Method and device for detecting content of ferrous oxide in glass

Abstract

The invention discloses a method and a device for detecting the content of ferrous oxide in glass, and belongs to the field of chemical detection and analysis. The method comprises the following steps: adding a glass sample into a first reaction container; adding a digestion solution into a second reaction container; introducing protective gas to displace air in a space where the first reaction container and the second reaction container are located; in a protective atmosphere environment, mixing and stirring the glass sample in the first reaction container and the digestion solution in the second reaction container until the glass sample is completely dissolved to form a reaction test solution; the content of ferrous oxide in the glass sample is measured through the reaction test solution, the problem that in the digestion process of the glass sample, Fe < 2 + > is prone to being oxidized into Fe < 3 + >, and consequently the detection result error is large can be solved, and the method is simple and rapid.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical detection and analysis, and in particular to a method and device for detecting the ferrous oxide content in glass. Background Art

[0002] Iron (FeO / Fe2O3) is an impurity component in glass, and its content can affect the color, optical properties, chemical stability and production process control of the glass.

[0003] In terms of color, Fe 2+ Usually blue-green, and Fe 3+ It is yellow, so the overall color of the glass depends on the ratio and content of the two. In terms of optical properties, Fe 2+ It may absorb ultraviolet or infrared rays. High content may cause the transmittance of glass to decrease at specific wavelengths. In terms of chemical stability, Fe2+ is more 3+ It is easier to participate in oxidation reaction, making the glass surface more susceptible to corrosion; in terms of production process, according to Fe 2+ with Fe 3+ The ratio of can accurately reflect the gas atmosphere (oxidation / reduction) of the furnace, and the Fe 2+ with Fe 3+ Therefore, for accurate detection of Fe 2+ Content is particularly important.

[0004] However, during the digestion of glass samples, Fe 2+ Easily oxidized to Fe by oxygen in the air 3 + , resulting in inaccurate test results. Summary of the Invention

[0005] The main purpose of the present invention is to provide a method for detecting the content of ferrous oxide in glass, which solves the problem of Fe 2+ Easily oxidized to Fe 3+ This is a technical problem that leads to large errors in the test results.

[0006] To achieve the above object, the present invention provides a method for detecting the ferrous oxide content in glass, comprising the following steps:

[0007] Adding a glass sample into a first reaction vessel;

[0008] Adding digestion solution to the second reaction vessel;

[0009] introducing a protective gas to displace the air in the space where the first reaction container and the second reaction container are located;

[0010] In a protective atmosphere, the glass sample in the first reaction container and the digestion solution in the second reaction container are mixed and stirred until the glass sample is completely dissolved to form a reaction solution;

[0011] The content of ferrous oxide in the glass sample is obtained by measuring the reaction solution.

[0012] In some embodiments of the present invention, the protective gas includes at least one of nitrogen and an inert gas.

[0013] In some embodiments of the present invention, the digestion solution includes hydrofluoric acid and sulfuric acid; and / or the volume ratio of the hydrofluoric acid to the sulfuric acid is (5:2) to (5:3).

[0014] In some embodiments of the present invention, the protective gas is nitrogen, and the purity of the nitrogen is greater than or equal to 99%.

[0015] In some embodiments of the present invention, the reaction solution is analyzed and measured by spectrophotometry to obtain the content of ferrous oxide in the glass sample.

[0016] In some embodiments of the present invention, analyzing and determining the content of ferrous oxide in the glass sample by spectrophotometry on the reaction solution comprises the following steps:

[0017] Draw a working curve related to the mass concentration and absorbance of the ferrous oxide standard sample;

[0018] Performing a color development treatment on the reaction solution to obtain a colorimetric solution, and measuring the absorbance of the colorimetric solution;

[0019] Substitute the absorbance of the colorimetric solution into the working curve to obtain the mass concentration of ferrous oxide in the colorimetric solution. Substitute the mass concentration of ferrous oxide in the colorimetric solution into the following formula to calculate the mass fraction of ferrous oxide in the glass sample:

[0020]

[0021] V represents the volume of the colorimetric solution, in mL;

[0022] m represents the mass of the glass sample, in g;

[0023] C represents the mass concentration of ferrous oxide in the colorimetric solution, in mg / L.

[0024] In some embodiments of the present invention, the step of performing a color development treatment on the reaction solution to obtain a colorimetric solution includes the following steps: adding saturated boric acid to the reaction solution to obtain a mixed solution, adjusting the pH of the mixed solution to acidity with an acid-base regulator and adding a color developer, adding water to the fixed volume, and placing it in a dark room for a predetermined time to develop color, thereby obtaining the colorimetric solution.

[0025] In some embodiments of the present invention, the acid-base regulator comprises acetic acid-sodium acetate buffer; and / or the pH of the mixed test solution is adjusted to 4.0-5.0 using the acid-base regulator.

[0026] In some embodiments of the present invention, the color developing agent includes a phenanthroline solution.

[0027] The present invention also provides a device for detecting the ferrous oxide content in glass, the device comprising:

[0028] A magnetic stirrer 10 , wherein a first reaction container 20 and a second reaction container 30 are fixed to the magnetic stirrer 10 , and the second reaction container 30 is placed in the body of the first reaction container 20 ;

[0029] The first reaction container 20 includes a container body and an upper cover, wherein the upper cover is provided with a first through hole 21 and a second through hole 22;

[0030] The first through hole 21 is connected to an air inlet pipe 40 and a reagent container 50;

[0031] A first valve 70 is provided between the first through hole 21 and the air intake pipe 40;

[0032] A second valve 80 is provided between the first through hole 21 and the reagent container 50.

[0033] The second through hole 22 is connected to an air outlet pipe 60;

[0034] A third valve 90 is provided between the second through hole 22 and the air outlet pipe 60;

[0035] The second reaction container 30 contains a magnetic material 100 .

[0036] The beneficial effects that can be achieved by the present invention are:

[0037] In the present invention, a glass sample is added to a first reaction container, a digestion solution is added to a second reaction container, a protective gas is introduced to exhaust the air in the space between the first reaction container and the second reaction container, and an oxygen-free reaction place is created. The glass sample in the first reaction container and the digestion solution in the second reaction container are mixed and stirred until the glass sample is completely dissolved to form a reaction solution. The content of ferrous oxide in the glass sample is measured based on the reaction solution, which can improve the Fe content of the glass sample during the digestion process. 2+ Easily oxidized to Fe 3+ The method is simple, feasible, convenient and fast. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying any creative work.

[0039] Figure 1 The figure is a schematic structural diagram of a device for detecting the ferrous oxide content in glass according to the present invention.

[0040] Figure Number:

[0041] 10. Magnetic stirrer; 20. First reaction vessel; 21. First through hole; 22. Second through hole; 30. Second stirring vessel; 40. Air inlet pipe; 50. Reagent container; 60. Air outlet pipe; 70. First valve; 80. Second valve; 90. Third valve; 100. Magnetic material.

[0042] The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings and in conjunction with the embodiments. DETAILED DESCRIPTION

[0043] It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0044] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0045] In the present invention, descriptions such as "first" and "second" are for descriptive purposes only and should not be understood as indicating or implying their relative importance or implicitly indicating the number of the technical features indicated. Therefore, features defined as "first" or "second" may explicitly or implicitly include at least one of such features. In addition, the technical solutions of various embodiments may be combined with each other, but this must be based on the fact that they can be implemented by a person of ordinary skill in the art. If the combination of technical solutions is mutually contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection claimed by the present invention.

[0046] The present invention provides a method for detecting the ferrous oxide content in glass, comprising the following steps:

[0047] S10, adding a glass sample into the first reaction container;

[0048] S20, adding digestion solution into the second reaction container;

[0049] S30, introducing a protective gas to displace the air in the space between the first reaction container and the second reaction container, and mixing and stirring the glass sample in the first reaction container and the digestion solution in the second reaction container in the protective atmosphere until the glass sample is completely dissolved to form a reaction solution;

[0050] Specifically, in one embodiment, a magnetic stirrer and a digestion solution are placed in a second reaction vessel, and the second reaction vessel is placed in a first reaction vessel. A glass sample to be tested is also placed in the first reaction vessel, and the first reaction vessel only has a magnetic stirrer. The air in the first and second reaction vessels is exhausted, and nitrogen or an inert gas is introduced into the first and second reaction vessels. The magnetic stirrer is then started, and the magnetic stirrer drives the magnetic stirrer in the second reaction vessel to rotate. This rotation causes the second reaction vessel to topple, and the digestion solution in the second reaction vessel flows out and contacts the glass sample to react, thereby obtaining a reaction solution. Of course, the digestion solution in the second reaction vessel and the glass sample in the first reaction vessel can also be mixed using a specialized mechanical device, such as a manipulator.

[0051] S40. Determine the content of ferrous oxide in the glass sample by using the reaction solution.

[0052] In the present invention, a glass sample is added to a first reaction container, a digestion solution is added to a second reaction container, a protective gas is introduced to exhaust the air in the space between the first reaction container and the second reaction container, and an oxygen-free reaction place is created. The glass sample in the first reaction container and the digestion solution in the second reaction container are mixed and stirred until the glass sample is completely dissolved to form a reaction solution. The content of ferrous oxide in the glass sample is measured based on the reaction solution, thereby improving the Fe content of the glass sample during the digestion process.2+ Easily oxidized to Fe 3+ The problem of large error in the test results is solved, and the method is simple, feasible, convenient and fast.

[0053] In some embodiments, the shielding gas includes at least one of nitrogen and an inert gas.

[0054] In some embodiments, the glass sample is in powder form, which can enhance contact with the digestion solution, promote the complete digestion reaction, and improve the accuracy of the test results.

[0055] In some embodiments, the glass sample is wetted with water before being placed in the first reaction container.

[0056] In some embodiments, the mass of the glass sample is weighed to an accuracy of 0.0001 g.

[0057] In some embodiments, a protective gas is introduced using a vacuum pump to exhaust the air in the space where the first reaction container and the second reaction container are located.

[0058] In some embodiments, the purity of the protective gas is ≥99% to prevent impurity gases from affecting the digestion reaction and causing large errors in the detection results.

[0059] In some embodiments, the digestion solution includes hydrofluoric acid and sulfuric acid.

[0060] In some embodiments, the volume ratio of hydrofluoric acid to sulfuric acid in the digestion solution is (5:2) to (5:3).

[0061] In some embodiments, the mass concentration of sulfuric acid is 50% to 60%.

[0062] In some embodiments, the start-up time of the magnetic stirrer is 5 min to 10 min.

[0063] In the present invention, the obtained reaction solution can be measured by spectrophotometry to determine the content of ferrous oxide in the glass sample. The spectrophotometry is fast and efficient and can reduce the contamination of the reaction solution by oxygen in the air during the measurement process, thereby increasing the error of the detection result.

[0064] In some embodiments, the reaction solution is analyzed by o-phenanthroline colorimetric analysis to determine the content of ferrous oxide in the glass sample. The o-phenanthroline colorimetric analysis can be performed according to GB / T 1549-2008 "Chemical Analysis Methods for Fiber Glass".

[0065] In some embodiments, the spectrophotometric method comprises the following steps:

[0066] S41. Draw a working curve related to the mass concentration and absorbance of the ferrous oxide standard sample;

[0067] S42, performing a color development treatment on the reaction solution to obtain a colorimetric solution, and measuring the absorbance of the colorimetric solution;

[0068] S43. Substitute the absorbance of the colorimetric solution into the working curve to obtain the mass concentration of ferrous oxide in the glass sample. Substitute the mass concentration of ferrous oxide in the glass sample into the following formula to calculate the mass fraction of ferrous oxide in the glass sample:

[0069]

[0070] V represents the volume of the colorimetric solution in milliliters (mL);

[0071] m represents the mass of the glass sample in grams (g);

[0072] C represents the mass concentration of ferrous oxide in the colorimetric solution, in milligrams per milliliter (mg / L).

[0073] In some embodiments, drawing a working curve related to the mass concentration and absorbance of the ferrous oxide standard sample in step S41 includes:

[0074] Prepare standard stock solution: prepare 100 mg / L ferrous oxide standard solution with ammonium ferrous sulfate;

[0075] Preparation of gradient standard stock solution: prepare 6 100mL brown volumetric flasks, add 25ml of water to each volumetric flask, use a pipette to add 0ml, 1ml, 2ml, 3ml, 4ml, and 5ml of ferrous oxide standard solution to the 6 volumetric flasks respectively, and add 1ml of hydroxylamine hydrochloride solution to each of the 6 volumetric flasks to prevent Fe2+ from being oxidized. At the same time, add 5ml of acetic acid-sodium acetate buffer solution to make the pH about 4.5, then add 1ml of the color developer o-phenanthroline to each of the 6 volumetric flasks, and dilute with water to the scale line. Shake well to obtain a colorimetric solution with a concentration gradient of 0mg / L, 1mg / L, 2mg / L, 3mg / L, 4mg / L, and 5mg / L. Let it stand in a dark room for 20min to allow it to develop color completely.

[0076] Prepare a blank control group: use 0 mg / L standard solution as the blank group, fill a 10 ml cuvette with the blank solution, and incubate at a wavelength of 510 nm.

[0077] Draw a working curve: measure the absorbance (A) of each concentration of colorimetric solution in turn, record the data, and draw a working curve with the mass concentration (mg / L) of the ferrous oxide standard solution as the horizontal axis and the absorbance (A) as the vertical axis.

[0078] In some embodiments, step S42 of performing color development treatment on the reaction solution to obtain a colorimetric solution includes: adding saturated boric acid to the reaction solution to obtain a mixed solution, adjusting the pH of the mixed solution to acidic using an acid-base regulator and adding a color developer, and then adding water to make up the volume to obtain a colorimetric solution.

[0079] In some embodiments, the acid-base regulator comprises acetic acid-sodium acetate buffer with a pH of 4-5, preferably 4.5.

[0080] In some embodiments, the pH of the mixed test solution is adjusted to 4.0-5.0 using an acid-base regulator.

[0081] In some embodiments, the color developer includes o-phenanthroline at a concentration of 8 to 12 g / L, preferably, 10 g / L.

[0082] The present invention also provides a device for detecting the ferrous oxide content in glass. The method for detecting the ferrous oxide content in glass of the present invention can be implemented by the device.

[0083] refer to Figure 1 The device of the present invention includes a magnetic stirrer 10, on which a first reaction container 20 and a second reaction container 30 are fixed. The first reaction container 20 includes a container body and an upper cover. The upper cover is covered on the container body to form a sealed reaction space. The second reaction container 30 is placed in the body of the first reaction container 20. The second reaction container 30 can be used to hold reagents used for the reaction.

[0084] The upper cover of the first reaction container 20 is provided with a first through hole 21 and a second through hole 22 . The first through hole 21 is connected to the air inlet pipe 40 and the reagent container 50 , and the second through hole 22 is connected to the air outlet pipe 60 .

[0085] A first valve 70 is provided between the first through-hole 21 and the air inlet pipe 40. By controlling the closing and opening of the first valve 70, the flow of gas from the air inlet pipe 40 through the first through-hole 21 into and out of the body of the first reaction vessel 20 can be controlled. A second valve 80 is provided between the first through-hole 21 and the reagent container 50. By controlling the closing and opening of the second valve 80, the flow of raw materials in the reagent container 50 into the body of the first reaction vessel 20 through the first through-hole 21 can be controlled. A third valve 90 is provided between the second through-hole 22 and the air outlet pipe 60. By controlling the closing and opening of the third valve 90, the discharge of gas from the first reaction vessel 20 can be controlled.

[0086] When using the device to digest a glass sample, the glass sample and the second reaction container are placed in the first reaction container, and the digestion solution and the magnetic material 100 are placed in the second reaction container, and it is ensured that the digestion solution does not contact the glass sample. Then, the second valve 70 and the third valve 80 are closed, the first valve 60 is opened, and the vacuum pump is connected to the air inlet pipe 40 to exhaust the air in the first reaction container. Then, the third valve 80 is opened, and protective gas is continuously input into the first reaction container from the air inlet pipe 40 to exhaust the air so that the first reaction container is filled with protective gas to create an oxygen-free reaction atmosphere. Then, the magnetic stirrer 30 is started, and the magnetic stirrer causes the magnetic material to rotate. The rotating magnetic material causes the second reaction container to tip over, and the digestion solution therein flows out and contacts the glass sample, causing a digestion reaction to obtain a reaction solution.

[0087] In some embodiments, the magnetic material is a magneton, which rotates under the action of a magnetic stirrer, thereby causing the second reaction container to tip over, allowing the digestion solution therein to flow out and directly contact and react with the glass sample.

[0088] In some embodiments, the rotation speed of the magnetic stirrer is preferably sufficient to drive the magnetic material and cause the second reaction container to tip over, so that the digestion solution therein flows out and contacts and reacts with the glass sample.

[0089] In some embodiments, the rotation speed of the magnetic stirrer is 200-300 revolutions per minute (rpm).

[0090] In step S20, the magnetic stirrer is started for a time sufficient to facilitate complete reaction between the glass sample and the digestion solution.

[0091] In some embodiments, continue to refer to Figure 1 The first reaction container is provided with an air inlet and an air outlet.

[0092] In some embodiments, when the reaction solution is analyzed and detected by spectrophotometry to determine the content of ferrous oxide in the glass sample, when the digestion reaction is completed, the first valve 60 and the third valve 80 are closed, and the reagent used for color development is added from the reagent container 50. For example, saturated boric acid is added from the reagent container 50 to the first reaction container 20. This can reduce the effect of oxygen in the air on the reaction solution during the colorimetric process.

[0093] The technical solutions of the present invention are further described in detail below in conjunction with specific embodiments. It should be understood that the following specific embodiments are only used to explain the present invention and are not used to limit the present invention.

[0094] Example 1

[0095] Example 1: Method for detecting ferrous oxide content in glass:

[0096] S10, take a glass sample ground into powder, weigh 0.2000g, and refer to Figure 1 The first reaction container 20 is connected to the magnetic stirrer 10 , and a glass sample moistened with water is added to the first reaction container 20 .

[0097] S20, continue reference Figure 1 , add digestion solution and magnets, i.e., magnetic material 100, into the second reaction container 30, place the second reaction container 30 filled with digestion solution and magnets into the first reaction container 20, and keep the second reaction container 30 upright to avoid direct contact between the digestion solution and the glass sample, wherein the digestion solution is 5 ml of hydrofluoric acid and 2 ml of sulfuric acid with a mass concentration of 50%.

[0098] S30: The lid of the first reaction container 20 is closed, and the air in the first reaction container 20 is exhausted by using an air pump. Then, nitrogen with a purity of more than 99% is continuously introduced into the first reaction container 20 to fill the first reaction container 20 with nitrogen. The magnetic stirrer 10 is started to drive the magnetic particles in the second reaction container 30. The second reaction container 30 is tilted under the drive of the magnetic particles. The digestion solution in the second reaction container 30 flows out and contacts the glass sample in the first reaction container 20 to react to obtain a reaction solution. The reaction lasts for 5 minutes.

[0099] S40, using o-phenanthroline colorimetric analysis method to measure the reaction solution, the steps are as follows:

[0100] S41. Draw a working curve of the relationship between the mass concentration and absorbance of the ferrous oxide standard:

[0101] Prepare standard stock solution: Use ammonium ferrous sulfate to prepare a 100 mg / L ferrous oxide standard solution.

[0102] Prepare gradient standard stock solution: prepare 6 100mL brown volumetric flasks, add 25ml of water to each volumetric flask, use pipette to add 0ml, 1ml, 2ml, 3ml, 4ml, 5ml of ferrous oxide standard solution to each of the 6 volumetric flasks, and add 1ml of hydroxylamine hydrochloride solution to each of the 6 volumetric flasks to avoid Fe 2+ At the same time, 5 ml of acetic acid-sodium acetate buffer solution was added to adjust the pH to about 4.5, and then 1 ml of the color developer 1-phenanthroline was added to 6 volumetric flasks respectively, and the mixture was diluted to the scale with water and shaken to obtain a colorimetric solution with a ferrous oxide concentration gradient of 0 mg / L, 1 mg / L, 2 mg / L, 3 mg / L, 4 mg / L, and 5 mg / L.

[0103] Color development: The colorimetric solution is allowed to stand in a dark room for 20 minutes until the color is completely developed. Then, the following colorimetric operation is performed in a dark room: the wavelength of the spectrophotometer is adjusted to 510 nm, a 10 mm absorption cell is used to hold the colorimetric solution, water is used as a reference, the absorbance of 6 groups of colorimetric solutions is measured, and a working curve is drawn related to the ferrous oxide standard solution and the absorbance.

[0104] S42, Reference Figure 1 , saturated boric acid was placed in the reagent container 60, 20 ml of saturated boric acid was added to the reaction solution of the first reaction container 20 through the air inlet, the lid of the first reaction container 20 was unscrewed, the reaction solution mixed with saturated boric acid was transferred to a 100 ml brown volumetric flask, 5 ml of acetic acid-sodium acetate buffer solution was added to adjust the pH to 4.3-4.8, 1 ml of o-phenanthroline solution was added at the same time, and then water was added to the scale line, and the colorimetric solution was shaken to obtain a colorimetric solution, and the colorimetric solution was placed in a dark place for color development for 20 minutes. The following colorimetric operation was performed in a dark room: the wavelength of the spectrophotometer was adjusted to 510 nm, a 10 mm absorption cell was used to hold the colorimetric solution, water was used as a reference, and the absorbance of the colorimetric solution was measured. The absorbance of the colorimetric solution was substituted into the working curve to obtain the mass concentration of ferrous oxide in the colorimetric solution, and then the mass fraction of ferrous oxide in the glass sample was calculated according to the following formula:

[0105]

[0106] V represents the volume of the colorimetric solution, in mL;

[0107] m represents the mass of the glass sample, in g;

[0108] C represents the mass concentration of ferrous oxide in the colorimetric solution, in mg / L.

[0109] Example 2

[0110] Example 2 The ferrous oxide content in the glass was detected by referring to the preparation method of Example 1, except that the digestion solution was 5 ml of hydrofluoric acid and 3 ml of 50% sulfuric acid.

[0111] Example 3

[0112] Example 3 The ferrous oxide content in the glass was detected by referring to the preparation method of Example 1, except that the reaction lasted for 8 minutes.

[0113] Comparative Example 1

[0114] The glass sample of Example 1 was used as a test object, and the ferrous oxide content in the glass sample was determined according to the ferrous oxide detection process of GB / T 1549-2008 "Chemical Analysis Methods for Fiber Glass".

[0115] Performance Testing

[0116] The ferrous oxide content in the glass samples measured in Examples 1 to 3 and Comparative Example 1 is recorded in Table 1.

[0117] Table 1

[0118] Experimental group Theoretical value Measured value Accuracy absorbance Example 1 0.0036％ 0.0033％ 91.67％ 0.0587Abs Example 2 0.0036％ 0.0032％ 88.89％ 0.0552Abs Example 3 0.0036％ 0.0034％ 94.44％ 0.0604Abs Comparative Example 1 0.0036％ 0.0029％ 80.55％ 0.0487Abs

[0119] Comparing Example 1 with Comparative Example 1, it can be seen that the content of ferrous oxide in the glass sample is detected according to the conventional method. 2+ Easily oxidized to Fe 3+ , resulting in the detected ferrous oxide content being too low.

[0120] The above are only preferred embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention description and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A method for detecting the ferrous oxide content in glass, characterized in that: The following steps are involved: Adding a glass sample into a first reaction vessel; Adding digestion solution to the second reaction vessel; introducing a protective gas to displace the air in the space where the first reaction container and the second reaction container are located; In a protective atmosphere, the glass sample in the first reaction container and the digestion solution in the second reaction container are mixed and stirred until the glass sample is completely dissolved to form a reaction solution; The content of ferrous oxide in the glass sample is obtained by measuring the reaction solution.

2. The method for detecting the ferrous oxide content in glass according to claim 1, characterized in that: The protective gas includes at least one of nitrogen and inert gas.

3. The method for detecting the ferrous oxide content in glass according to claim 1, characterized in that: The digestion solution includes hydrofluoric acid and sulfuric acid; and / or the volume ratio of the hydrofluoric acid to the sulfuric acid is (5:2) to (5:3).

4. The method for detecting the ferrous oxide content in glass according to claim 1, wherein: The protective gas is nitrogen, and the purity of the nitrogen is greater than or equal to 99%.

5. The method for detecting the ferrous oxide content in glass according to any one of claims 1 to 4, characterized in that: The reaction solution is analyzed and measured by spectrophotometry to obtain the content of ferrous oxide in the glass sample.

6. The method for detecting the ferrous oxide content in glass according to claim 5, characterized in that: The reaction solution is analyzed and determined by spectrophotometry to obtain the content of ferrous oxide in the glass sample, comprising the following steps: Draw a working curve related to the mass concentration and absorbance of the ferrous oxide standard sample; Performing a color development treatment on the reaction solution to obtain a colorimetric solution, and measuring the absorbance of the colorimetric solution; Substitute the absorbance of the colorimetric solution into the working curve to obtain the mass concentration of ferrous oxide in the colorimetric solution. Substitute the mass concentration of ferrous oxide in the colorimetric solution into the following formula to calculate the mass fraction of ferrous oxide in the glass sample: V represents the volume of the colorimetric solution, in mL; m represents the mass of the glass sample, in g; C represents the mass concentration of ferrous oxide in the colorimetric solution, in mg / L.

7. The method for detecting the ferrous oxide content in glass according to claim 6, characterized in that: The step of performing a color development treatment on the reaction solution to obtain a colorimetric solution includes the following steps: adding saturated boric acid to the reaction solution to obtain a mixed solution, adjusting the pH of the mixed solution to acidity with an acid-base regulator and adding a color developer, adding water to make up the volume, and placing it in a dark room for a predetermined time for color development to obtain the colorimetric solution.

8. The method for detecting the ferrous oxide content in glass according to claim 7, characterized in that: The acid-base regulator includes acetic acid-sodium acetate buffer; and / or the pH of the mixed test solution is adjusted to 4.0-5.0 using the acid-base regulator.

9. The method for detecting the ferrous oxide content in glass according to claim 8, characterized in that: The color developer includes o-phenanthroline solution.

10. A device for detecting the content of ferrous oxide in glass, characterized in that: The device comprises: A magnetic stirrer 10 , wherein a first reaction container 20 and a second reaction container 30 are fixed to the magnetic stirrer 10 , and the second reaction container 30 is placed in the body of the first reaction container 20 ; The first reaction container 20 includes a container body and an upper cover, wherein the upper cover is provided with a first through hole 21 and a second through hole 22; The first through hole 21 is connected to an air inlet pipe 40 and a reagent container 50; A first valve 70 is provided between the first through hole 21 and the air intake pipe 40; A second valve 80 is provided between the first through hole 21 and the reagent container 50. The second through hole 22 is connected to an air outlet pipe 60; A third valve 90 is provided between the second through hole 22 and the air outlet pipe 60; The second reaction container 30 contains a magnetic material 100 .

Images