CN114739982A - Method for detecting element content in glass - Google Patents
Method for detecting element content in glass Download PDFInfo
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- CN114739982A CN114739982A CN202210283876.6A CN202210283876A CN114739982A CN 114739982 A CN114739982 A CN 114739982A CN 202210283876 A CN202210283876 A CN 202210283876A CN 114739982 A CN114739982 A CN 114739982A
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- 239000011521 glass Substances 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 42
- 230000029087 digestion Effects 0.000 claims abstract description 90
- 239000012086 standard solution Substances 0.000 claims abstract description 43
- 239000000243 solution Substances 0.000 claims abstract description 41
- 239000002904 solvent Substances 0.000 claims abstract description 36
- 238000012360 testing method Methods 0.000 claims abstract description 35
- 230000002378 acidificating effect Effects 0.000 claims abstract description 29
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 43
- 229910052710 silicon Inorganic materials 0.000 claims description 43
- 239000010703 silicon Substances 0.000 claims description 43
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 239000005328 architectural glass Substances 0.000 claims description 4
- 239000006059 cover glass Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 20
- 239000011550 stock solution Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 13
- 239000000523 sample Substances 0.000 description 13
- 239000000843 powder Substances 0.000 description 11
- 229910052697 platinum Inorganic materials 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 150000002500 ions Chemical group 0.000 description 3
- 238000013098 chemical test method Methods 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Engineering & Computer Science (AREA)
- Glass Compositions (AREA)
Abstract
The invention relates to the technical field of glass component detection, and discloses a method for detecting element content in glass. The method comprises the following steps: (1) in the presence of an acidic solvent I, performing first digestion on a standard solution to obtain a first digestion solution, testing the first digestion solution by using an inductively coupled plasma atomic emission spectrometer, and fitting to obtain a standard working curve; performing second digestion on the glass to be detected in the presence of an acidic solvent II to obtain a second digestion solution; (2) and testing the second digestion solution by adopting an inductively coupled plasma emission spectrometer under the condition of a standard working curve. The detection method provided by the invention can obtain the content of the elements in the glass to be detected without conversion of the recovery rate, and the detection result has high accuracy.
Description
Technical Field
The invention relates to the technical field of glass component detection, in particular to a method for detecting element content in glass.
Background
The method for testing the element content in the glass component mainly comprises a chemical test method and an instrument test method. The chemical test method has long detection period, great chemical hazard and high labor and time cost. Therefore, the prior art generally uses instrumental methods to detect the content of elements in the glass composition.
Among them, the method of detecting the element content in the glass component by using inductively coupled plasma emission spectrometry is one of the most widely used methods.
The traditional inductively coupled plasma emission spectrometry method for measuring the element content in the glass components is to dilute a standard solution, prepare a series of concentrations, directly test on a machine, and fit a standard curve through an instrument; and analyzing the pretreated sample solution by an instrument, and substituting the sample solution into the standard curve to calculate the content of the component to be measured in the sample.
However, the deviation between the detection result of the test mode and the theoretical value of the sample is large, and the accuracy is low; in addition, it is usually necessary to obtain an accurate value through complicated calculation, and particularly, for a glass sample containing a volatile trace amount of oxide, the volatile element is lost along with pretreatment in a pretreatment process, and a detection value obtained by substituting the sample into a standard curve through instrumental analysis is usually low.
Disclosure of Invention
The invention aims to solve the problem of low accuracy of the element detection method in the glass component in the prior art.
In order to achieve the above object, the present invention provides a method for detecting the content of elements in glass, the method comprising:
(1) in the presence of an acidic solvent I, performing first digestion on a standard solution to obtain a first digestion solution, testing the first digestion solution by using an inductively coupled plasma atomic emission spectrometer, and fitting to obtain a standard working curve; and
in the presence of an acid solvent II, carrying out second digestion on the glass to be detected to obtain a second digestion solution;
(2) testing the second digestion solution by adopting an inductively coupled plasma atomic emission spectrometer under the condition of the standard working curve;
wherein the acid solvent I is prepared from the following components in a mass ratio of 1: 1.2-1.6: 0.5-1 of a combination of hydrofluoric acid, nitric acid and hydrochloric acid; the conditions of the first digestion comprise: the temperature is 150 ℃ and 250 ℃, and the time is 2-4 h.
Preferably, in step (1), the conditions of the first digestion comprise: the temperature is 180 ℃ and 190 ℃, and the time is 2-4 h.
Preferably, in step (1), the acidic solvent II and the acidic solvent I are the same.
Preferably, in step (1), the amount of the acidic solvent I used is 0.3 to 1mL relative to 1mL of the standard solution.
Preferably, in the step (1), the amount of the acidic solvent II is 10-20mL relative to 1g of the glass to be tested.
Preferably, in the step (1), the glass to be tested is selected from at least one of architectural glass, cover glass and substrate glass.
Preferably, in the step (1), the glass to be tested contains 48-73 wt% of SiO based on the total weight of the glass to be tested20-20% by weight of Al2O33-12 wt% CaO, 0-4 wt% MgO and 0-11 wt% B2O3。
Preferably, in the step (1), the glass to be measured is glass powder with an average particle size of 3-7 μm.
Preferably, in step (1), the conditions of the second digestion comprise: the temperature is 150 ℃ and 250 ℃, and the time is 2-4 h.
Preferably, the element is selected from at least one of silicon, iron, calcium and magnesium.
The detection method provided by the invention can obtain the content of the element in the glass to be detected without complex calculation, and the detection result has high accuracy.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
In the present invention, unless otherwise specified, the room temperature or the ambient temperature both indicate 25. + -. 2 ℃.
As previously mentioned, the present invention provides a method for detecting the content of elements in glass, the method comprising:
(1) in the presence of an acidic solvent I, performing first digestion on a standard solution to obtain a first digestion solution, testing the first digestion solution by using an inductively coupled plasma atomic emission spectrometer, and fitting to obtain a standard working curve; and
in the presence of an acid solvent II, carrying out second digestion on the glass to be detected to obtain a second digestion solution;
(2) testing the second digestion solution by adopting an inductively coupled plasma atomic emission spectrometer under the condition of the standard working curve;
wherein the acid solvent I is prepared from the following components in a mass ratio of 1: 1.2-1.6: 0.5-1 of a combination of hydrofluoric acid, nitric acid and hydrochloric acid; the conditions of the first digestion comprise: the temperature is 150 ℃ and 250 ℃, and the time is 2-4 h.
The invention has no special requirement on the content of the element to be detected, can be determined according to the detection limit of an inductively coupled plasma atomic emission spectrometer, and can detect the element with the content of not less than 0.01 wt% in the glass exemplarily.
Preferably, in step (1), the standard operating curve formula is: KX + B, where K is 1320-; x represents the concentration of the element to be detected, the unit is mg/L, and B is 5-8.
The K value of the standard curve prepared by the method of the invention is in the range of 1320-1360, and the skilled person should not be construed as limiting the invention.
Preferably, in step (1), the conditions of the first digestion comprise: the temperature is 180 ℃ and 190 ℃, and the time is 2-4 h. The inventors have found that with this preferred embodiment, more accurate test results are obtained.
Preferably, in step (1), the acidic solvent I and the acidic solvent II are the same.
Preferably, in the step (1), the acidic solvent I is a mixture of acidic solvents in a mass ratio of 1: 1.2-1.6: 0.5-1 of hydrofluoric acid, nitric acid and hydrochloric acid. The inventors have found that, in this preferred embodiment, a more accurate detection result can be obtained.
Preferably, in the step (1), the concentration of the hydrofluoric acid is 30-40 wt%, the concentration of the nitric acid is 65-68 wt%, and the concentration of the hydrochloric acid is 36-38 wt%.
Preferably, in step (1), the amount of the acidic solvent I used is 0.3 to 1mL relative to 1mL of the standard solution.
Preferably, in step (1), the standard solution contains the element to be detected.
Preferably, in the step (1), the amount of the acidic solvent II used is 10-20mL relative to 1g of the glass to be tested.
Preferably, in the step (1), the glass to be tested is selected from at least one of architectural glass, cover glass and substrate glass.
Preferably, in the step (1), the glass to be tested contains 48-73 wt% of SiO based on the total weight of the glass to be tested20-20% by weight of Al2O33-12 wt% CaO, 0-4 wt% MgO and 0-11 wt% B2O3。
Preferably, in the step (1), the glass to be measured is glass powder with an average particle size of 3-7 μm.
Preferably, in step (1), the method further comprises: before the glass to be detected is subjected to second digestion, the glass to be detected is crushed to obtain glass powder to be detected with the average particle size of 3-7 microns.
Preferably, in step (1), the conditions of the second digestion include: the temperature is 150 ℃ and 250 ℃, and the time is 2-4 h.
According to a particularly preferred embodiment, the conditions of the first digestion and the second digestion are identical. The inventors have found that with this preferred embodiment, more accurate test results are obtained.
The apparatus for performing the first digestion and the second digestion is not particularly required by the present invention, and apparatuses known in the art may be used, and the present invention exemplarily performs the first digestion and the second digestion on a hot plate.
The concentration of the first digestion solution is not particularly required, and can be adjusted according to actual conditions.
According to a particularly preferred embodiment, in step (1), the method further comprises: and (2) fixing the volume of the material subjected to the first digestion by using water to obtain stock solution (for example, the concentration is 10mg/L) with determined concentration of the element to be detected, respectively sucking a certain amount of the stock solution into a sample bottle by using scale suction pipes with different measuring ranges, and adding water to prepare first digestion solution (for example, the concentration is 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L and 5.0mg/L) with different concentrations).
According to a particularly preferred embodiment, in step (1), the method further comprises: and (4) fixing the volume of the material subjected to the second digestion by using water to obtain the second digestion solution with determined concentration.
Preferably, the element is selected from at least one of silicon, iron, calcium and magnesium.
The present invention will be described in detail below by way of examples. In the following examples, various raw materials used are commercially available ones unless otherwise specified.
Standard solution: the standard solution containing silicon with the concentration of 1000mg/L calculated by silicon element is purchased from an environmental protection standard sample research institute;
in the following examples, the standard working curve of the undigested standard solution is Y ═ 1416X +17.098, where X represents the concentration of the element to be measured in the standard solution, and Y represents the ionic signal intensity of the element to be measured during the instrument test.
Glass to be tested 1: architectural glass comprising 70% by weight of SiO as the main component23% by weight of Al2O38% by weight of CaO, 2% by weight of MgO;
and 2, glass to be detected: cover glass comprising 60% by weight of SiO as the main component220% by weight of Al2O3And 5% by weight of B2O3；
Glass to be measured 3: a substrate glass comprising 58% by weight of SiO as a main component215% by weight of Al2O310% by weight of B2O3And 5 wt% CaO;
in the following examples, the glass to be measured was in the form of powder having an average particle diameter of 5 μm;
in the following examples, the concentrations of hydrofluoric acid, nitric acid and hydrochloric acid were 40 wt%, 65 wt% and 36 wt%, respectively;
in the following examples, inductively coupled plasma atomic emission spectrometer (ICP) model ICAP7000, available from seimer feishell technologies ltd, usa, was used with the following detection parameters: the RF power was 1150w, the pump speed was 50rpm, the assist gas flow rate was 0.5L/min, and the atomizing gas flow rate was 0.5L/min.
Example 1
The embodiment provides a method for detecting the content of silicon element in glass, which comprises the following steps:
(1) adding 10mL of standard solution into a platinum crucible, adding 3mL of acidic solvent I (wherein the mass ratio of hydrofluoric acid, nitric acid and hydrochloric acid in terms of dry basis is 1: 1.5: 0.7), placing on an electric hot plate at 180 ℃ for first digestion for 3h, cooling the material subjected to the first digestion, then fixing the volume to 100mL with water to obtain stock solutions with the concentration of 100mg/L, respectively sucking a certain amount of the stock solutions into a sample bottle by using graduated straws with different ranges, adding water to prepare first digestion solutions with the concentrations of 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L and 5.0mg/L, testing the obtained first digestion solutions by using an inductively coupled plasma atomic emission spectrometer, taking the ionic signal intensity of silicon elements during instrument testing as a vertical coordinate, taking the concentration of the silicon element in the standard solution as an abscissa, and drawing to obtain a standard working curve Y which is 1331.1X + 7.6547;
0.2501g of glass 1 powder to be detected is added into a platinum crucible, 3mL of an acidic solvent II (wherein the mass ratio of hydrofluoric acid to nitric acid to hydrochloric acid is 1: 1.5: 0.7 in terms of dry basis) is added, the mixture is placed on an electric hot plate at 180 ℃ for second digestion for 3 hours, the material subjected to second digestion is cooled, and then water is used for fixing the volume to 100mL to obtain a second digestion solution with the concentration of 2.501 mg/L;
(2) and testing the obtained second digestion solution by using an inductively coupled plasma atomic emission spectrometer, and obtaining the content of the silicon element in the glass 1 to be tested on the standard working curve.
The experiment was repeated 3 times with the content of silicon element in the glass 1 to be measured being 1mg/g as a standard value, and the results are shown in table 1.
Comparative example 1
Detecting the content of silicon element in the glass according to the method of the embodiment 1, except that in the step (1), the standard solution 1 is directly tested to obtain a standard working curve of the undigested standard solution without first digesting;
the method comprises the following specific operation steps:
(1) measuring 10mL of standard solution, then fixing the volume to 100mL by using water to obtain 100mg/L standard stock solution, respectively sucking a certain amount of standard stock solution into a sample bottle by using graduated pipettes with different ranges, adding water to prepare 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L and 5.0mg/L standard solutions, testing the obtained standard solutions with different concentrations by using an inductively coupled plasma atomic emission spectrometer, and drawing a standard working curve of the undigested standard solution by using the ion signal intensity of silicon element as a vertical coordinate and the concentration of the silicon element in the standard solution as a horizontal coordinate during instrument testing;
0.2501g of glass 1 powder to be detected is added into a platinum crucible, 3mL of an acidic solvent II (wherein the mass ratio of hydrofluoric acid to nitric acid to hydrochloric acid is 1: 1.5: 0.7 in terms of dry basis) is added, the mixture is placed on an electric hot plate at 180 ℃ for digestion for 3 hours, the digested material is cooled, and then the volume is determined to be 100mL by water to obtain a digestion solution with the concentration of 2.501 mg/L;
(2) and testing the obtained digestion solution by using an inductively coupled plasma atomic emission spectrometer, and obtaining the content of the silicon element in the glass 1 to be tested on the standard working curve.
The experiment was repeated 3 times with the content of silicon element in the glass 1 to be measured as 1mg/g as the standard value, and the results are shown in table 1.
Example 2
The embodiment provides a method for detecting the content of silicon element in glass, which comprises the following steps:
(1) adding 10mL of standard solution into a platinum crucible, adding 3mL of acidic solvent I (wherein the mass ratio of hydrofluoric acid, nitric acid and hydrochloric acid on a dry basis is 1: 1.5: 0.7), placing on an electric hot plate at 190 ℃ for first digestion for 2h, cooling the material subjected to the first digestion, then adding water to a constant volume of 100mL to obtain stock solutions with the concentration of 100mg/L, respectively sucking a certain amount of the stock solutions into a sample bottle by using graduated pipettes with different measuring ranges, adding water to prepare first digestion solutions with the concentrations of 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L and 5.0mg/L, testing the obtained first digestion solutions by using an inductively coupled plasma atomic emission spectrometer, taking the ionic signal intensity of a silicon element during instrument testing as a vertical coordinate, taking the concentration of the silicon element in the standard solution as an abscissa, and drawing to obtain a standard working curve Y which is 1327.9X + 5.2838;
0.2001g of glass 2 powder to be detected is added into a platinum crucible, 3mL of an acidic solvent II (wherein the mass ratio of hydrofluoric acid to nitric acid to hydrochloric acid is 1: 1.5: 0.7 in terms of dry basis) is added, the mixture is placed on an electric hot plate at 190 ℃ for second digestion for 2 hours, the material subjected to second digestion is cooled, and then water is used for fixing the volume to 100mL to obtain a second digestion solution with the concentration of 2.001 mg/L;
(2) and testing the obtained second digestion solution by using an inductively coupled plasma atomic emission spectrometer, and obtaining the content of the silicon element in the glass 2 to be tested on the standard working curve.
The experiment was repeated 3 times with the content of silicon element in the glass 2 to be measured being 1mg/g as a standard value, and the results are shown in table 1.
Comparative example 2
Detecting the content of silicon element in the glass according to the method of the embodiment 2, except that in the step (1), the standard solution 2 is directly tested to obtain a standard working curve of the undigested standard solution without first digesting;
the method comprises the following specific operation steps:
(1) measuring 10mL of standard solution, then using water to fix the volume to 100mL to obtain standard stock solution with the concentration of 100mg/L, respectively using scale suction pipes with different ranges to suck a certain amount of standard stock solution into a sample bottle, then adding water to prepare standard solution with the concentrations of 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L and 5.0mg/L, and using an inductively coupled plasma atomic emission spectrometer to test the obtained standard solution with different concentrations, and drawing a standard working curve of the standard solution without digestion by taking the ion signal intensity of silicon element as a vertical coordinate and the concentration of the silicon element in the standard solution as a horizontal coordinate during instrument test;
0.2001g of glass 1 powder to be detected is added into a platinum crucible, 3mL of an acidic solvent II (wherein the mass ratio of hydrofluoric acid to nitric acid to hydrochloric acid is 1: 1.5: 0.7 in terms of dry basis) is added, the mixture is placed on an electric hot plate at 190 ℃ for digestion for 2 hours, the digested material is cooled, and then the volume is determined to be 100mL by water to obtain a digestion solution with the concentration of 2.001 mg/L;
(2) and testing the obtained digestion solution by using an inductively coupled plasma atomic emission spectrometer, and obtaining the content of the silicon element in the glass 2 to be tested on the standard working curve.
The experiment was repeated 3 times with the content of silicon element in the glass 2 to be measured being 1mg/g as the standard value, and the results are shown in table 1.
Example 3
The embodiment provides a method for detecting the content of silicon element in glass, which comprises the following steps:
(1) adding 10mL of standard solution into a platinum crucible, adding 3mL of acidic solvent I (wherein the mass ratio of hydrofluoric acid, nitric acid and hydrochloric acid in terms of dry basis is 1: 1.5: 0.7), placing on a hot plate at 185 ℃ for first digestion for 4h, cooling the material subjected to the first digestion, then fixing the volume to 100mL with water to obtain stock solutions with the concentration of 100mg/L, respectively sucking a certain amount of the stock solutions into a sample bottle by using graduated straws with different ranges, adding water to prepare first digestion solutions with the concentrations of 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L and 5.0mg/L, testing the obtained first digestion solutions by using an inductively coupled plasma atomic emission spectrometer, taking the ionic signal intensity of silicon elements during instrument testing as a vertical coordinate, taking the concentration of the silicon element in the standard solution as an abscissa, and drawing to obtain a standard working curve Y which is 1341.7X + 6.5531;
0.2001g of glass 3 powder to be detected is added into a platinum crucible, 3mL of an acidic solvent II is added (wherein the mass ratio of hydrofluoric acid to nitric acid to hydrochloric acid on a dry basis is 1: 1.5: 0.7), the mixture is placed on an electric hot plate at 185 ℃ for second digestion for 4 hours, the material subjected to the second digestion is cooled, and then the volume is determined to 100mL by water to obtain a second digestion solution with the concentration of 2.001 mg/L;
(2) and testing the obtained second digestion solution by using an inductively coupled plasma atomic emission spectrometer, and obtaining the content of the silicon element in the glass 3 to be tested on the standard working curve.
The experiment was repeated 3 times with the content of silicon element in the glass 3 to be measured being 1mg/g as a standard value, and the results are shown in table 1.
Comparative example 3
Detecting the content of silicon element in the glass according to the method of the embodiment 3, except that in the step (1), the standard solution is directly tested to obtain a standard working curve of the undigested standard solution without first digesting;
(1) measuring 10mL of standard solution, then fixing the volume to 100mL by using water to obtain 100mg/L standard stock solution, respectively sucking a certain amount of standard stock solution into a sample bottle by using graduated pipettes with different ranges, adding water to prepare 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L and 5.0mg/L standard solutions, testing the obtained standard solutions with different concentrations by using an inductively coupled plasma atomic emission spectrometer, and drawing a standard working curve of the undigested standard solution by using the ion signal intensity of silicon element as a vertical coordinate and the concentration of the silicon element in the standard solution as a horizontal coordinate during instrument testing;
0.2001g of glass 3 powder to be detected is added into a platinum crucible, 3mL of an acidic solvent II is added (wherein the mass ratio of hydrofluoric acid to nitric acid to hydrochloric acid on a dry basis is 1: 1.5: 0.7), the mixture is placed on an electric hot plate at 185 ℃ for digestion for 4 hours, the digested material is cooled, and then the volume is determined to 100mL by water to obtain a digestion solution with the concentration of 2.001 mg/L;
(2) and testing the obtained digestion solution by using an inductively coupled plasma atomic emission spectrometer, and obtaining the content of the silicon element in the glass 3 to be tested on the standard working curve.
The experiment was repeated 3 times with the content of silicon element in the glass 3 to be measured being 1mg/g as a standard value, and the results are shown in table 1.
Example 4
The content of silicon element in the glass was measured according to the method of example 1, except that the temperatures of the first digestion and the second digestion were both 160 ℃, and the standard working curve obtained in step (1) was Y-1331.7X + 6.4748.
The experiment was repeated 3 times with the content of silicon element in the glass 1 to be measured being 1mg/g as a standard value, and the results are shown in table 1.
Example 5
The content of silicon element in the glass was measured according to the method of example 1, except that the temperatures of the first and second digestions were 240 ℃, and the standard working curve obtained in step (1) was Y-1350.2X + 7.7728.
The experiment was repeated 3 times with the content of silicon element in the glass 1 to be measured being 1mg/g as a standard value, and the results are shown in table 1.
Comparative example 4
Detecting the content of silicon element in the glass according to the method of the embodiment 1, except that in the step (1), an acid solvent is not added in the digestion process of the standard solution 1;
the specific operation method of the step (1) comprises the following steps:
placing 10mL of standard solution 1 on an electric hot plate at 180 ℃ for first digestion for 3h, cooling the material subjected to the first digestion, then adding water to a constant volume of 100mL to obtain stock solutions with the concentration of 100mg/L, respectively sucking a certain amount of the stock solutions into sample bottles by using graduated pipettes with different ranges, adding water to prepare first digestion solutions with the concentrations of 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L and 5.0mg/L, testing the obtained first digestion solutions by using an inductively coupled plasma atomic emission spectrometer, and drawing to obtain a standard working curve Y which is 1143.4X +5.2206 by using the ionic signal intensity of silicon element as a vertical coordinate and the concentration of silicon element in the standard solution as a horizontal coordinate when testing by an instrument; and
0.2501g of glass 1 powder to be detected is added into a platinum crucible, 3mL of an acidic solvent II (wherein the mass ratio of hydrofluoric acid to nitric acid to hydrochloric acid is 1: 1.5: 0.7 in terms of dry basis) is added, the mixture is placed on an electric hot plate at 180 ℃ for second digestion for 3 hours, the material subjected to second digestion is cooled, and then water is used for fixing the volume to 100mL, so that a second digestion solution with the concentration of 2.501mg/L is obtained.
The experiment was repeated 3 times with the content of silicon element in the glass 1 to be measured being 1mg/g as a standard value, and the results are shown in table 1.
TABLE 1
As can be seen from the results in Table 1, the content of the element in the glass to be detected can be obtained by the detection method provided by the invention without complex calculation, the detection result can be directly obtained after ICP (inductively coupled plasma) test, and the detection result has high accuracy.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for detecting the content of an element in glass, the method comprising:
(1) in the presence of an acidic solvent I, performing first digestion on a standard solution to obtain a first digestion solution, testing the first digestion solution by using an inductively coupled plasma atomic emission spectrometer, and fitting to obtain a standard working curve; and
in the presence of an acid solvent II, carrying out second digestion on the glass to be detected to obtain a second digestion solution;
(2) testing the second digestion solution by adopting an inductively coupled plasma atomic emission spectrometer under the condition of the standard working curve;
wherein the acid solvent I is prepared from the following components in a mass ratio of 1: 1.2-1.6: 0.5-1 of a combination of hydrofluoric acid, nitric acid and hydrochloric acid; the conditions of the first digestion comprise: the temperature is 150 ℃ and 250 ℃ and the time is 2-4 h.
2. The method according to claim 1, wherein in step (1), the conditions of the first digestion comprise: the temperature is 180 ℃ and 190 ℃, and the time is 2-4 h.
3. The process according to claim 1 or 2, characterized in that in step (1), the acidic solvent II and the acidic solvent I are the same.
4. The method according to any one of claims 1 to 3, wherein in step (1), the amount of the acidic solvent I used is 0.3 to 1mL relative to 1mL of the standard solution.
5. The method according to any one of claims 1 to 4, wherein in step (1), the amount of the acidic solvent II used is 10 to 20mL relative to 1g of the glass to be tested.
6. The method according to any one of claims 1 to 5, wherein in step (1), the glass to be tested is selected from at least one of architectural glass, cover glass, and substrate glass.
7. The method according to any one of claims 1 to 6, wherein in step (1), the glass to be tested contains 48 to 73 wt% of SiO based on the total weight of the glass to be tested20-20% by weight of Al2O33-12 wt% CaO, 0-4 wt% MgO and 0-11 wt% B2O3。
8. The method according to claim 7, wherein in the step (1), the glass to be measured is glass frit having an average particle diameter of 3 to 7 μm.
9. The method according to any one of claims 1 to 8, wherein in step (1), the conditions of the second digestion comprise: the temperature is 150 ℃ and 250 ℃, and the time is 2-4 h.
10. The method according to any one of claims 1 to 9, wherein the element is selected from at least one of silicon, iron, calcium and magnesium.
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