CN114486614A - Method for detecting content of magnesium hydroxide in brucite - Google Patents
Method for detecting content of magnesium hydroxide in brucite Download PDFInfo
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- CN114486614A CN114486614A CN202210057547.XA CN202210057547A CN114486614A CN 114486614 A CN114486614 A CN 114486614A CN 202210057547 A CN202210057547 A CN 202210057547A CN 114486614 A CN114486614 A CN 114486614A
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- brucite
- magnesium hydroxide
- thermogravimetric
- content
- weight loss
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- 229910052599 brucite Inorganic materials 0.000 title claims abstract description 57
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 44
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 44
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000001514 detection method Methods 0.000 claims abstract description 25
- 238000002411 thermogravimetry Methods 0.000 claims abstract description 25
- 230000004580 weight loss Effects 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 10
- 238000000354 decomposition reaction Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- ZRBROGSAUIUIJE-UHFFFAOYSA-N azanium;azane;chloride Chemical compound N.[NH4+].[Cl-] ZRBROGSAUIUIJE-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- AMMWFYKTZVIRFN-UHFFFAOYSA-N sodium 3-hydroxy-4-[(1-hydroxynaphthalen-2-yl)diazenyl]-7-nitronaphthalene-1-sulfonic acid Chemical compound [Na+].C1=CC=CC2=C(O)C(N=NC3=C4C=CC(=CC4=C(C=C3O)S(O)(=O)=O)[N+]([O-])=O)=CC=C21 AMMWFYKTZVIRFN-UHFFFAOYSA-N 0.000 description 1
- ORFSSYGWXNGVFB-UHFFFAOYSA-N sodium 4-amino-6-[[4-[4-[(8-amino-1-hydroxy-5,7-disulfonaphthalen-2-yl)diazenyl]-3-methoxyphenyl]-2-methoxyphenyl]diazenyl]-5-hydroxynaphthalene-1,3-disulfonic acid Chemical compound COC1=C(C=CC(=C1)C2=CC(=C(C=C2)N=NC3=C(C4=C(C=C3)C(=CC(=C4N)S(=O)(=O)O)S(=O)(=O)O)O)OC)N=NC5=C(C6=C(C=C5)C(=CC(=C6N)S(=O)(=O)O)S(=O)(=O)O)O.[Na+] ORFSSYGWXNGVFB-UHFFFAOYSA-N 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention belongs to the technical field of brucite detection, and particularly relates to a method for detecting the content of magnesium hydroxide in brucite. The invention provides a method for detecting the content of magnesium hydroxide in brucite, which comprises the following steps: performing thermogravimetric analysis on the brucite to be detected to obtain a thermogravimetric curve, and obtaining the moisture weight loss rate of the brucite to be detected from the thermogravimetric curve; calculating to obtain the mass content of magnesium hydroxide in brucite by using a formula I; the thermogravimetric curve temperature interval of the water weight loss rate is 300-650 ℃. The determination method provided by the invention is simple to operate and strong in operability, the whole determination process takes about 1 hour, and compared with the national standard determination method, the determination method improves the detection efficiency and can provide data for daily production detection in time.
Description
Technical Field
The invention belongs to the technical field of brucite detection, and particularly relates to a method for detecting the content of magnesium hydroxide in brucite.
Background
Currently, brucite is Mg (OH)2The content is generally detected according to the national standard (HG/T3607-2007)The determination of the content of the 5.4 magnesium hydroxide is carried out, and the determination method specifically comprises the following steps: about 7.0g of sample was weighed to the nearest 0.0002 g. Placing the sample in a 250mL beaker, adding a small amount of water for wetting, covering a watch glass, adding a proper amount of hydrochloric acid solution (about 45mL) to dissolve the sample, and heating and boiling the sample on an electric furnace for 3-5 min. After filtration through medium-rate filter paper while hot, it was washed with hot water until free of chloride ions (checked with silver nitrate solution). After cooling, the filtrate and wash solution were transferred to a 500mL volumetric flask, diluted to the mark with water and shaken up. Then, 25mL of the above solution was pipetted into a 250mL volumetric flask, diluted to the mark with water and shaken up. And transferring 25mL of the diluted solution by using a pipette, adding 50mL of water, 5mL of triethanolamine solution, 10mL of ammonia-ammonium chloride buffer solution A and about 0.1g of chrome black T indicator into a 250mL conical flask, titrating by using an EDTA standard solution until the solution is changed from purple red to pure blue, namely the end point, calculating the content of magnesium oxide, and converting the content of magnesium hydroxide from the content of magnesium oxide according to the molecular mass. However, the method has long testing time, more operation steps and more complexity, and is not suitable for daily detection.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for detecting the content of magnesium hydroxide in brucite. The detection method provided by the invention is simple to operate and strong in operability, and greatly improves the detection efficiency.
The invention provides a method for measuring the content of magnesium hydroxide in brucite, which comprises the following steps:
performing thermogravimetric analysis on the brucite to be detected to obtain a thermogravimetric curve, and obtaining the water weight loss rate of the brucite to be detected according to the thermogravimetric curve;
calculating to obtain the mass content of magnesium hydroxide in brucite by using a formula I;
the temperature interval of the thermogravimetric curve of the water weight loss rate is 300-650 ℃.
Preferably, the temperature rise rate of the thermogravimetric analysis is 5 ℃/min to 20 ℃/min.
Preferably, the temperature rise range of the thermogravimetric analysis is 25-800 ℃.
Preferably, the thermogravimetric analysis is performed under nitrogen.
Preferably, the flow rate of the nitrogen is 40-50 mL/min.
Preferably, the brucite to be detected is brucite powder; the particle size of the brucite powder is 100-300 meshes.
Preferably, the amount of the brucite is 1/3-1/2 of the volume of the container for thermogravimetric analysis.
The invention provides a method for measuring the content of magnesium hydroxide in brucite, which comprises the following steps: performing thermogravimetric analysis on the brucite to be detected to obtain a thermogravimetric curve, and obtaining the water weight loss rate of the brucite to be detected according to the thermogravimetric curve; using the formula:
calculating to obtain the content of magnesium hydroxide; the temperature interval of the thermogravimetric curve of the water molecule weight loss rate is 300-650 ℃. The determination method provided by the invention is simple to operate and strong in operability, improves the detection efficiency compared with the determination method of the national standard (HG/T3607-2007), and can provide data for daily production detection in time. Meanwhile, the method does not need to adopt the steps of washing, titrating and the like by using various solutions in a national standard (HG/T3607-2007) determination method in the determination process, so that the use of chemical reagents is saved, the detection cost is reduced, and the pollution of solution discharge to the environment in the determination process is avoided. Meanwhile, in the determination process, the national standard (HG/T3607-2007) determination method is not needed to be adopted to dry the sample to constant weight, so that the energy consumption is greatly reduced, and the detection time is shortened.
Furthermore, the invention limits the heating rate of the thermogravimetric analysis to be 5-20 ℃/min, so that the whole test process can be completed within 1 hour, and the detection efficiency is improved.
Detailed Description
The invention provides a method for detecting the content of magnesium hydroxide in brucite, which comprises the following steps:
performing thermogravimetric analysis on the brucite to be detected to obtain a thermogravimetric curve, and obtaining the water weight loss rate of the brucite to be detected according to the thermogravimetric curve; calculating to obtain the mass content of the magnesium hydroxide in the brucite by using a formula I; the mass percentage content of the magnesium hydroxide is 3.222 multiplied by the weight loss ratio of water as formula I; the temperature interval of the thermogravimetric curve of the water weight loss rate is 300-650 ℃.
In the present invention, the starting materials used in the present invention are preferably commercially available products unless otherwise specified.
The method comprises the steps of carrying out thermogravimetric analysis on brucite to be detected to obtain a thermogravimetric curve, and obtaining the moisture weight loss rate of the brucite to be detected according to the thermogravimetric curve.
In the embodiment of the present invention, in order to determine the temperature range of the brucite with the loss of water, the following scheme is preferably performed:
thermogravimetric analysis is carried out on the high-purity brucite with known magnesium hydroxide content to obtain a thermogravimetric curve and a water molecule weight loss rate, which are marked as A%. The temperature range of the thermogravimetric analysis is 25-800 ℃, and the heating rate is 10 ℃/min.
Obtaining a first-order derivation of the obtained thermogravimetric curve to obtain a DTG curve;
determining the decomposition initial temperature of the magnesium hydroxide from the decomposition peak position in the DTG curve, wherein the decomposition initial temperature is 300 ℃; the temperature corresponding to the water molecule weight loss rate A% in the DTG curve is the temperature for completely decomposing the magnesium hydroxide and is 650 ℃.
In the invention, the determination of the water molecule weight loss rate temperature interval is used for largely verifying brucite with different magnesium hydroxide contents, and the embodiment 1 is only one of the brucite.
In the invention, the brucite to be detected is preferably used in the form of brucite powder; the particle size of the brucite powder is preferably 100-300 meshes, and is further preferably 150-250 meshes. In the invention, the usage amount of the brucite is preferably 1/3-1/2, and more preferably 1/3 of the volume of the container for thermogravimetric analysis. In the present invention, the vessel for thermogravimetric analysis is preferably a standard aluminum crucible of 70. mu.L.
In the examples of the present invention, an equivalent standard reference crucible was also used in the thermogravimetric analysis.
In the present invention, the thermogravimetric analysis is performed in a thermogravimetric analyzer.
In the present invention, the thermogravimetric analysis is preferably performed in a nitrogen atmosphere; the flow rate of the nitrogen is preferably 40-50 mL/min, and more preferably 50 mL/min. In the present invention, the heating rate of thermogravimetric analysis is preferably 5 ℃/min to 20 ℃/min, and in the embodiment of the present invention, the heating rate can be specifically 5 ℃/min, 10 ℃/min, 15 ℃/min or 20 ℃/min.
In the invention, the temperature rise range of the thermogravimetric curve is preferably 25-800 ℃, and the termination temperature of the temperature interval is set to 800 ℃ in order to ensure the complete water loss of magnesium hydroxide in brucite.
The invention calculates the magnesium hydroxide mass content in brucite by using the mass percentage content of magnesium hydroxide which is 3.222 multiplied by the water weight loss ratio.
In the invention, in the range of the thermogravimetric temperature interval, magnesium hydroxide in brucite is decomposed to generate magnesium oxide and water, the water is vaporized, and the water loss rate of water molecules is shown on a thermogravimetric curve, namely the mass ratio of the water generated by decomposing magnesium hydroxide to the initial brucite. According to the law of conservation of mass, the mass of magnesium hydroxide is 58/18 times (the ratio of the relative molecular weight of magnesium hydroxide to the relative molecular weight of water molecules) of the mass of water produced by its decomposition, and therefore, the mass percentage formula of magnesium hydroxide is determined as follows:
in the embodiment of the present invention, the ratio of the relative molecular weight of magnesium hydroxide to the relative molecular weight of water molecules is preferably 3.222.
The principle of the detection method provided by the invention is as follows: brucite containing magnesium hydroxide primarily undergoes release of water molecules at 25 ℃ to 300 ℃; the breaking of Mg-OH bonds occurs at 300-400 ℃; forming a dehydration intermediate product at 400-600 ℃; the formation of intermediate products and end products MgO occurs at 600-800 ℃. The amount of magnesium hydroxide can be calculated by the amount of water molecules generated by decomposing magnesium hydroxide according to the mass conservation law by utilizing the thermal decomposition principle of magnesium hydroxide.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
According to the invention, samples with magnesium hydroxide contents of 0, 30.3 +/-0.1%, 49.8 +/-0.2%, 79.7 +/-0.4%, 90.9 +/-0.5% and 99.2 +/-0.7% after being determined by an HG/T3607-2007 determination method are respectively set as sample 1, sample 2, sample 3, sample 4, sample 5 and sample 6.
Example 1
Determining a thermogravimetric curve temperature interval of the water weight loss rate:
thermogravimetric analysis is carried out on brucite with the known magnesium hydroxide content of 99.5%, and a thermogravimetric curve and the weight loss rate of water molecules are obtained, wherein the weight loss rate is 30.88%.
And (3) performing horizontal step by taking the temperature and the water molecule weight loss rate in the obtained thermogravimetric curve, and taking the water molecule weight loss rate as a vertical coordinate and the temperature as a horizontal coordinate to obtain a DTG curve.
The decomposition initial temperature of the magnesium hydroxide can be determined from the decomposition peak position in the DTG curve and is 300 ℃; the temperature corresponding to 30.88% of the weight loss rate of water molecules in the DTG curve is the temperature for completely decomposing magnesium hydroxide, and is 650 ℃.
Example 2
Placing a 70uL standard aluminum crucible at the position of a sensor sample crucible of a thermogravimetric analyzer, and clearing; weighing brucite powder to be detected (the particle size of the brucite powder is 200 meshes) with the volume of about 1/3 standard aluminum crucible, and accurately obtaining the brucite powder to be detected to be 0.0001 mg;
placing the weighed sample in a sample crucible position, and simultaneously placing an empty 70uL standard aluminum crucible in a reference crucible position, wherein the temperature range is set from 25 ℃ to 800 ℃, the temperature rise rate is 5 ℃/min, and the atmosphere is N2The gas flow is 50 mL/min; and performing thermogravimetric analysis to obtain a thermogravimetric curve, and analyzing to obtain the water weight loss rate in the temperature range of 300-650 ℃ of the thermogravimetric curve.
The formula is adopted: and (3) calculating the mass percent of the magnesium hydroxide, wherein the mass percent of the magnesium hydroxide is 3.222 multiplied by the weight loss ratio of water molecules.
Samples 1 to 6 were all tested by the method of example 1, and the two experiments were performed in parallel, and the average value was taken.
Example 3
Example 3 differs from example 1 only in that the temperature rise rate is 10 ℃/min.
Example 4
Example 4 differs from example 1 only in that the temperature rise rate is 15 deg.C/min.
Example 5
Example 5 differs from example 1 only in that the temperature rise rate is 20 ℃/min.
The detection results of examples 2-5 on magnesium hydroxide in brucite are compared with the detection results on magnesium hydroxide in brucite by adopting the national standard (HG/T3607-2007) shown in Table 1.
Table 1 comparison of detection results of examples 2-5 and national standard (HG/T3607-2007)
The data in the table show that the detection method provided by the invention has no significant difference from the data detected by the detection method adopted by the national standard (HG/T3607-2007), so that the detection method provided by the invention can be proved to be capable of accurately detecting the content of magnesium hydroxide in brucite.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A method for detecting the content of magnesium hydroxide in brucite is characterized by comprising the following steps:
performing thermogravimetric analysis on the brucite to be detected to obtain a thermogravimetric curve, and obtaining the water weight loss rate of the brucite to be detected according to the thermogravimetric curve;
calculating to obtain the mass content of magnesium hydroxide in brucite by using a formula I;
the temperature interval of the thermogravimetric curve of the water weight loss rate is 300-650 ℃.
2. The detection method according to claim 1, wherein the temperature increase rate of the thermogravimetric analysis is 5 ℃/min to 20 ℃/min.
3. The detection method according to claim 1, wherein the temperature rise range of the thermogravimetric analysis is 25 to 800 ℃.
4. The detection method according to claim 1, wherein the thermogravimetric analysis is carried out in nitrogen.
5. The detection method according to claim 4, wherein the flow rate of the nitrogen gas is 40 to 50 mL/min.
6. The detection method according to claim 1, wherein the brucite to be detected is a brucite powder; the particle size of the brucite powder is 100-300 meshes.
7. The detection method according to claim 1 or 6, wherein the brucite is used in an amount of 1/3 to 1/2 times the volume of the container for thermogravimetric analysis.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210057547.XA CN114486614A (en) | 2022-01-19 | 2022-01-19 | Method for detecting content of magnesium hydroxide in brucite |
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| CN202210057547.XA CN114486614A (en) | 2022-01-19 | 2022-01-19 | Method for detecting content of magnesium hydroxide in brucite |
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| JP2005043086A (en) * | 2003-07-23 | 2005-02-17 | Nippon Steel Corp | Evaluation method of resistivity to slaking of magnesia-containing monolithic refractory |
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| JP2014209101A (en) * | 2013-03-26 | 2014-11-06 | Ｊｆｅスチール株式会社 | Quantifying method for magnesium oxide and magnesium hydroxide in inorganic compound sample |
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2022
- 2022-01-19 CN CN202210057547.XA patent/CN114486614A/en active Pending
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| JP2005043086A (en) * | 2003-07-23 | 2005-02-17 | Nippon Steel Corp | Evaluation method of resistivity to slaking of magnesia-containing monolithic refractory |
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| JP2014209101A (en) * | 2013-03-26 | 2014-11-06 | Ｊｆｅスチール株式会社 | Quantifying method for magnesium oxide and magnesium hydroxide in inorganic compound sample |
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| CN106885752A (en) * | 2017-03-24 | 2017-06-23 | 中国建筑材料科学研究总院 | The assay method of periclase weight/mass percentage composition in cement |
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