CN111721726A - Method for determining content of ferric oxide in ore by using spectrophotometer - Google Patents
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 37
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000843 powder Substances 0.000 claims abstract description 44
- 229910052742 iron Inorganic materials 0.000 claims abstract description 21
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 239000000523 sample Substances 0.000 claims description 38
- 239000011550 stock solution Substances 0.000 claims description 17
- 238000002835 absorbance Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000010459 dolomite Substances 0.000 claims description 13
- 229910000514 dolomite Inorganic materials 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- 239000012086 standard solution Substances 0.000 claims description 13
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 10
- 235000019738 Limestone Nutrition 0.000 claims description 9
- 239000006028 limestone Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000004575 stone Substances 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000012496 blank sample Substances 0.000 claims description 4
- 230000003203 everyday effect Effects 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 2
- 239000012488 sample solution Substances 0.000 claims description 2
- 238000011088 calibration curve Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 13
- 230000007246 mechanism Effects 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 5
- 239000012085 test solution Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 229960005070 ascorbic acid Drugs 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 3
- 239000011668 ascorbic acid Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 description 1
- 201000004569 Blindness Diseases 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000007793 ph indicator Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—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
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Abstract
The invention provides a method for determining the content of ferric oxide in ore by using a spectrophotometer, which comprises the steps of preparing standard powder, respectively detecting the iron content of the standard powder by using an atomic absorption method and a spectrophotometer method to obtain a corrected value, adding the corrected value to a sample determination result, adding a correction mechanism, correcting in real time and improving the detection accuracy.
Description
Technical Field
The invention relates to the technical field of chemical component analysis, in particular to a method for determining the content of ferric oxide in ore by using a spectrophotometer.
Background
In the production process of general ores, certain requirements are made on whiteness. The iron impurities not only can reduce the natural whiteness of the ore, but also can influence the calcination whiteness of the ore, thereby reducing the industrial value of the ore. Particularly, limestone and dolomite, which are high-quality raw materials of photovoltaic glass, have strict requirements on the iron content. Therefore, in actual production, the iron content needs to be detected in real time.
At present, the iron content in the ore can be measured by an X-ray fluorescence method (XRF), an inductively coupled plasma emission spectrometry (ICP-OES), an inductively coupled plasma mass spectrometry (ICP-MS), an EDTA complex titration method, a sulfosalicylic acid colorimetric method, a o-diazaphenanthrene method and the like. In industrial production, the content of the iron oxide is detected by a phenanthroline spectrophotometer method according to the national standard GB/T3286.4-2012.
However, when the content of iron oxide is detected by a spectrophotometer method, errors often occur due to instruments, solvents and the like, and the detection result is inaccurate. The existing detection method has no correction mechanism, so that whether the detection result is accurate or not can not be judged in time, and the normal operation of downstream industries is directly influenced.
Disclosure of Invention
The invention aims to solve the problems, provides a method for measuring the content of iron oxide in ore by using a spectrophotometer, adds a correction mechanism, corrects in real time and improves the detection accuracy.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for determining the content of iron oxide in ore by using a spectrophotometer comprises the following steps:
s1, sample preparation: the sample was dissolved to obtain a stock solution.
S2, preparing an iron standard solution.
S3, standard curve drawing: drawing "Fe2O3Standard curve of quantity-absorbance.
S4, preparing standard powder:
s41, selecting ores with iron content of 0.04-0.1 per mill, grinding, and sieving with a 100-mesh sieve to obtain stone powder;
and S42, adding distilled water into the prepared stone powder, fully stirring and homogenizing, drying, and grinding to obtain standard powder.
S5, calculating the content of ferric oxide in the sample:
s51, dividing the stock solution, detecting the absorbance of the sample solution by using a spectrophotometer, and finding out Fe in the sample from the standard curve2O3Amount of Fe in the sample, and calculating2O3Mass fraction of (c).
S52, detecting Fe in standard powder by using atomic absorption method2O3And then dissolving the standard powder to obtain a standard powder measured value by detecting according to the method of the step S51, wherein the difference value between the standard value and the standard powder measured value is a corrected value.
S53, the content of iron oxide in the sample is equal to that of Fe in the sample2O3Mass fraction of + correction value.
Preferably, in step S1, the sample is dissolved with dilute hydrochloric acid.
Preferably, the ore is limestone or dolomite.
Preferably, in step S2, Fe is first mixed2O3Burning and cooling to room temperature, adding hydrochloric acid and water, heating for dissolving, and diluting to obtain a series of iron standard solutions with different concentrations.
Preferably, in step S3, the iron standard solution is removed, the same amount of mixed color developing solution is added, a blank sample is set, and the absorbances of the iron standard solution and the blank sample are detected by a spectrophotometer, so as to draw "Fe2O3Standard curve of quantity-absorbance ".
Preferably, in the step S4, the drying temperature is 105 to 110 ℃.
Preferably, in step S5, Fe2O3The mass fraction calculating method comprises the following steps:
wherein, W (Fe)2O3)—Fe2O3Mass fraction of (a);
v-volume of stock solution in milliliters (ml);
v1-dividing the volume of the stock solution in milliliters (ml);
m1fe from a standard curve2O3Amount in micrograms (μ g);
m represents the weight of the sample and is expressed in (g).
Preferably, in step S5, step S52 is repeated every day to obtain a correction value, which is within ± 10ppm to be qualified, and if the correction value is not qualified after 2 consecutive times, the standard curve needs to be redrawn.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. the method for measuring the content of the ferric oxide in the ore by using the spectrophotometer disclosed by the invention is characterized in that a correction mechanism is added, and real-time correction is carried out, so that the detection accuracy is improved.
2. The method for determining the content of iron oxide in the ore by using a spectrophotometer comprises the steps of selecting the ore with the iron content of 0.04-0.1 per mill, grinding, and sieving by using a 100-mesh sieve to obtain stone powder; and adding distilled water into the prepared stone powder, fully stirring and homogenizing, then drying and grinding to obtain standard powder. Because the big problem of the homogenization degree of difficulty, hardly purchase, this application is through adding the distilled water stirring, dries again, reaches the purpose of homogenization, can regard as standard powder to use. The standard powder is sent to a third-party organization for detection, and is compared with detection data of a spectrophotometer method to obtain a correction value, so that the effect of self-checking and self-correcting can be achieved, the authority is improved, and the reliability of product detection is improved.
3. The method for determining the content of the iron oxide in the ore by using the spectrophotometer detects and calculates the correction value every day, the correction value is required to be qualified within +/-10 ppm, if the correction value is not qualified after being continuously made for 2 times, the iron standard curve is required to be drawn again, or other reasons are required to be searched, so that the detection result is within the error range, and the working blindness is reduced.
Drawings
FIG. 1 shows Fe in an example of the present invention2O3Content-absorbance standard curve.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1 the starting material was dolomite and the batch was 200627-07.
A method for measuring the content of ferric oxide in dolomite by using a spectrophotometer comprises the following steps:
s1, sample preparation: a dolomite sample of about 3.0194g was weighed into a 100ml beaker and added to a 1: 1, heating until a sample is fully dissolved, clearing the test solution, transferring the test solution into a 100ml volumetric flask, diluting with water to a scale, and uniformly mixing to obtain a stock solution;
s2, preparing an iron standard solution: 0.5000g of high-purity ferric trioxide is weighed out and placed in a 300ml beaker, and 20ml of a 1: 1, covering the watch glass with hydrochloric acid, heating at low temperature to dissolve, and cooling to room temperature. Transferring the solution into a 500ml volumetric flask, adding water to dilute the solution to a scale to obtain a ferric trioxide standard solution, wherein 1.00ml of the solution contains 1.00mg of ferric oxide;
s3, standard curve drawing: the ferric oxide standard solution was diluted to 1.00ml containing 10. mu.g, 20. mu.g, 30. mu.g, 40. mu.g, 50. mu.g, 60. mu.g, 70. mu.g, 80. mu.g, 90. mu.g and 100. mu.g of ferric oxide, and the ferric oxide standard solution was put into a 100ml color developing volumetric flask, and 5ml of ascorbic acid solution was added thereto, followed by mixing, and adjusting the pH to about 5 with aqueous ammonia (test using a pH indicator). Then adding 5ml of phenanthroline solution (2 g of phenanthroline is dissolved in 100ml of absolute ethyl alcohol, adding water to dilute to 500ml, mixing uniformly, storing in a brown bottle), diluting with water to the scale, and mixing uniformly. A part of the color developing solution was transferred to a 5cm cuvette, and the absorption light was measured at a wavelength of 510nm in a spectrophotometer with reference to a blank test solution. Absorbances were measured as 0.062, 0.128, 0.193, 0.257, 0.319, 0.380, 0.441, 0.504, 0.562, and 0.625, respectively, as Fe2O3The amount is plotted as abscissa and absorbance as ordinate2O3The standard curve of quantity-absorbance is shown in Table 1.
S4, preparing standard powder:
s41, selecting 10-120 meshes of dolomite with iron content of 0.04-0.1 per mill, grinding the dolomite with an agate mortar, and sieving the dolomite with a 100-mesh sieve to obtain dolomite powder;
s42, adding distilled water into the prepared dolomite powder, fully stirring and homogenizing, then drying at 105 ℃, and grinding to obtain standard powder;
s5, calculating the content of ferric oxide in the sample:
s51, dividing 25ml of stock solution, adding the stock solution into a 100ml color developing volumetric flask, adding 5ml of ascorbic acid solution, uniformly mixing, and adjusting the pH value to about 5 by using ammonia water (testing by using a pH test paper). Then 5ml of phenanthroline solution is added, diluted to the scale with water, mixed evenly, and the absorbance is measured at the wavelength of 510nm of a spectrophotometer to be 0.311. Finding out corresponding Fe from standard curve2O3The amount was 49. mu.g, and Fe in the sample was calculated2O3The mass fraction of (A) is 65ppm (65 ‰).
The calculation formula is as follows:
wherein, W (Fe)2O3)—Fe2O3Mass fraction of (a);
v-volume of stock solution in milliliters (ml);
v1-dividing the volume of the stock solution in milliliters (ml);
m1fe from a standard curve2O3Amount in micrograms (μ g);
m represents the weight of the sample and is expressed in (g).
S52, sending the standard powder to a third-party detection mechanism, and detecting Fe in the standard powder by using an atomic absorption method2O3The standard value is 65ppm (65 ‰), then the standard powder is detected according to the method of step S51 to obtain 68ppm standard powder measured value, and the difference between the standard value and the standard powder measured value is a corrected value of-3;
s53, the content of ferric oxide in the sample is as follows: fe in the sample2O3The mass fraction of (b) plus a correction value of 65ppm to 3ppm to 62 ppm.
Example 2 the raw material was dolomite and the batch was 200628-03.
The detection method used was the same as in example 1.
Re-detecting the correction value every day, detecting the standard powder according to the method of the step S51 to obtain a standard powder measured value of 66ppm, wherein the standard value is 65ppm, and the difference value between the standard value and the standard powder measured value is a correction value of-1;
a dolomite sample of about 3.0087g was weighed out and the absorbance measured at a spectrophotometer wavelength of 510nm was 0.305. Finding out corresponding Fe from standard curve2O3The amount was 47. mu.g, and Fe in the sample was calculated2O362ppm by mass.
The content of iron oxide in the sample is: fe in the sample2O3The mass fraction of (b) plus a correction value of 62ppm to 1ppm to 61 ppm.
Example 3 limestone was selected as the raw material and 200625-06 batches were selected.
A method for determining the content of iron oxide in limestone by using a spectrophotometer comprises the following steps:
s1, sample preparation: a limestone sample of about 3.0215g was weighed into a 100ml beaker and added to a 1: 1, heating until a sample is fully dissolved, clearing the test solution, transferring the test solution into a 100ml volumetric flask, diluting with water to a scale, and uniformly mixing to obtain a stock solution;
s2, preparing an iron standard solution: the same as example 1;
s3, standard curve drawing: the same as in example 1.
S4, preparing standard powder:
s41, selecting limestone with 10-120 meshes and iron content of 0.04-0.1 per mill, grinding, and sieving with a 100-mesh sieve to obtain limestone powder;
s42, adding distilled water into the prepared limestone powder, fully stirring and homogenizing, drying at 110 ℃, and grinding to obtain standard powder;
s5, calculating the content of ferric oxide in the sample:
s51, adding 25ml of stock solution into a 100ml color developing volumetric flask, adding 5ml of ascorbic acid solution, uniformly mixing, and adjusting the pH value to about 5 by using ammonia water (testing by using a pH test paper). Then 5ml of phenanthroline solution is added, diluted to the scale with water, mixed evenly, and the absorbance is measured at the wavelength of 510nm of a spectrophotometer to be 0.335. Finding out corresponding Fe from standard curve2O3The amount was 53. mu.g, and Fe in the sample was calculated2O370ppm by mass.
The calculation formula is as follows:
wherein, W (Fe)2O3)—Fe2O3Mass fraction of (a);
v-volume of stock solution in milliliters (ml);
v1-dividing the volume of the stock solution in milliliters (ml);
m1fe from a standard curve2O3Amount in micrograms (μ g);
m represents the weight of the sample and is expressed in (g).
S52, sending the standard powder to a third-party detection mechanism, and detecting Fe in the standard powder by using an atomic absorption method2O3The standard value is 70ppm, then the standard powder is detected according to the method of the step S51 to obtain 68ppm of the measured value of the standard powder, and the difference value between the standard value and the measured value of the standard powder is a corrected value 2;
s53, the content of ferric oxide in the sample is as follows: fe in the sample2O3The corrected value added to the mass fraction of (c) is 70ppm +2ppm to 72 ppm.
The above description is directed to the details of the preferred and possible embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention. All changes and modifications that come within the spirit of the invention are desired to be protected.
Claims (8)
1. A method for determining the content of iron oxide in ore by using a spectrophotometer is characterized by comprising the following steps:
s1, sample preparation: dissolving a sample to obtain a stock solution;
s2, preparing an iron standard solution;
s3, standard curve drawing: drawing "Fe2O3A standard curve of quantity-absorbance;
s4, preparing standard powder:
s41, selecting ores with iron content of 0.04-0.1 per mill, grinding, and sieving with a 100-mesh sieve to obtain stone powder;
s42, adding distilled water into the prepared stone powder, fully stirring and homogenizing, then drying, and grinding to obtain standard powder;
s5, calculating the content of ferric oxide in the sample:
s51, dividing the stock solution, detecting the absorbance of the sample solution by using a spectrophotometer, and finding out Fe in the sample from the standard curve2O3Amount of Fe in the sample, and calculating2O3Mass fraction of (a);
s52, detecting Fe in standard powder by using atomic absorption method2O3The standard powder is dissolved and detected according to the method of the step S51 to obtain a measured value of the standard powder, and the difference value between the standard value and the measured value of the standard powder is a corrected value;
s53, calculating the content of iron oxide in the sample to be Fe in the sample2O3Mass fraction of + correction value.
2. The method of claim 1, wherein the sample is dissolved in dilute hydrochloric acid in step S1.
3. The method for determining the iron oxide content of an ore using a spectrophotometer as claimed in claim 1, wherein the ore is limestone or dolomite.
4. The method of claim 1, wherein in step S2, Fe is first mixed with the ore2O3Burning and cooling to room temperature, adding hydrochloric acid and water, heating for dissolving, and diluting to obtain a series of iron standard solutions with different concentrations.
5. The method of claim 1, wherein in step S3, the mixed color solution is added into the iron standard solution in equal amount, a blank sample is set, and the absorbance of each iron standard solution and blank sample is detected by the spectrophotometer to draw "Fe2O3Standard curve of quantity-absorbance ".
6. The method for measuring the content of iron oxide in ore by using spectrophotometer according to claim 1, wherein the drying temperature is 105-110 ℃ in step S4.
7. The method for measuring the content of iron oxide in ore using spectrophotometer of claim 1, wherein in step S5, Fe2O3The mass fraction calculating method comprises the following steps:
wherein, W (Fe)2O3)—Fe2O3Mass fraction of (a); v-volume of stock solution in milliliters (ml); v. of1-dividing the volume of the stock solution in milliliters (ml); m is1Fe from a standard curve2O3Amount in micrograms (μ g); m represents the weight of the sample and is expressed in (g).
8. The method of claim 1, wherein the step S52 is repeated every day to obtain a correction value that is within + -10 ppm and is acceptable, and the calibration curve is re-drawn if it is not acceptable after 2 consecutive runs in step S5.
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