombination center in a light-emitting area, namely a light-emitting trap, so that the stability of a device is influenced, even the device is invalid, and the industrialized application of the material is influenced.
For the detection method of the residual metal element, the existing national standard and literature are mostly found in the fields of medicines, foods, toys and the like, and the method mainly adopts a pretreatment mode of digestion by a dry method and an acid method, and adopts equipment such as an atomic absorption spectrum, an inductive coupling plasma spectrometer, an inductive coupling plasma mass spectrometer and the like for detection.
For the determination of metal elements in the OLED material, the cited standard is only SJ/T11637-2016 electronic chemical inductively coupled plasma mass spectrometry, and the method is the only standard method capable of being referenced so far for testing the content of the metal elements in the OLED material. However, in practical applications, it is found that the method of fully carrying out the test on the OLED material according to the standard method may give an inaccurate or poorly reproducible detection result. The detection is eyes for raw material management, product research and development, production control and final product quality control, and a detection result capable of reflecting objective facts of things can play a positive role in research and production activities, and a problematic detection result can enable people to make wrong judgment, so that the brought results are often catastrophic.
Disclosure of Invention
In view of the above-mentioned needs in the art, the present application provides a method for determining the content of residual metal elements in an OLED material; the detection method is simple to operate, the measured result reflects the objective nature of things, and the detection method has positive effects on quality evaluation of materials and better guides production activities.
A method for determining the content of residual metallic elements in an OLED material, comprising the steps of:
(1) Preparing a standard solution:
1) The 24 multi-element standard solutions 1 and 9 multi-element standard solutions 2 are prepared into mixed multi-element standard solution mother solution with gradient concentration by using nitric acid solution as solvent,
2) The multi-element standard solution 3 of Ge, in, re, rh, sc and Y is prepared into an internal standard solution by using a nitric acid solution as a solvent;
3) Taking X mul of mixed multi-element standard solution mother liquor with gradient concentration, adding the X mul of mixed multi-element standard solution mother liquor into different PFA sample tanks, and respectively adding Y mul of internal standard solution; finally NMP is added into the PFA sample tank to lead the mass of the solution to m 1 Preparing a mixed multi-element standard solution with gradient concentration;
(2) Preparation of sample liquid to be tested
a) Sample m 0 g, into a PFA sample tank;
b) Adding Y μl of the internal standard solution in the step 2);
c) Sample quantitative preparation: NMP is added into a PFA sample tank which is weighed with a sample and added with an internal standard until the total solid-liquid mass is m 1 g, screwing a threaded sealing cover for sealing;
d) Extracting metal elements: placing the sealed PFA sample tank in a water bath, performing ultrasonic treatment for 30min for extraction, and taking out the PFA sample tank to be detected after macroscopic observation of the sample liquid is transferred to be clear and transparent;
(3) Preparing blank solution
Except for reducing the links of weighing the sample, the steps are identical to the step (2).
(4) Sample detection
An inductively coupled plasma mass spectrometer using an organic sample injection system adopts an organic sample injection mode, argon is used as carrier gas, oxygen is used as reaction gas, helium is used as collision gas, the organic sample injection system is matched, mixed multi-element standard solution with gradient concentration is sequentially subjected to sample injection analysis from low to high, the response value of an element to be measured is corrected according to the ratio of the internal standard value of an actually measured internal standard element to an expected value, a standard curve is obtained through a least square method, and a standard curve and linear R are obtained 2 More than or equal to 0.999, respectively testing blank and sample to-be-tested liquid; 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 calculating a formula of metal element content:
X i : metal element content of OLED material, mug/kg
C i : the concentration of the element i in the sample to be measured, mug/kg
C 0 : concentration of the element i in blank liquid to be measured, mug/kg
m 0 : weighing mass of solid sample g
m 1 : and g, weighing mass of the liquid to be measured.
The concentrations of the multi-element standard solutions 1, 2 and 3 are 1000 mug/ml, the solvent is 10% nitric acid solution, the concentration of the internal standard solution is 2 mug/ml, the multi-standard solution 1 in the step 1) is the same as the multi-element standard solution 2, 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. Mu.g/kg.
The X μl is 100 μl, and the Y μl is 100 μl; m is m 0 g is 0.1g, m 1 The g is 10g, and the accuracy is 0.0001g.
The preparation method of the internal standard solution comprises the following steps: and sucking 1ml to 50ml 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 mug/ml Ge, in, re, rh, sc and Y multi-element standard solution mother solution as an internal standard solution.
The preparation method of the mixed multi-element standard solution with gradient concentration comprises the following steps: respectively sucking 0.5ml to 50ml PFA volumetric flasks from the multielement standard solution 1 and the multielement standard solution 2, fixing the volume by 10% nitric acid to obtain 10 mug/ml mixed multielement standard solution, respectively sucking 0.5ml, 2.5ml, 5ml and 25ml to 4 different 50ml PFA volumetric flasks from the 10 mug/ml mixed multielement standard solution, fixing the volume by 10% nitric acid to obtain 0.1 mug/ml, 0.5 mug/ml, 1 mug/ml and 5 mug/ml mixed multielement standard solution mother solution, respectively sucking 0.5ml to 2 different 50ml PFA volumetric flasks from the 1 mug/ml mixed multielement standard solution mother solution and fixing the volume by 10% nitric acid to obtain 0.01 mug/ml and 0.05 mug/ml mixed multielement standard solution mother solution; 100. Mu.l of each mixed multi-element standard solution mother solution from 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 are taken into different PFA sample tanks, meanwhile 100. Mu.l of 2. Mu.g/ml Ge, in, re, rh, sc and Y multi-element standard solution mother solution are added into each PFA sample tank, and finally NMP is added into the mixed multi-element standard solution with 6 gradient concentrations of the solutions In the PFA sample tanks to 10g so as to prepare the mixed multi-element standard solution with 0.1, 0.5, 1, 5, 10 and 50. Mu.g/kg.
The multi-element standard solution 1 contains metal elements Al, as, B, ba, be, bi, ca, cd, co, cr, cu, fe, K, li, mg, mn, na, ni, P, pb, se, sr, V, zn.
The multi-element standard solution 2 contains metal elements: mo, pd, re, S, sb, si, sn, ti, W.
The PFA sample tank must be subjected to a cleaning step before use, wherein the cleaning step is as follows: soaking the PFA sample tank in a 30% nitric acid tank for not less than 24 hours; repeatedly washing the container with at least 10 times of ultrapure water after soaking, and eluting the residual metal elements on the surface of the container.
According to the application, the organic solvent is adopted to extract the OLED material main body to form a homogeneous solution, the metal elements remained in the material are further fully extracted under the acidic environment and the ultrasonic condition, and the organic solvent is directly sampled and detected through the organic sampling system, so that compared with the dry digestion and acid digestion methods, the organic solvent used as the material main body is fully combusted and cracked and eliminated in the aerobic environment in the plasma, and microwave high-pressure heating or high-risk operation conditions such as concentrated sulfuric acid, hydrofluoric acid, perchloric acid and the like are not required, and the organic solvent has the advantages of rapid pretreatment and less process interference. In the selection of the pretreatment reagent, the organic solvent selected in the application is N-methyl pyrrolidone (marked by NMP), and the method has the advantages that:
1) The commercial product has high purity and 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 quantitative liquid adding process;
2) The relative density is close to that of water, the sample obtained by pretreatment can be mutually dissolved with water in any proportion, even if an acidic medium exists, the sample is uniform, layering phenomenon can not occur, trace metal elements are further ensured to be fully extracted in an acidic environment, the toxicity is low, no large amount of concentrated acid tail gas is generated, and the operation environment is relatively friendly.
According to the pretreatment method, an organic solvent NMP is adopted to extract a sample, and the single four-stage rod inductive coupling plasma mass spectrometer equipped with an organic sample injection system is used for detection. Compared with the conventional dry digestion and acid digestion pretreatment method, the pretreatment method has the characteristics of rapid pretreatment, less process interference, low detection limit, small background blank, good precision, high accuracy and environment-friendly operation.
Detailed Description
The present application will be further described more fully hereinafter with reference to the accompanying drawings, in which some, but not all embodiments of the application are shown. All other embodiments obtained by those skilled in the art without making any inventive effort are within the scope of the present application.
The standard solutions used are all commercially available
24 kinds of multi-element standard solutions 1 (brand: SPEX Certifrep, number: XNEF-54, concentration: 1000. Mu.g/ml), the multi-element standard solutions 1 contained metal element: 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 multi-element standard solutions 2 (brand: SPEX Certiprep, number: XNEF-55C, concentration: 1000. Mu.g/ml) the multi-element standard solution 2 contains metallic elements: mo, pd, re, S, sb, si, sn, ti, W.
Ge, in, re, rh, sc and Y multi-element standard solution 3 (brand: national non-ferrous metal and electronic material 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 the present application.
Example 1
The first step: preparation of standard solution:
sucking 1ml to 50ml of PFA volumetric flask from Ge, in, re, rh, sc and Y multi-element standard solution 3, and using 10% nitric acid to fix the volume to obtain 2 mug/ml Ge, in, re, rh, sc and Y multi-element standard solution mother solution as an internal standard solution;
respectively sucking 0.5ml to 50ml PFA volumetric flasks from the multielement standard solution 1 and the multielement standard solution 2, fixing the volume by 10% nitric acid to obtain 10 mug/ml mixed multielement standard solution, respectively sucking 0.5ml, 2.5ml, 5ml and 25ml to 4 different 50ml PFA volumetric flasks from the 10 mug/ml mixed multielement standard solution, fixing the volume by 10% nitric acid to obtain 0.1 mug/ml, 0.5 mug/ml, 1 mug/ml and 5 mug/ml mixed multielement standard solution mother solution, respectively sucking 0.5ml to 2 different 50ml PFA volumetric flasks from the 1 mug/ml mixed multielement standard solution mother solution and fixing the volume by 10% nitric acid to obtain 0.01 mug/ml and 0.05 mug/ml mixed multielement standard solution mother solution;
taking 100 mu l of mixed multi-element standard solution mother solution from 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 solution of 2 mu g/ml of Ge, in, re, rh, sc and Y into each PFA sample tank, finally adding NMP to the mixed multi-element standard solution with 6 gradient concentrations of 0.1, 0.5, 1, 5, 10 and 50 mu g/kg into the PFA sample tank, sequentially feeding the mixed multi-element standard solution according to the concentration from low to high after the preparation, obtaining a standard curve through a least square method, and obtaining R 2 ≥0.999；
And a second step of: sample pretreatment method:
1) The PFA sample tank is soaked in a 30% nitric acid tank in advance, and the soaking time is not less than 24 hours; repeatedly flushing the container with ultrapure water with the volume of not less than 10 times of the container after the soaking is finished, and eluting residual metal elements on the surface of the container;
2) Sample weighing: the sample was weighed 0.1g (accurate to 0.0001 g) into a PFA sample tank and the weighed mass m was recorded 0 ；
3) Adding an internal standard: 100 μl was aspirated from 2 μg/ml internal standard solution and added to a PFA sample tank with sample;
4) Sample quantitative preparation: NMP is added into a PFA sample tank weighed with a sample and added with an internal standard until the total solid-liquid mass is 10g, and the weighed mass m is recorded 1 Screwing a threaded sealing cover for sealing;
5) Extracting metal elements: and (3) placing the PFA sample tank subjected to quantitative preparation and sealing in a water bath, performing ultrasonic extraction for 30min, and taking out the PFA sample tank to be detected after the sample liquid is observed by naked eyes and is turned to be clear and transparent.
And a third step of: the preparation and treatment links of the blank solution are reduced by the step 2) of sample weighing, and the rest is consistent with the second step.
Fourth step: sample detection
Inductively coupled plasma mass spectrometer using organic sample injection system adopts organic sample injection mode, argon as carrier gas, oxygen as reaction gas, helium as collision gas, and gas injectionThe method comprises the steps of carrying out sample injection analysis on 6 mixed multi-element standard solutions with gradient concentrations of 0.1, 0.5, 1, 5, 10 and 50 mug/kg in sequence, correcting the response value of an element to be detected according to the ratio of the internal standard value of an actually measured internal standard element to an expected value, and obtaining a standard curve by a least square method to obtain a standard curve linear R 2 More than or equal to 0.999, respectively testing blank and sample to-be-tested liquid; 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; .
Fifth step: the metal element content calculation formula:
X i : metal element content of OLED material, mug/kg
C i : the concentration of the element i in the sample to be measured, mug/kg
C 0 : concentration of the element i in blank liquid to be measured, mug/kg
m 0 : weighing mass of solid sample g
m 1 : weighing mass of liquid to be measured g
Through calculation, the sample to be detected in the embodiment contains 9 metal elements, the content of which is shown in the following table 1, meets the requirement of annex B.1 in GB/T27417-2017 standard assessment chemical analysis method confirmation and verification guide on the variation coefficient of a laboratory, and shows that the result is accurate.
Table 1 results of the test for the content of metallic element (μg/kg)
11 sample blank tests were performed consecutively, by calculating 3 times the standard deviation of the test results as the detection limit of the test method, which is lower than the conventional detection limit of international standard IEC-62321-5 by 2ppm, see table 2 below:
TABLE 2 detection limits (. Mu.g/kg) obtained from 11 blank test results
Meanwhile, 6 sample blanks are prepared, blank samples are prepared, the metal element concentrations of the blank samples are tested under the same standard curve condition, blank test results of table 3 are obtained, blank results are all less than 1 mug/kg, the range difference between blanks is less than 1 mug/kg, no difference exists between different PFA sample tanks after cleaning, and the background blank is stable.
Table 3 6 sample blank test results (μg/kg)
15 parallel OLED material samples are prepared from batch samples, one of the samples is taken as an original sample, and the other 14 samples are subjected to 7 parallel results of parallel labeling tests (the labeling concentration is 2000 mug/kg and 1000 mug/kg), the relative standard deviation and the labeling recovery rate of the test results are calculated, the average recovery rate of each element labeled sample is 86% -102% as shown in the following table 4, the accuracy of the method is high, the relative standard deviation RSD is 0.4% -4.5%, the precision is high, 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 labeled 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 every 3 hours, the test results are shown in the following table 5, the average recovery rate is 92% -111%, the stability change of the same gradient sample at 9 hours is recorded, the RSD is less than 5%, the sample is not basically changed after being placed for 9 hours, and the long-term stability of the sample is considered to be good.
Table 5 3 gradient-labeled samples over 9 hours (3 h each interval) change results
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 environmental friendliness in operation.
Claims (8)
1. A method for determining the content of residual metallic elements in an OLED material, comprising the steps of:
(1) Preparing a standard solution:
1) The 24 multi-element standard solutions 1 and 9 multi-element standard solutions 2 are prepared into mixed multi-element standard solution mother solution with gradient concentration by using nitric acid solution as solvent,
2) The multi-element standard solution 3 of Ge, in, re, rh, sc and Y is prepared into an internal standard solution by using a nitric acid solution as a solvent;
3) Taking X mul of mixed multi-element standard solution mother liquor with gradient concentration, adding the X mul of mixed multi-element standard solution mother liquor into different PFA sample tanks, and respectively adding Y mul of internal standard solution; finally NMP is added into the PFA sample tank to lead the mass of the solution to m 1 Preparing a mixed multi-element standard solution with gradient concentration;
(2) Preparation of sample liquid to be tested
a) Sample m 0 g, into a PFA sample tank;
b) Adding Y μl of the internal standard solution in the step 2);
c) Sample quantitative preparation: NMP is added into a PFA sample tank which is weighed with a sample and added with an internal standard until the total solid-liquid mass is m 1 g, screwing a threaded sealing cover for sealing;
d) Extracting metal elements: placing the sealed PFA sample tank in a water bath, performing ultrasonic treatment for 30min for extraction, and taking out the PFA sample tank to be detected after macroscopic observation of the sample liquid is transferred to be clear and transparent;
(3) Preparing blank solution
Except for reducing the links of weighing the sample, the steps are identical to the step (2);
(4) Sample detection
An inductively coupled plasma mass spectrometer using an organic sample injection system adopts an organic sample injection mode, argon is used as carrier gas, oxygen is used as reaction gas, helium is used as collision gas, the organic sample injection system is matched, mixed multi-element standard solution with gradient concentration is sequentially subjected to sample injection analysis from low to high, the response value of an element to be measured is corrected according to the ratio of the internal standard value of an actually measured internal standard element to an expected value, a standard curve is obtained through a least square method, and a standard curve and linear R are obtained 2 More than or equal to 0.999, respectively testing blank and sample to-be-tested liquid; 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 calculating a formula of metal element content:
X i : metal element content of OLED material, mug/kg
C i : the concentration of the element i in the sample to be measured, mug/kg
C 0 : concentration of the element i in blank liquid to be measured, mug/kg
m 0 : weighing mass of solid sample g
m 1 : and g, weighing mass of the liquid to be measured.
2. The method according to claim 1, wherein the concentrations of the multi-element standard solutions 1, 2 and 3 are 1000 μg/ml, the solvent is 10% nitric acid solution, the concentration of the internal standard solution is 2 μg/ml, the multi-standard solution 1 in the step 1) is the same as the multi-element standard solution 2, and the concentrations of the mixed multi-element standard solutions with gradient concentrations are respectively: 0.1, 0.5, 1, 5, 10, 50. Mu.g/kg.
3. The method of claim 2, wherein X μl is 100 μl and Y μl is 100 μl; m is m 0 g is 0.1g, m 1 The g is 10g, and the accuracy is 0.0001g.
4. The method of claim 3, wherein the method for preparing the internal standard solution comprises the following steps: and sucking 1ml to 50ml 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 mug/ml Ge, in, re, rh, sc and Y multi-element standard solution mother solution as an internal standard solution.
5. The method of claim 4, wherein the method for preparing the mixed multi-element standard solution with gradient concentration comprises the following steps: respectively sucking 0.5ml to 50ml PFA volumetric flasks from the multielement standard solution 1 and the multielement standard solution 2, fixing the volume by 10% nitric acid to obtain 10 mug/ml mixed multielement standard solution, respectively sucking 0.5ml, 2.5ml, 5ml and 25ml to 4 different 50ml PFA volumetric flasks from the 10 mug/ml mixed multielement standard solution, fixing the volume by 10% nitric acid to obtain 0.1 mug/ml, 0.5 mug/ml, 1 mug/ml and 5 mug/ml mixed multielement standard solution mother solution, respectively sucking 0.5ml to 2 different 50ml PFA volumetric flasks from the 1 mug/ml mixed multielement standard solution mother solution and fixing the volume by 10% nitric acid to obtain 0.01 mug/ml and 0.05 mug/ml mixed multielement standard solution mother solution; 100. Mu.l of each mixed multi-element standard solution mother solution from 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 are taken into different PFA sample tanks, meanwhile 100. Mu.l of 2. Mu.g/ml Ge, in, re, rh, sc and Y multi-element standard solution mother solution are added into each PFA sample tank, and finally NMP is added into the mixed multi-element standard solution with 6 gradient concentrations of the solutions In the PFA sample tanks to 10g so as to prepare the mixed multi-element standard solution with 0.1, 0.5, 1, 5, 10 and 50. Mu.g/kg.
6. The method of claim 1, wherein the multi-element standard solution 1 contains Al, as, B, ba, be, bi, ca, cd, co, cr, cu, fe, K, li, mg, mn, na, ni, P, pb, se, sr, V, zn as the metal element.
7. The method of claim 1, wherein the multi-element standard solution 2 comprises metal elements of: mo, pd, re, S, sb, si, sn, ti, W.
8. The method of any one of claims 1-7, wherein the PFA sample canisters must be subjected to a cleaning step prior to use, the cleaning step being: soaking the PFA sample tank in a 30% nitric acid tank for not less than 24 hours; repeatedly washing the container with at least 10 times of ultrapure water after soaking, and eluting the residual metal elements on the surface of the container.
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