CN117191769A - Method for detecting total iron content in red mud - Google Patents
Method for detecting total iron content in red mud Download PDFInfo
- Publication number
- CN117191769A CN117191769A CN202311182416.5A CN202311182416A CN117191769A CN 117191769 A CN117191769 A CN 117191769A CN 202311182416 A CN202311182416 A CN 202311182416A CN 117191769 A CN117191769 A CN 117191769A
- Authority
- CN
- China
- Prior art keywords
- red mud
- sample
- iron content
- total iron
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 224
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 50
- 239000000523 sample Substances 0.000 claims abstract description 64
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 40
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 36
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012086 standard solution Substances 0.000 claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 17
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims abstract description 15
- 238000012417 linear regression Methods 0.000 claims abstract description 15
- 238000007865 diluting Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 11
- 239000012498 ultrapure water Substances 0.000 claims abstract description 11
- 238000000295 emission spectrum Methods 0.000 claims abstract description 10
- 239000012488 sample solution Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000012085 test solution Substances 0.000 claims description 22
- 239000013068 control sample Substances 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000004364 calculation method Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 15
- 230000000052 comparative effect Effects 0.000 description 17
- 238000012360 testing method Methods 0.000 description 13
- 238000005259 measurement Methods 0.000 description 12
- 238000013112 stability test Methods 0.000 description 7
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 6
- 239000013074 reference sample Substances 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000009616 inductively coupled plasma Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 238000005238 degreasing Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- YXANNIUJXVGEJX-UHFFFAOYSA-K potassium hydroxy-(hydroxy(dioxo)chromio)oxy-dioxochromium chloride Chemical compound [Cl-].[K+].O[Cr](=O)(=O)O[Cr](O)(=O)=O YXANNIUJXVGEJX-UHFFFAOYSA-K 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229960002523 mercuric chloride Drugs 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 1
- DGXTZMPQSMIFEC-UHFFFAOYSA-M sodium;4-anilinobenzenesulfonate Chemical compound [Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=CC=C1 DGXTZMPQSMIFEC-UHFFFAOYSA-M 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to the technical field of iron content detection, and discloses a method for detecting total iron content in red mud. The detection method comprises the following steps: (1) Adding the red mud sample to be measured into mixed acid consisting of nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid, heating until the red mud sample is completely dissolved, cooling, and diluting with ultrapure water to obtain a sample solution to be measured; (2) Preparing an iron standard solution with a certain concentration gradient, and then measuring the iron standard solution by adopting an inductively coupled plasma atomic emission spectrometry to obtain a linear regression equation of the concentration of iron element and the intensity of emission spectrum; (3) And (3) measuring the sample solution to be measured in the step (1) by adopting an inductively coupled plasma atomic emission spectrometry, and calculating the total iron content in the red mud according to the linear regression equation in the step (2). The detection method can accurately and reliably detect the total iron content in the red mud sample, and is simple and quick to operate.
Description
Technical Field
The invention belongs to the technical field of iron content detection, and particularly relates to a method for detecting total iron content in red mud.
Background
Red mud is solid waste produced in the production process of alumina, and the discharge amountLarge. The content of iron element in the red mud is higher and can reach 20 to 60 percent (Fe is used) 2 O 3 Meter) can be used as valuable components for secondary utilization, and realizes the synergy and emission reduction of red mud waste. Therefore, a method for determining the iron content in the red mud sample is urgently needed. At present, no standard method for measuring the total iron content of red mud exists, and the method is generally carried out by referring to a method for detecting the total iron content of iron ore, such as a classical stannous chloride-potassium dichromate method and methods used in national standards of GB/T6730.5-2007 method for measuring the total iron content of iron ore, GB/T6730.65-2009 method for measuring the total iron content of iron ore, namely a method for reducing potassium dichromate by titanium trichloride titration. However, the stannous chloride-potassium dichromate method needs to use a mercuric chloride medicament, which may endanger the health of operators and make the treatment of the test waste liquid difficult; the traditional national standard method for measuring the total iron content of the iron ore is complex in analysis process, long in detection time, large in possible human error in the detection process and limited in test precision.
CN 112179899A proposes a method for detecting total iron content in iron ore, which comprises the steps of adopting sulfuric-phosphoric mixed acid and perchloric acid to decompose a sample at high temperature, then adding hydrochloric acid to dissolve salts, adding sodium tungstate solution, standing, dripping titanium trichloride solution to make the sample liquid light blue, and standing for 1-2 min; 120-150 ml of water is added, copper sulfate is added to ensure that blue color is just removed, sodium diphenylamine sulfonate solution is immediately added, potassium dichromate standard solution is used for titration until stable purple is taken as an end point, and then the total iron content is calculated according to a formula. The method optimizes the sample dissolution effect and reduces the chemical reagent class, but the method still uses potassium dichromate as a titration reagent, thereby having potential chromium pollution risk; and the detection precision of titration chemical analysis is low, and the method is still not suitable for detecting red mud samples.
CN 115308356A discloses a method for detecting total iron in alkaline degreasing fluid, which comprises the steps of adding active carbon to adsorb grease after a concentrated hydrochloric acid sample is dissolved, adding oxalic acid to prevent iron from being adsorbed, and then carrying out iron content detection in the alkaline degreasing fluid, wherein three methods of potentiometric titration, inductively coupled plasma atomic emission spectrometry and flame atomic absorption spectrophotometry are respectively used for detecting the total iron content in the alkaline degreasing fluid. However, the concentrated hydrochloric acid adopted in the patent cannot completely release iron element in the red mud sample, and cannot accurately detect the total iron content in the red mud sample.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the primary purpose of the invention is to provide a method for detecting the total iron content in red mud. The detection method can accurately and reliably detect the total iron content in the red mud sample, and is simple and quick to operate.
The invention aims at realizing the following technical scheme:
a method for detecting total iron content in red mud comprises the following steps:
(1) Adding the red mud sample to be measured into mixed acid consisting of nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid, heating until the red mud sample is completely dissolved, cooling, and diluting with ultrapure water to obtain a sample solution to be measured;
(2) Preparing an iron standard solution with a certain concentration gradient, and then measuring the iron standard solution by adopting an inductively coupled plasma atomic emission spectrometry (ICP-AES) to obtain a linear regression equation of the concentration of iron element and the intensity of an emission spectrum;
(3) And (3) measuring the sample solution to be measured in the step (1) by adopting an inductively coupled plasma atomic emission spectrometry, and calculating the total iron content in the red mud according to the linear regression equation in the step (2).
Further, in the step (1), the volume ratio of the nitric acid to the hydrochloric acid to the perchloric acid to the hydrofluoric acid is 4-8:4-8:2-5:2-5; more preferably, the volume ratio of nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid is 4-6:4-6:3-4:3-5.
Further preferably, the addition amount of the red mud sample to be detected in the step (1) is 0.1000 g+/-0.0100 g; the addition amount of nitric acid is 4-8 mL, the addition amount of hydrochloric acid is 4-8 mL, the addition amount of perchloric acid is 2-5 mL, and the addition amount of hydrofluoric acid is 2-5 mL.
Further, the heating temperature in the step (1) is 140-270 ℃.
Further, the dilution with ultrapure water in the step (1) means that the dilution with ultrapure water is 20000 to 200000 times.
Further, the preparation of the iron standard solution with a certain concentration gradient in the step (2) refers to the preparation of the iron standard solution with the concentration of iron element of 0.4ppm, 1ppm, 2ppm, 4ppm, 6ppm and 8ppm respectively.
Further preferably, the linear regression equation in the step (2) is y=170314.78dx+2908.85817, and the correlation coefficient r is 0.999958; where x is the elemental iron concentration (ppm) and y is the emission spectrum intensity.
Further, the inductively coupled plasma atomic emission spectrometry in the steps (2) and (3) is performed at a wavelength corresponding to any one of the 4 more sensitive lines 238.204nm, 239.562nm, 259.939nm and 234.349nm of iron.
Further, the inductively coupled plasma atomic emission spectrometry in steps (2) and (3) is performed in a wavelength range of 238.20 to 238.21 nm.
Further, the detection method further comprises the steps of heating and diluting the mixed acid with the same dosage under the condition that the red mud sample to be detected is not added, so as to prepare an empty white control sample, and detecting the concentration of the iron element in the empty white control sample; the calculation formula of the total iron content in the red mud is as follows:
wherein: w is the total iron content (mass fraction, unit:%) of the red mud sample to be measured, c represents the iron element concentration in the solution of the sample to be measured, and unit is mg/kg (ppm); c 0 The concentration of iron element in the blank control sample is expressed in mg/kg (ppm); a represents dilution multiple of the test solution, and has no dimension.
The principle of the invention is as follows: by adopting reasonable acid type and acid liquor proportion, various insoluble and insoluble minerals in the red mud sample can be fully digested, iron element in the red mud sample is completely released into the test solution, and then the iron element content is tested by adopting an inductively coupled plasma atomic emission spectrometry with high accuracy, stable result and simple operation.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the method, nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid are adopted to carry out high-temperature digestion on the red mud sample, and after the obtained test solution is diluted, an inductively coupled plasma emission spectrometer is adopted to measure the content of iron element in the test solution, so that the result is reliable, and the data is stable.
(2) The method provides a simpler and practical pretreatment mode aiming at the composition of red mud waste, avoids test deviation caused by insoluble release of iron element in indissolvable minerals, ensures that the iron element in a red mud sample completely enters into a test solution, ensures the accuracy of data, and simultaneously has good data reproducibility, and is suitable for measuring the total iron content in the red mud.
(3) The method of the invention effectively avoids the use of mercury-containing reagents and chromium-containing reagents in the whole detection process, and effectively reduces the environmental pollution risk.
Drawings
FIG. 1 is a graph of Fe standard plotted against standard solution iron element concentration (ppm) and emission spectrum intensity in an example of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
The experimental process adopts an inductively coupled plasma atomic emission spectrometer (Perkinelmer Avio 200), high-purity argon [ omega (Ar) > 99.999% ], and the following table 1 is the main working condition of the inductively coupled plasma atomic emission spectrometer.
Table 1 main operating conditions of the instrument
| Cooling water pump temperature | 19℃ |
| Radio frequency power | 1300W |
| Radio Frequency (RF) frequency | 40.68MHz |
| Atomizer flow | 0.7L/min |
| Observation angle | RADIAL |
| Viewing height of height | 15mm |
| Analyzing pump speed | 1.5mL/min |
The main reagents include: iron standard solution, 1000. Mu.g/mL; the iron standard solution series for test is obtained by diluting an iron standard solution, and the concentrations are respectively 0.4ppm, 1ppm, 2ppm, 4ppm, 6ppm and 8ppm; nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid are all analytically pure; the experimental water is ultrapure water, and meets the second-level water specified by GB/T668-2008.
Example 1
The method for detecting the total iron content in the red mud comprises the following steps:
(1) Sample solution preparation:
accurately weighing 0.1000 g+/-0.0100 g red mud sample, placing the red mud sample in a 50mL polytetrafluoroethylene beaker, adding 6mL nitric acid, 6mL hydrochloric acid, 3mL perchloric acid and 3mL hydrofluoric acid for a small amount of times, dissolving the sample at 240 ℃ until the sample is completely dissolved to form a test solution, diluting the test solution 60000 times by ultrapure water after cooling, and measuring.
(2) Preparing an iron standard solution series:
the standard solutions of iron with the concentration of 0.04mL, 0.1mL, 0.2mL, 0.4mL, 0.6mL and 0.8mL of 1000 mug/mL are respectively removed by a pipette, diluted to scale marks by ultrapure water, and iron standard solution series with the concentration of iron element of 0.4ppm, 1ppm, 2ppm, 4ppm, 6ppm and 8ppm are prepared.
(3) Determination of iron element content in the test solution:
measuring the iron standard solution series by an inductively coupled plasma atomic emission spectrometry, wherein the selected spectral line is 238.204nm, the linear relation between the iron standard solution series and the emission spectrum intensity is shown in figure 1 when the concentration of the iron in parts by weight is 0.4 ppm-8 ppm, the obtained linear regression equation is y=170314.7822+2908.85817, and the correlation coefficient r is 0.999958; where x is the elemental iron concentration (ppm) and y is the emission spectrum intensity. And measuring the emission spectrum intensity in the diluted test solution by an inductive coupling plasma atomic emission spectrometry, and obtaining the iron concentration of the red mud test solution according to a linear regression equation, wherein the iron concentration of the red mud test solution is 8.093mg/kg. And (3) heating and diluting the mixed acid with the same dosage under the same condition as the step (1) under the condition that the red mud sample to be measured is not added, so as to prepare the blank reference sample. The iron concentration in the blank control was determined to be 0.012mg/kg by the same method.
(4) Calculating the total iron content in the red mud:
according to the formula, the total iron content w (mass fraction,%) in the red mud sample is:
(5) Stability test:
then, 4 parts of the red mud sample (labeled as # 2, # 3, # 4 and # 5, respectively) were taken, and the total iron content in the 4 parts of the sample was repeatedly measured and calculated, and the measurement results are shown in table 2 below:
TABLE 2 example 1 assay stability test results
| 1# | 2# | 3# | 4# | 5# |
| 48.49％ | 48.41％ | 48.25％ | 48.18％ | 48.66％ |
The data in Table 2 shows that the method described in example 1 has a measurement result error of less than 0.5% after five times of stability detection, which indicates that the stability of the measurement method of the invention is better.
Example 2
The method for detecting the total iron content in the red mud comprises the following steps:
(1) Sample solution preparation:
accurately weighing 0.1000 g+/-0.0100 g red mud sample, placing the red mud sample in a 50mL polytetrafluoroethylene beaker, adding 4mL nitric acid, 4mL hydrochloric acid and 4mL perchloric acid for a small amount of times, dissolving the sample at 270 ℃ by 5mL hydrofluoric acid until the sample is completely dissolved to form a test solution, diluting the test solution by 46000 times by ultrapure water after cooling, and measuring.
(2) The iron standard solution series was prepared as in example 1.
(3) Determination of iron element content in the test solution:
the intensity of the emission spectrum in the diluted test solution is measured by an inductively coupled plasma atomic emission spectrometry, the selected spectral line is 238.204nm, and the iron concentration of the red mud test solution is 4.490mg/kg according to the linear regression equation obtained in the embodiment 1. And (3) heating and diluting the mixed acid with the same dosage under the same condition as the step (1) under the condition that the red mud sample to be measured is not added, so as to prepare the blank reference sample. The iron concentration in the blank control was measured to be 0.016mg/kg by the same method.
(4) Calculating the total iron content in the red mud:
according to the formula, the total iron content w (mass fraction,%) in the red mud sample is:
(5) Stability test:
then, 4 parts of the red mud sample (labeled as # 2, # 3, # 4 and # 5, respectively) were taken, and the total iron content in the 4 parts of the sample was repeatedly measured and calculated, and the measurement results are shown in table 3 below:
TABLE 3 test results for stability detection by example 2 assay
| 1# | 2# | 3# | 4# | 5# |
| 20.58％ | 21.01％ | 20.74％ | 20.93％ | 20.60％ |
The data in Table 3 shows that the method in example 2 has a measurement result error of less than 0.5% after five times of stability detection, which indicates that the stability of the measurement method of the invention is better.
Comparative example 1
In this comparative example, compared with example 1, the sample was dissolved, diluted and tested under the same conditions using a mixed acid of hydrochloric acid, perchloric acid and hydrofluoric acid in an equivalent (18 mL) volume ratio of 2:1:1 without adding nitric acid. According to the linear regression equation obtained in the example 1, the iron concentration of the red mud test solution is 7.425mg/kg. And (3) heating and diluting the mixed acid with the same dosage under the same condition as the step (1) under the condition that the red mud sample to be measured is not added, so as to prepare the blank reference sample. The iron concentration in the blank control sample was measured to be 0.011mg/kg by the same method.
According to the formula, the total iron content w (mass fraction,%) in the red mud sample is:
then, 4 parts of the red mud sample (labeled as # 2, # 3, # 4, and # 5, respectively) in example 1 were taken, and the total iron content in the 4 parts of the sample was repeatedly measured and calculated, and the measurement results are shown in table 4 below:
TABLE 4 test results for stability test of comparative example 1
| 1# | 2# | 3# | 4# | 5# |
| 44.48％ | 43.56％ | 45.31％ | 44.88％ | 43.76％ |
The data in Table 4 shows that the comparative example has a measurement result error of less than 2% and has general stability; the overall test results were low.
Comparative example 2
In this comparative example, compared with example 1, the sample was dissolved, diluted and tested under the same conditions using a mixed acid of nitric acid, perchloric acid and hydrofluoric acid in the same volume ratio of 2:1:1 (18 mL) without adding hydrochloric acid. According to the linear regression equation obtained in the example 1, the iron concentration of the red mud test solution is 7.241mg/kg. And (3) heating and diluting the mixed acid with the same dosage under the same condition as the step (1) under the condition that the red mud sample to be measured is not added, so as to prepare the blank reference sample. The iron concentration in the blank control was determined to be 0.018mg/kg by the same method.
According to the formula, the total iron content w (mass fraction,%) in the red mud sample is:
then, 4 parts of the red mud sample (labeled as # 2, # 3, # 4, and # 5, respectively) in example 1 were taken, and the total iron content in the 4 parts of the sample was repeatedly measured and calculated, and the measurement results are shown in table 5 below:
TABLE 5 test results for stability test of comparative example 2
| 1# | 2# | 3# | 4# | 5# |
| 43.34％ | 42.66％ | 43.01％ | 41.88％ | 41.42％ |
The data in Table 5 shows that the comparative example has a measurement result error of less than 2% and has general stability; the overall test results were low.
Comparative example 3
In this comparative example, compared with example 1, the sample was dissolved, diluted and tested under the same conditions using a mixed acid of nitric acid, hydrochloric acid and hydrofluoric acid in an equivalent (18 mL) volume ratio of 2:2:1 without adding perchloric acid. According to the linear regression equation obtained in the example 1, the iron concentration of the red mud test solution is 6.542mg/kg. And (3) heating and diluting the mixed acid with the same dosage under the same condition as the step (1) under the condition that the red mud sample to be measured is not added, so as to prepare the blank reference sample. The iron concentration in the blank control was determined to be 0.007mg/kg by the same method.
According to the formula, the total iron content w (mass fraction,%) in the red mud sample is:
then, 4 parts of the red mud sample (labeled as # 2, # 3, # 4, and # 5, respectively) in example 1 were taken, and the total iron content in the 4 parts of the sample was repeatedly measured and calculated, and the measurement results are shown in table 6 below:
TABLE 6 test results for stability test of comparative example 3
| 1# | 2# | 3# | 4# | 5# |
| 39.21％ | 37.24％ | 32.10％ | 33.25％ | 38.67％ |
The data in Table 6 show that the comparative example has a measurement error of greater than 6% and poor stability; the overall test results were severely lower.
Comparative example 4
In this comparative example, compared with example 1, the sample was dissolved, diluted and tested under the same conditions using a mixed acid of nitric acid, hydrochloric acid and perchloric acid in an equivalent (18 mL) volume ratio of 2:2:1 without adding hydrofluoric acid. According to the linear regression equation obtained in the example 1, the iron concentration of the red mud test solution is 5.622mg/kg. And (3) heating and diluting the mixed acid with the same dosage under the same condition as the step (1) under the condition that the red mud sample to be measured is not added, so as to prepare the blank reference sample. The iron concentration in the blank control was measured to be 0.014mg/kg by the same method.
According to the formula, the total iron content w (mass fraction,%) in the red mud sample is:
then, 4 parts of the red mud sample (labeled as # 2, # 3, # 4, and # 5, respectively) in example 1 were taken, and the total iron content in the 4 parts of the sample was repeatedly measured and calculated, and the measurement results are shown in table 7 below:
TABLE 7 test results for stability test of comparative example 4
| 1# | 2# | 3# | 4# | 5# |
| 33.65％ | 29.41％ | 38.17％ | 36.21％ | 30.35％ |
The data in Table 7 show that the comparative example has a measurement error of greater than 8% and poor stability; the overall test results were severely lower.
As can be seen from the results of the above examples and comparative examples, the method provided by the invention adopts mixed acid of nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid to carry out high-temperature digestion on the red mud sample, and combines an inductively coupled plasma emission spectrometer to measure the content of iron element in the test solution, so that the detection result is accurate and reliable, and the stability is good.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The method for detecting the total iron content in the red mud is characterized by comprising the following steps of:
(1) Adding the red mud sample to be measured into mixed acid consisting of nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid, heating until the red mud sample is completely dissolved, cooling, and diluting with ultrapure water to obtain a sample solution to be measured;
(2) Preparing an iron standard solution with a certain concentration gradient, and then measuring the iron standard solution by adopting an inductively coupled plasma atomic emission spectrometry to obtain a linear regression equation of the concentration of iron element and the intensity of emission spectrum;
(3) And (3) measuring the sample solution to be measured in the step (1) by adopting an inductively coupled plasma atomic emission spectrometry, and calculating the total iron content in the red mud according to the linear regression equation in the step (2).
2. The method for detecting the total iron content in the red mud according to claim 1, wherein the volume ratio of the nitric acid, the hydrochloric acid, the perchloric acid and the hydrofluoric acid in the step (1) is 4-8:4-8:2-5:2-5.
3. The method for detecting the total iron content in the red mud according to claim 2, wherein the addition amount of the red mud sample to be detected in the step (1) is 0.1000 g+/-0.0100 g; the addition amount of nitric acid is 4-8 mL, the addition amount of hydrochloric acid is 4-8 mL, the addition amount of perchloric acid is 2-5 mL, and the addition amount of hydrofluoric acid is 2-5 mL.
4. The method for detecting the total iron content in the red mud according to claim 1, wherein the heating temperature in the step (1) is 140-270 ℃.
5. The method for detecting the total iron content in the red mud according to claim 1, wherein the dilution with ultrapure water in the step (1) means that the dilution with ultrapure water is 20000 to 200000 times.
6. The method for detecting the total iron content in the red mud according to claim 1, wherein the preparation of the iron standard solution with a certain concentration gradient in the step (2) is to prepare iron standard solutions with the concentration of iron element of 0.4ppm, 1ppm, 2ppm, 4ppm, 6ppm and 8ppm respectively.
7. The method for detecting the total iron content in the red mud according to claim 6, wherein the linear regression equation in the step (2) is y=170314.7822+2908.85817, and the correlation coefficient r is 0.999958; wherein x is the concentration of iron element, the unit is ppm, and y is the intensity of the emission spectrum.
8. The method for detecting the total iron content in the red mud according to claim 1, wherein the inductively coupled plasma atomic emission spectrometry in the steps (2) and (3) is performed at a wavelength corresponding to any one of 4 more sensitive lines 238.204nm, 239.562nm, 259.939nm and 234.349nm of iron.
9. The method for detecting the total iron content in the red mud according to claim 1, wherein the inductively coupled plasma atomic emission spectrometry in the steps (2) and (3) is performed within a wavelength range of 238.20-238.21 nm.
10. The method for detecting the total iron content in the red mud according to claim 1, wherein the method further comprises the steps of heating and diluting the same amount of mixed acid under the same condition as that of the step (1) without adding a red mud sample to be detected, so as to prepare an empty white control sample, and detecting the concentration of iron element in the empty white control sample; the calculation formula of the total iron content in the red mud is as follows:
wherein: w is the total iron content in the red mud sample to be measured, c represents the iron element concentration in the solution of the sample to be measured, and the unit is mg/kg; c 0 The concentration of iron element in the blank control sample is expressed in mg/kg; a represents dilution multiple of the test solution, and has no dimension.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311182416.5A CN117191769A (en) | 2023-09-14 | 2023-09-14 | Method for detecting total iron content in red mud |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311182416.5A CN117191769A (en) | 2023-09-14 | 2023-09-14 | Method for detecting total iron content in red mud |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117191769A true CN117191769A (en) | 2023-12-08 |
Family
ID=88986596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311182416.5A Pending CN117191769A (en) | 2023-09-14 | 2023-09-14 | Method for detecting total iron content in red mud |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117191769A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10330856A (en) * | 1997-05-28 | 1998-12-15 | Nisshin Steel Co Ltd | Detection of iron content in water granulated slag |
| CN102998274A (en) * | 2012-11-30 | 2013-03-27 | 华南理工大学 | Method for rapidly measuring total sulfur content in black pulping liquor |
| CN103439324A (en) * | 2013-08-13 | 2013-12-11 | 武汉钢铁(集团)公司 | Method for rapidly measuring iron content in continuous casting mold fluxes |
| CN111257247A (en) * | 2019-11-22 | 2020-06-09 | 浙江省海洋水产研究所 | Method for measuring iron content in marine sediments |
-
2023
- 2023-09-14 CN CN202311182416.5A patent/CN117191769A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10330856A (en) * | 1997-05-28 | 1998-12-15 | Nisshin Steel Co Ltd | Detection of iron content in water granulated slag |
| CN102998274A (en) * | 2012-11-30 | 2013-03-27 | 华南理工大学 | Method for rapidly measuring total sulfur content in black pulping liquor |
| CN103439324A (en) * | 2013-08-13 | 2013-12-11 | 武汉钢铁(集团)公司 | Method for rapidly measuring iron content in continuous casting mold fluxes |
| CN111257247A (en) * | 2019-11-22 | 2020-06-09 | 浙江省海洋水产研究所 | Method for measuring iron content in marine sediments |
Non-Patent Citations (5)
| Title |
|---|
| 姜云军等: "四酸敞口溶解-电感耦合等离子体发射光谱法测定土壤中的硫", 岩矿测试, vol. 37, no. 2, 31 March 2018 (2018-03-31), pages 152 - 158 * |
| 张旺强;王春妍;李瑞仙;巨力佩;陈月源;余志峰;毛振才;: "电感耦合等离子体发射光谱法测定富镁铁橄榄岩类矿石中铜镍铁和氧化镁", 岩矿测试, no. 02, 15 April 2011 (2011-04-15), pages 195 - 199 * |
| 陈祝海等: "电感耦合等离子体原子发射光谱法测定金矿石中铅锌砷铋镉汞", 分析测试, vol. 41, no. 4, 31 December 2020 (2020-12-31), pages 79 - 82 * |
| 饶正勇: "赤泥中金属元素分析和CTAB/ATAB改性赤泥吸附Cr(VI)的研究", 中国优秀硕士学位论文全文数据库工程科技I辑, 15 October 2012 (2012-10-15), pages 027 - 1130 * |
| 鲁海妍等: "湿法消解-电感耦合等离子体质谱法测定多金属矿中碲", 桂林理工大学学报, vol. 43, no. 2, 30 June 2023 (2023-06-30), pages 211 - 217 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101694470A (en) | Method for detecting content of calcium element in calcium powder | |
| CN110987918A (en) | Detection reagent and rapid detection method for total nitrogen in water | |
| CN111289499B (en) | Method for simultaneously detecting multiple trace elements in iron-containing waste acid | |
| CN107402204A (en) | A kind of lead ion detection method | |
| CN112213279A (en) | Method for measuring iron ions in denitration absorption liquid | |
| CN109738419B (en) | Method for measuring boron content in aluminum-based boron carbide material | |
| CN111443079A (en) | Method for simultaneously detecting contents of trace As, Pb, Cd, Zn, Cr, Co and V elements in ferric trichloride | |
| CN112268883B (en) | Method for determining mercury and arsenic in coal by microwave digestion atomic fluorescence spectrometry | |
| CN105954250A (en) | Novel method for measuring arsenic in urine | |
| CN105334208B (en) | A kind of iron, copper metal ion interfere the measuring method of ammonia nitrogen in lower micro solution | |
| CN117191769A (en) | Method for detecting total iron content in red mud | |
| CN111443078A (en) | Method for simultaneously detecting contents of trace As, Pb, Cd, Zn and Cr elements in ferrous chloride | |
| CN116242817A (en) | Method for detecting lanthanum in aluminum-silicon-strontium series alloy | |
| CN105021591B (en) | A kind of method of silicomanganese phosphorus molybdenum copper titanium magnesium lanthanum cerium yttrium content in measurement cast iron | |
| CN100535637C (en) | Continuous detecting method for lead-cadmium in plastic sample | |
| CN104655610B (en) | The analysis method and assay method of vanadyl oxalate oxalate ion concentration | |
| CN115078055A (en) | Serum sample diluent, serum medium trace element detection kit and application | |
| CN113777095A (en) | Method for detecting content of potassium and sodium in molybdenum trioxide for high-solubility catalyst | |
| CN108776125A (en) | A kind of sample pre-treatments reagent and method measured in urine during arsenic | |
| CN113804673A (en) | Method for measuring boron content in glass | |
| CN109085164B (en) | Method for accurately measuring vanadium content in vanadium-chromium hydrogen storage alloy | |
| CN113484260A (en) | Method for measuring fluoride in water by spectrophotometry | |
| CN118032742A (en) | Method for detecting chloride content in industrial potassium nitrate by ICP-OES | |
| CN115015509B (en) | Method for determining chemical oxygen demand of wastewater containing chlorine and bromine simultaneously | |
| CN113433291B (en) | Digestion method and determination method of total nitrogen, phosphorus and potassium in soil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |