CN111624170A - Method for detecting iron content in calcite and dolomite - Google Patents
Method for detecting iron content in calcite and dolomite Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 51
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 34
- 229910021532 Calcite Inorganic materials 0.000 title claims abstract description 26
- 229910000514 dolomite Inorganic materials 0.000 title claims abstract description 23
- 239000010459 dolomite Substances 0.000 title claims abstract description 23
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 69
- 238000001514 detection method Methods 0.000 claims abstract description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 30
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 27
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 22
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004327 boric acid Substances 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 33
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 32
- 238000001816 cooling Methods 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 18
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- 229910052697 platinum Inorganic materials 0.000 claims description 16
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 16
- 238000002835 absorbance Methods 0.000 claims description 10
- 238000005070 sampling Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 8
- 229960005070 ascorbic acid Drugs 0.000 claims description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims description 8
- 239000011668 ascorbic acid Substances 0.000 claims description 8
- 238000007865 diluting Methods 0.000 claims description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002372 labelling Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000012046 mixed solvent Substances 0.000 claims description 8
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000001632 sodium acetate Substances 0.000 claims description 8
- 235000017281 sodium acetate Nutrition 0.000 claims description 8
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 abstract description 4
- 238000004737 colorimetric analysis Methods 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
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- 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
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- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- 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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- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention provides a method for detecting the content of iron in calcite and dolomite, which relates to the field of detection of the content of iron in calcite and dolomite, and comprises the following raw materials: hydrochloric acid, hydrofluoric acid, anhydrous sodium carbonate and boric acid, and the method comprises the following steps: (1) instrument preparation, (2) reagent preparation, (3) sample selection, (4) reagent grinding, dissolution and (5) colorimetry. According to the method for detecting the content of iron in calcite and dolomite, the high-grade pure reagent is adopted to replace the analytical pure reagent, so that the interference of trace iron elements brought by the analytical pure reagent on the monitoring result is reduced in the sample treatment process, the accuracy of data is improved, the detection result is stable, the detection data can be reported in time, and the detection result is scientific and accurate.
Description
Technical Field
The invention relates to the field of detection of iron content in calcite and dolomite, and particularly relates to a method for detecting iron content in calcite and dolomite.
Background
At present, the entrance raw materials are calcite and dolomite iron content detection structures which fluctuate in different time, detection results cannot be confirmed in time, a supplier has a doubt on the monitoring results, secondary rechecking is needed to influence the detection report issuing speed, and therefore workers improve the detection method, and the problems are solved.
The newly researched detection method utilizes the increase of sampling base number and the secondary quartering method sampling standard, and simultaneously changes the purity of the medicine reagent, thereby improving the stability and accuracy of the detection result.
Disclosure of Invention
The invention aims to provide a method for detecting the iron content in calcite and dolomite, so as to solve the technical problems.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for detecting the iron content in calcite and dolomite is characterized by comprising the following steps: the feed is prepared from the following raw materials in parts by weight:
hydrochloric acid, hydrofluoric acid, anhydrous sodium carbonate and boric acid.
Preferably, the method for detecting the iron content in calcite and dolomite is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing an instrument: UV-1750 UV-vis spectrophotometer, analytical balance (parts per million standard);
(2) preparation of reagents: a high-grade pure reagent of hydrochloric acid, anhydrous sodium carbonate, hydrofluoric acid and boric acid;
(3) selecting a sample: according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theories, sampling a sample by adopting a secondary quartering method, and dividing the sample to 100 g;
(4) grinding and dissolving a reagent: grinding and crushing the sample obtained in the step (3) by a grinder, drying the sample in a drying box for 2-3h after the particle diameter of the crushed sample is less than or equal to 74um, taking out the dried sample and placing the dried sample in a dryer for cooling until the temperature reaches the room temperature, thereby obtaining a reagent;
then weighing 3.5-4.5g of dried sample, placing the sample in a platinum pot, adding a mixed solvent of 4g of sodium carbonate and 2 g of boric acid, mixing uniformly, placing the mixture in a platinum crucible, dissolving the mixture at the temperature of 900-950 ℃ for 15-20min, placing the mixture in a dryer for cooling until the temperature reaches room temperature, placing the obtained soluble block in a beaker containing 10-15ml of hydrochloric acid solution, cooling to the room temperature after the soluble block and the mixed solution are completely dissolved, placing the soluble block in a volumetric flask, shaking uniformly to obtain a required reagent, and transferring the reagent into a cuvette;
(5) color comparison: weighing 0mg, 2mg, 4mg, 6mg, 8mg, 10mg, 20mg, 50mg and 100mg ferric oxide standard in a colorimetric tube by using an analytical balance, simultaneously adding 5ml of 25% sodium acetate solution and 1ml of 1% ascorbic acid solution with the reagent prepared in the step (4), shaking uniformly, standing for 5min, diluting until the scales are balanced, standing overnight, using an ultraviolet visible light spectrophotometer, taking the clear liquid at the wavelength of 510nm, simultaneously measuring the absorbance with the standard series, and drawing a labeling curve.
Preferably, the specific steps of step (3) are as follows:
A. firstly, taking a mixed sample, dividing the mixed sample into four parts at a time, and taking 500g of one part;
B. then, 500g of the solution was split into four portions, 100g of which were taken out.
Preferably, the temperature of the drying box in the step (4) is 105-110 ℃.
Preferably, the cooling in the step (4) is carried out to room temperature, and the specific temperature is 20-25 ℃.
Preferably, the ultraviolet-visible spectrophotometer used in the step (5) is a UV-1750 ultraviolet-visible spectrophotometer.
The invention has the beneficial effects that:
the invention designs a method for detecting the iron content in calcite and dolomite, firstly, a superior pure reagent is adopted to replace an analytical pure reagent, in the sample treatment process, the interference of trace iron elements brought by the analytical pure reagent on a monitoring result is reduced, the accuracy of data is improved, the detection result is stable, the detection data can be reported in time, the detection result is scientific and accurate, secondly, according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theory, and a quadratic quartile method is adopted to sample the sample, the method can ensure the representativeness and feasibility of the sample, thereby reducing the deviation caused by the non-uniformity of the sample, simultaneously increasing the sample weight of the sample to be detected, increasing the original 0.5g to 4g, ensuring that a working curve obtained by the iron elements in the sample in a spectrophotometric weighing is in a standard working curve, and finally, a method for data comparison is adopted, and comparing the experimental detection data with the submission data to determine the validity and authenticity of the laboratory data, and finding out that the improved detection method is further improved in the aspects of data stability and authenticity through a large amount of experimental data.
Drawings
FIG. 1 is a graph of iron concentration versus absorbance with concentration on the abscissa and absorbance on the ordinate.
Detailed Description
The present invention will be further described with reference to specific embodiments for the purpose of facilitating an understanding of technical means, characteristics of creation, objectives and functions realized by the present invention, but the following embodiments are only preferred embodiments of the present invention, and are not intended to be exhaustive. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention. The experimental methods in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
The method for detecting the iron content in the calcite comprises the following steps:
(1) preparing an instrument: UV-1750 UV-vis spectrophotometer, analytical balance (parts per million standard);
(2) preparation of reagents: a high-grade pure reagent of hydrochloric acid, anhydrous sodium carbonate, hydrofluoric acid and boric acid;
(3) selecting a sample: according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theories, sampling a sample by adopting a secondary quartering method, and dividing the sample to 100 g;
(4) grinding and dissolving a reagent: grinding and crushing the sample obtained in the step (3) by a grinding machine, drying the sample in a drying box for 2 hours after the particle diameter of the crushed sample is less than or equal to 74um, taking out the dried sample and placing the dried sample in a dryer for cooling until the temperature reaches the room temperature to obtain a reagent;
then weighing 3.5 dried samples, placing the samples into a platinum pot, adding a mixed solvent of 4g of sodium carbonate and 2 g of boric acid, mixing and uniformly mixing the samples, placing the mixture into a platinum crucible, dissolving the mixture for 15min at 900 ℃, placing the mixture into a dryer, cooling the mixture until the temperature reaches room temperature, placing the obtained dissolved block into a beaker containing 10ml of hydrochloric acid solution, cooling the mixture to the room temperature after the melted block and the mixed solution are completely dissolved, placing the mixture into a volumetric flask, shaking the mixture uniformly to obtain a required reagent, and transferring the reagent into a cuvette;
(5) color comparison: weighing 0mg, 2mg, 4mg, 6mg, 8mg, 10mg, 20mg, 50mg and 100mg ferric oxide standard in a colorimetric tube by using an analytical balance, simultaneously adding 5ml of 25% sodium acetate solution and 1ml of 1% ascorbic acid solution with the reagent prepared in the step (4), shaking uniformly, standing for 5min, diluting until the scales are balanced, standing overnight, using an ultraviolet visible light spectrophotometer, taking the clear liquid at the wavelength of 510nm, simultaneously measuring the absorbance with the standard series, and drawing a labeling curve.
Example 2
The method for detecting the iron content in the calcite comprises the following steps:
(1) preparing an instrument: UV-1750 UV-vis spectrophotometer, analytical balance (parts per million standard);
(2) preparation of reagents: a high-grade pure reagent of hydrochloric acid, anhydrous sodium carbonate, hydrofluoric acid and boric acid;
(3) selecting a sample: according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theories, sampling a sample by adopting a secondary quartering method, and dividing the sample to 100 g;
(4) grinding and dissolving a reagent: grinding and crushing the sample obtained in the step (3) by a grinder, drying the sample in a drying box for 2.5 hours after the particle diameter of the crushed sample is less than or equal to 74um, taking out the dried sample and placing the dried sample in a dryer for cooling until the temperature reaches the room temperature, thereby obtaining a reagent;
weighing 4.0g of dried sample, placing the sample in a platinum pot, adding a mixed solvent of 4g of sodium carbonate and 2 g of boric acid, mixing uniformly, placing the mixture in a platinum crucible, dissolving the mixture at 925 ℃ for 18min, placing the mixture in a dryer, cooling the mixture until the temperature reaches room temperature, placing the obtained dissolved block in a beaker containing 13ml of hydrochloric acid solution, cooling the dissolved block to the room temperature after the melted block and the mixed solution are completely dissolved, placing the dissolved block in a volumetric flask, shaking the dissolved block uniformly to obtain a required reagent, and transferring the reagent into a cuvette;
(5) color comparison: weighing 0mg, 2mg, 4mg, 6mg, 8mg, 10mg, 20mg, 50mg and 100mg ferric oxide standard in a colorimetric tube by using an analytical balance, simultaneously adding 5ml of 25% sodium acetate solution and 1ml of 1% ascorbic acid solution with the reagent prepared in the step (4), shaking uniformly, standing for 5min, diluting until the scales are balanced, standing overnight, using an ultraviolet visible light spectrophotometer, taking the clear liquid at the wavelength of 510nm, simultaneously measuring the absorbance with the standard series, and drawing a labeling curve.
Example 3
The method for detecting the iron content in the calcite comprises the following steps:
(1) preparing an instrument: UV-1750 UV-vis spectrophotometer, analytical balance (parts per million standard);
(2) preparation of reagents: a high-grade pure reagent of hydrochloric acid, anhydrous sodium carbonate, hydrofluoric acid and boric acid;
(3) selecting a sample: according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theories, sampling a sample by adopting a secondary quartering method, and dividing the sample to 100 g;
(4) grinding and dissolving a reagent: grinding and crushing the sample obtained in the step (3) by a grinder, drying the sample in a drying box for 3 hours after the particle diameter of the crushed sample is less than or equal to 74um, taking out the dried sample and placing the dried sample in a dryer for cooling until the temperature reaches the room temperature, thereby obtaining a reagent;
weighing 4.5g of dried sample, placing the sample in a platinum pot, adding a mixed solvent of 4g of sodium carbonate and 2 g of boric acid, mixing uniformly, placing the mixture in a platinum crucible, dissolving the mixture at 950 ℃ for 20min, placing the mixture in a dryer, cooling the mixture until the temperature reaches room temperature, placing the obtained dissolved block in a beaker containing 15ml of hydrochloric acid solution, cooling the dissolved block to the room temperature after the melted block and the mixed solution are completely dissolved, placing the dissolved block in a volumetric flask, shaking the dissolved block uniformly to obtain a required reagent, and transferring the reagent into a cuvette;
(5) color comparison: weighing 0mg, 2mg, 4mg, 6mg, 8mg, 10mg, 20mg, 50mg and 100mg ferric oxide standard in a colorimetric tube by using an analytical balance, simultaneously adding 5ml of 25% sodium acetate solution and 1ml of 1% ascorbic acid solution with the reagent prepared in the step (4), shaking uniformly, standing for 5min, diluting until the scales are balanced, standing overnight, using an ultraviolet visible light spectrophotometer, taking the clear liquid at the wavelength of 510nm, simultaneously measuring the absorbance with the standard series, and drawing a labeling curve.
Example 4
The method for detecting the content of iron in dolomite comprises the following steps:
(1) preparing an instrument: UV-1750 UV-vis spectrophotometer, analytical balance (parts per million standard);
(2) preparation of reagents: a high-grade pure reagent of hydrochloric acid, anhydrous sodium carbonate, hydrofluoric acid and boric acid;
(3) selecting a sample: according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theories, sampling a sample by adopting a secondary quartering method, and dividing the sample to 100 g;
(4) grinding and dissolving a reagent: grinding and crushing the sample obtained in the step (3) by a grinding machine, drying the sample in a drying box for 2 hours after the particle diameter of the crushed sample is less than or equal to 74um, taking out the dried sample and placing the dried sample in a dryer for cooling until the temperature reaches the room temperature to obtain a reagent;
then weighing 3.5g of dried sample, placing the sample in a platinum pot, adding a mixed solvent of 4g of sodium carbonate and 2 g of boric acid, mixing uniformly, placing the mixture in a platinum crucible, dissolving the mixture for 15min at 900 ℃, placing the mixture in a dryer, cooling the mixture until the temperature reaches room temperature, placing the obtained dissolved block in a beaker containing 10ml of hydrochloric acid solution, cooling the dissolved block to the room temperature after the melted block and the mixed solution are completely dissolved, placing the dissolved block in a volumetric flask, shaking the dissolved block uniformly to obtain a required reagent, and transferring the reagent into a cuvette;
(5) color comparison: weighing 0mg, 2mg, 4mg, 6mg, 8mg, 10mg, 20mg, 50mg and 100mg ferric oxide standard in a colorimetric tube by using an analytical balance, simultaneously adding 5ml of 25% sodium acetate solution and 1ml of 1% ascorbic acid solution with the reagent prepared in the step (4), shaking uniformly, standing for 5min, diluting until the scales are balanced, standing overnight, using an ultraviolet visible light spectrophotometer, taking the clear liquid at the wavelength of 510nm, simultaneously measuring the absorbance with the standard series, and drawing a labeling curve.
Example 5
The method for detecting the content of iron in dolomite comprises the following steps:
(1) preparing an instrument: UV-1750 UV-vis spectrophotometer, analytical balance (parts per million standard);
(2) preparation of reagents: a high-grade pure reagent of hydrochloric acid, anhydrous sodium carbonate, hydrofluoric acid and boric acid;
(3) selecting a sample: according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theories, sampling a sample by adopting a secondary quartering method, and dividing the sample to 100 g;
(4) grinding and dissolving a reagent: grinding and crushing the sample obtained in the step (3) by a grinder, drying the sample in a drying box for 2.5 hours after the particle diameter of the crushed sample is less than or equal to 74um, taking out the dried sample and placing the dried sample in a dryer for cooling until the temperature reaches the room temperature, thereby obtaining a reagent;
weighing 4.0g of dried sample, placing the sample in a platinum pot, adding a mixed solvent of 4g of sodium carbonate and 2 g of boric acid, mixing uniformly, placing the mixture in a platinum crucible, dissolving the mixture at 925 ℃ for 18min, placing the mixture in a dryer, cooling the mixture until the temperature reaches room temperature, placing the obtained dissolved block in a beaker containing 13ml of hydrochloric acid solution, cooling the dissolved block to the room temperature after the melted block and the mixed solution are completely dissolved, placing the dissolved block in a volumetric flask, shaking the dissolved block uniformly to obtain a required reagent, and transferring the reagent into a cuvette;
(5) color comparison: weighing 0mg, 2mg, 4mg, 6mg, 8mg, 10mg, 20mg, 50mg and 100mg ferric oxide standard in a colorimetric tube by using an analytical balance, simultaneously adding 5ml of 25% sodium acetate solution and 1ml of 1% ascorbic acid solution with the reagent prepared in the step (4), shaking uniformly, standing for 5min, diluting until the scales are balanced, standing overnight, using an ultraviolet visible light spectrophotometer, taking the clear liquid at the wavelength of 510nm, simultaneously measuring the absorbance with the standard series, and drawing a labeling curve.
Example 6
The method for detecting the content of iron in dolomite comprises the following steps:
(1) preparing an instrument: UV-1750 UV-vis spectrophotometer, analytical balance (parts per million standard);
(2) preparation of reagents: a high-grade pure reagent of hydrochloric acid, anhydrous sodium carbonate, hydrofluoric acid and boric acid;
(3) selecting a sample: according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theories, sampling a sample by adopting a secondary quartering method, and dividing the sample to 100 g;
(4) grinding and dissolving a reagent: grinding and crushing the sample obtained in the step (3) by a grinder, drying the sample in a drying box for 3 hours after the particle diameter of the crushed sample is less than or equal to 74um, taking out the dried sample and placing the dried sample in a dryer for cooling until the temperature reaches the room temperature, thereby obtaining a reagent;
weighing 4.5g of dried sample, placing the sample in a platinum pot, adding a mixed solvent of 4g of sodium carbonate and 2 g of boric acid, mixing uniformly, placing the mixture in a platinum crucible, dissolving the mixture at 950 ℃ for 20min, placing the mixture in a dryer, cooling the mixture until the temperature reaches room temperature, placing the obtained dissolved block in a beaker containing 15ml of hydrochloric acid solution, cooling the dissolved block to the room temperature after the melted block and the mixed solution are completely dissolved, placing the dissolved block in a volumetric flask, shaking the dissolved block uniformly to obtain a required reagent, and transferring the reagent into a cuvette;
(5) color comparison: weighing 0mg, 2mg, 4mg, 6mg, 8mg, 10mg, 20mg, 50mg and 100mg ferric oxide standard in a colorimetric tube by using an analytical balance, simultaneously adding 5ml of 25% sodium acetate solution and 1ml of 1% ascorbic acid solution with the reagent prepared in the step (4), shaking uniformly, standing for 5min, diluting until the scales are balanced, standing overnight, using an ultraviolet visible light spectrophotometer, taking the clear liquid at the wavelength of 510nm, simultaneously measuring the absorbance with the standard series, and drawing a labeling curve.
Selecting a representative pure white calcite sample, comparing the method with an external test result, and obtaining the following test results by the method for testing the iron content in calcite and dolomite designed in the embodiments 1-6:
analyzing experimental data:
as can be seen from the table above, the method for determining the iron content in the high-purity calcite is basically consistent with the feedback result of the sample to be detected, and the detection requirement of the iron in the high-purity calcite is met.
The invention has the beneficial effects that:
the invention designs a method for detecting the iron content in calcite and dolomite, firstly, a superior pure reagent is adopted to replace an analytical pure reagent, in the sample treatment process, the interference of trace iron elements brought by the analytical pure reagent on a monitoring result is reduced, the accuracy of data is improved, the detection result is stable, the detection data can be reported in time, the detection result is scientific and accurate, secondly, according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theory, and a quadratic quartile method is adopted to sample the sample, the method can ensure the representativeness and feasibility of the sample, thereby reducing the deviation caused by the non-uniformity of the sample, simultaneously increasing the sample weight of the sample to be detected, increasing the original 0.5g to 4g, ensuring that a working curve obtained by the iron elements in the sample in a spectrophotometric weighing is in a standard working curve, and finally, a method for data comparison is adopted, and comparing the experimental detection data with the submission data to determine the validity and authenticity of the laboratory data, and finding out that the improved detection method is further improved in the aspects of data stability and authenticity through a large amount of experimental data.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A method for detecting the iron content in calcite and dolomite is characterized by comprising the following steps: the feed is prepared from the following raw materials in parts by weight:
hydrochloric acid, hydrofluoric acid, anhydrous sodium carbonate and boric acid.
2. The method for detecting the iron content in calcite and dolomite according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) preparing an instrument: UV-1750 UV-vis spectrophotometer, analytical balance (parts per million standard);
(2) preparation of reagents: a high-grade pure reagent of hydrochloric acid, anhydrous sodium carbonate, hydrofluoric acid and boric acid;
(3) selecting a sample: according to GB/T3286, GB/T5762 and GB/T2007 national standard detection theories, sampling a sample by adopting a secondary quartering method, and dividing the sample to 100 g;
(4) grinding and dissolving a reagent: grinding and crushing the sample obtained in the step (3) by a grinder, drying the sample in a drying box for 2-3h after the particle diameter of the crushed sample is less than or equal to 74um, taking out the dried sample and placing the dried sample in a dryer for cooling until the temperature reaches the room temperature, thereby obtaining a reagent;
then weighing 3.5-4.5g of dried sample, placing the sample in a platinum pot, adding a mixed solvent of 4g of sodium carbonate and 2 g of boric acid, mixing uniformly, placing the mixture in a platinum crucible, dissolving the mixture at the temperature of 900-950 ℃ for 15-20min, placing the mixture in a dryer for cooling until the temperature reaches room temperature, placing the obtained soluble block in a beaker containing 10-15ml of hydrochloric acid solution, cooling to the room temperature after the soluble block and the mixed solution are completely dissolved, placing the soluble block in a volumetric flask, shaking uniformly to obtain a required reagent, and transferring the reagent into a cuvette;
(5) color comparison: weighing 0mg, 2mg, 4mg, 6mg, 8mg, 10mg, 20mg, 50mg and 100mg ferric oxide standard in a colorimetric tube by using an analytical balance, simultaneously adding 5ml of 25% sodium acetate solution and 1ml of 1% ascorbic acid solution with the reagent prepared in the step (4), shaking uniformly, standing for 5min, diluting until the scales are balanced, standing overnight, using an ultraviolet visible light spectrophotometer, taking the clear liquid at the wavelength of 510nm, simultaneously measuring the absorbance with the standard series, and drawing a labeling curve.
3. The method for detecting the iron content in calcite and dolomite according to claim 2, wherein the method comprises the following steps: the specific steps of the step (3) are as follows:
A. firstly, taking a mixed sample, dividing the mixed sample into four parts at a time, and taking 500g of one part;
B. then, 500g of the solution was split into four portions, 100g of which were taken out.
4. The method for detecting the iron content in calcite and dolomite according to claim 2, wherein the method comprises the following steps: the temperature of the drying box in the step (4) is 105-110 ℃.
5. The method for detecting the iron content in calcite and dolomite according to claim 2, wherein the method comprises the following steps: and (4) cooling to room temperature in the step (4), wherein the specific temperature is 20-25 ℃.
6. The method for detecting the iron content in calcite and dolomite according to claim 2, wherein the method comprises the following steps: the ultraviolet-visible spectrophotometer used in the step (5) is a UV-1750 ultraviolet-visible spectrophotometer.
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Non-Patent Citations (3)
| Title |
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| 蔡祖成；韩金凤；张军: "电感耦合等离子体原子发射光谱法测定硅灰石中钙镁铝铁锰", 《冶金分析》 * |
| 闻向东等: "《石灰石及白云石化学分析第4部分：氧化铁含量的测定 邻二氮杂菲分光光度法和火焰原子吸收光谱法》", 31 May 2013, 中国标准出版社 * |
| 陈金凤等: "电感耦合等离子体原子发射光谱法同时测定石灰石和白云石中镁等6种元素含量", 《检验检疫学刊》 * |
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