CN115684136A - Method for measuring content of calcium oxide in samarium oxide - Google Patents
Method for measuring content of calcium oxide in samarium oxide Download PDFInfo
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- CN115684136A CN115684136A CN202211332497.8A CN202211332497A CN115684136A CN 115684136 A CN115684136 A CN 115684136A CN 202211332497 A CN202211332497 A CN 202211332497A CN 115684136 A CN115684136 A CN 115684136A
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- 229940075630 samarium oxide Drugs 0.000 title claims abstract description 124
- 229910001954 samarium oxide Inorganic materials 0.000 title claims abstract description 124
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 238000000034 method Methods 0.000 title claims abstract description 70
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000000292 calcium oxide Substances 0.000 title claims abstract description 55
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 title claims abstract description 55
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 67
- 239000000523 sample Substances 0.000 claims abstract description 45
- 239000012488 sample solution Substances 0.000 claims abstract description 36
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 33
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 33
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 30
- 239000012086 standard solution Substances 0.000 claims abstract description 23
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 34
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000005119 centrifugation Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 4
- 239000012085 test solution Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 description 18
- 239000011575 calcium Substances 0.000 description 17
- 239000011159 matrix material Substances 0.000 description 14
- 238000005259 measurement Methods 0.000 description 13
- 229910052791 calcium Inorganic materials 0.000 description 12
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 11
- BCYBEIXXOVNETJ-UHFFFAOYSA-K samarium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Sm+3] BCYBEIXXOVNETJ-UHFFFAOYSA-K 0.000 description 10
- 238000001914 filtration Methods 0.000 description 8
- 229910052772 Samarium Inorganic materials 0.000 description 7
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 7
- 238000010790 dilution Methods 0.000 description 5
- 239000012895 dilution Substances 0.000 description 5
- 239000012490 blank solution Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000009616 inductively coupled plasma Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 240000004922 Vigna radiata Species 0.000 description 3
- 235000010721 Vigna radiata var radiata Nutrition 0.000 description 3
- 235000011469 Vigna radiata var sublobata Nutrition 0.000 description 3
- -1 ammonium ions Chemical class 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 3
- 239000000920 calcium hydroxide Substances 0.000 description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000013582 standard series solution Substances 0.000 description 1
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Abstract
The invention relates to a method for measuring the content of calcium oxide in samarium oxide, which comprises the following steps: providing a samarium oxide sample, and dissolving the samarium oxide sample by using acid liquor to obtain a samarium oxide sample solution; adjusting the pH value of a samarium oxide sample solution to 9-11 by adopting ammonia water, carrying out solid-liquid separation, taking supernate, and determining by adopting ICP-OES (inductively coupled plasma-optical emission spectrometry); providing a plurality of calcium ion standard solutions with different calcium ion concentrations, and respectively measuring the emission intensity of calcium ions in the plurality of calcium ion standard solutions by adopting ICP-OES (inductively coupled plasma-optical emission spectrometry) to obtain a standard curve equation of the emission intensity and the calcium ion concentration; and calculating to obtain the content of calcium oxide in the samarium oxide sample according to a standard curve equation. The method for measuring the content of calcium oxide in the samarium oxide adopts an ICP-OES method to obtain a standard curve equation of emission intensity and calcium ion concentration, adopts the ICP-OES method to measure the emission intensity of the samarium oxide sample, and calculates the content of calcium oxide in the samarium oxide sample according to the standard curve equation.
Description
Technical Field
The invention relates to the technical field of chemical determination, in particular to a method for determining the content of calcium oxide in samarium oxide.
Background
The calcium oxide content in the samarium oxide influences the product quality, the calcium oxide content in the samarium oxide also influences the trade price of the samarium oxide, and the samarium oxide can be selected according to actual requirements in the market. At present, the national standard GB/T12690.15-2018 provides three methods for measuring calcium in samarium oxide: in the first method and the second method, a matrix matching method and a standard addition method are respectively adopted to eliminate matrix interference of a samarium matrix on calcium determination, and in the third method, an inductively coupled plasma mass spectrometer (ICP-MS/MS) with a collision cell is adopted. However, the matrix matching method requires high-purity samarium oxide, which is costly; the standard addition method is cumbersome to operate and is not suitable for batch measurement; inductively coupled plasma mass spectrometers are very expensive and have strict requirements on calcium contamination control during the measurement process, as well as extremely high requirements on reagents.
Therefore, the method for measuring the content of calcium oxide in the samarium oxide, which has the advantages of low cost, simple operation and high accuracy, is of great significance.
Disclosure of Invention
Based on the method, the method for determining the content of the calcium oxide in the samarium oxide is low in cost, simple to operate and high in accuracy.
The technical scheme of the invention for solving the technical problems is as follows.
A method for measuring the content of calcium oxide in samarium oxide comprises the following steps:
providing a samarium oxide sample, and dissolving the samarium oxide sample by using an acid solution to obtain a samarium oxide sample solution;
adjusting the pH value of the samarium oxide sample solution to 9-11 by adopting ammonia water, carrying out solid-liquid separation, taking supernatant, and measuring the emission intensity of calcium ions in the supernatant by adopting ICP-OES (inductively coupled plasma-optical emission spectrometry);
providing a plurality of calcium ion standard solutions with different calcium ion concentrations, and respectively measuring the emission intensity of calcium ions in the plurality of calcium ion standard solutions by adopting ICP-OES (inductively coupled plasma-optical emission spectrometry) to obtain a standard curve equation of the emission intensity and the calcium ion concentration;
and calculating to obtain the content of calcium oxide in the samarium oxide sample according to the standard curve equation.
In some of the examples, the solid-liquid separation is performed by centrifugation in the method for measuring the calcium oxide content in samarium oxide.
In some of the embodiments, in the method for determining the calcium oxide content in samarium oxide, the acid solution is at least one selected from nitric acid, hydrochloric acid, and perchloric acid.
In some embodiments, in the method for determining the content of calcium oxide in samarium oxide, the acid solution is nitric acid.
In some embodiments, in the method for determining the content of calcium oxide in samarium oxide, the acid liquor is 30 to 60 percent by mass.
In some embodiments, in the method for determining the content of calcium oxide in samarium oxide, the mass fraction of the ammonia water is 10% to 50%.
In some embodiments, in the method for determining the calcium oxide content in samarium oxide, the standard curve equation of the emission intensity and the calcium ion concentration is as follows:
Y＝k·X+b
wherein Y is the emission intensity; x is the concentration of calcium ions in the test solution, and the unit is mg/L; k and b are both constants.
In some embodiments, the method for determining the content of calcium oxide in samarium oxide further comprises a step of removing acid from the samarium oxide sample solution before the step of adjusting the pH of the samarium oxide sample solution to 9 to 11 by using ammonia water.
In some embodiments, the method for determining the content of calcium oxide in samarium oxide further comprises the step of diluting the samarium oxide sample solution with water before the step of adjusting the pH of the samarium oxide sample solution to 9 to 11 with ammonia water.
In some embodiments, in the method for measuring the content of calcium oxide in samarium oxide, in the step of measuring the emission intensity of calcium ions in the plurality of calcium ion standard solutions respectively by ICP-OES, the method further comprises the step of adding ammonia water to each of the plurality of calcium ion standard solutions.
Compared with the prior art, the method for measuring the content of calcium oxide in the samarium oxide has the following beneficial effects:
the method for measuring the content of calcium oxide in the samarium oxide adopts an ICP-OES method to obtain a standard curve equation of emission intensity and calcium ion concentration, adopts the ICP-OES method to measure the emission intensity of the samarium oxide sample, and calculates the content of calcium oxide in the samarium oxide sample according to the standard curve equation. Wherein, after dissolving a samarium oxide sample with an acid solution, the obtained samarium oxide sample solution is adjusted to a specific pH value with ammonia water, since samarium hydroxide (Ksp =4.6 × 10) -12 ) And calcium hydroxide (Ksp =5.5 × 10) -6 ) The solubility product of the method has larger difference, the effects that the samarium matrix is completely precipitated and calcium ions are not precipitated can be basically realized under the condition of the specific pH value, the interference of the samarium matrix on the matrix for calcium ion determination is effectively solved, and the accuracy of the determination result is effectively improved.
According to the method for measuring the content of calcium oxide in the samarium oxide, an inductively coupled plasma emission spectrometer (ICP-OES) is relatively low in price, high-purity samarium oxide is not needed, the operation is simple and rapid, and the method is suitable for batch measurement.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a standard curve of the emission intensity versus the calcium ion concentration obtained in example 1.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. It is to be understood that these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The weight of the related components mentioned in the description of the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present invention as long as it is in accordance with the description of the embodiments of the present invention. Specifically, the weight described in the description of the embodiment of the present invention may be a unit of mass known in the chemical industry field, such as μ g, mg, g, and kg.
The embodiment of the invention provides a method for measuring the content of calcium oxide in samarium oxide, which comprises the following steps of S10-S40:
step S10: providing a samarium oxide sample, and dissolving the samarium oxide sample by using an acid solution to obtain a samarium oxide sample solution.
It is understood that acid solutions include, but are not limited to, nitric acid, hydrochloric acid, perchloric acid, sulfuric acid, acetic acid, hydrofluoric acid, hypochlorous acid.
In some examples, in step S10, the acid solution is at least one selected from nitric acid, hydrochloric acid, and perchloric acid.
Optionally, the acid solution is nitric acid.
In some examples, in step S10, the acid solution is 30% to 60% by mass.
It is understood that the mass fraction of the acid solution includes, but is not limited to, 30%, 35%, 40%, 45%, 50%, 55%, 56%, 57%, 58%, 59%, 60%.
In some examples, in step S10, the acid solution is 40% to 60% by mass.
Optionally, the acid solution has a mass fraction of 55% to 60%.
In some specific examples, in step S10, the acid solution is nitric acid (1+1).
It is understood that nitric acid (1+1) is formulated from 1 volume of concentrated nitric acid and 1 volume of water. It is further understood that the mass fraction of nitric acid (1+1) is about 58.33%.
In some examples, in step S10, the ratio of the mass of the samarium oxide sample to the volume of the acid solution is (0.1 to 0.5) g/1mL.
It is understood that the ratio of the mass of the samarium oxide sample to the volume of the acid solution includes, but is not limited to, 0.1g/1mL, 0.125g/1mL, 0.15g/1mL, 0.2g/1mL, 0.25g/1mL, 0.3g/1mL, 0.35g/1mL, 0.4g/1mL, 0.45g/1mL, 0.5g/1mL.
In some specific examples, in step S10, the ratio of the mass of the samarium oxide sample to the volume of the acid solution is 0.125g/1mL.
Step S20: adjusting the pH value of a samarium oxide sample solution to 9-11 by adopting ammonia water, carrying out solid-liquid separation, taking supernate, and measuring the emission intensity of calcium ions in the supernate by adopting ICP-OES.
It is understood that a pH of 9 to 11 includes, but is not limited to, 9, 9.2, 9.5, 9.8, 10, 10.2, 10.5, 10.8, 11.
In some examples, ammonia is used to adjust the pH of the samaric oxide sample solution to 9-10 in step S20.
Ksp =4.6 × 10 for samarium hydroxide Sm (OH) 3 -12 Calcium hydroxide Ca (OH) 2 Ksp =5.5 × 10 -6 The pH value of a samarium oxide sample solution is controlled in a specific range by adopting ammonia water, so that the samarium oxide test is effectively ensuredThe samarium matrix in the sample solution is completely precipitated, and the calcium ions are not precipitated, so that the interference of the samarium matrix on the matrix for calcium ion determination is effectively solved, and the accuracy of the determination result is effectively improved.
In some examples, in step S20, the solid-liquid separation is performed by centrifugation.
The centrifugal method is adopted to realize rapid separation of the samarium hydroxide and the calcium ion solution, so that the calcium pollution caused by filtering by using filter paper is effectively avoided, and the problem of penetration caused by the slow filtering speed of the samarium hydroxide is solved, thereby further improving the accuracy of the measurement result.
In some examples, in step S20, the mass fraction of the ammonia water is 10% to 50%.
It is understood that the mass fraction of ammonia includes, but is not limited to, 10%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 20%, 25%, 28%, 30%, 35%, 40%, 45%, 50%.
In some specific examples, in step S20, the aqueous ammonia is aqueous ammonia (1+5).
It is understood that aqueous ammonia (1+5) is formulated from 1 volume of concentrated ammonia and 5 volumes of water. It is further understood that the mass fraction of ammonia (1+5) is about 15.4%.
In some examples, in step S20, before the step of adjusting the pH of the samarium oxide sample solution to 9 to 11 by using ammonia water, a step of performing acid removal on the samarium oxide sample solution is further included.
In some examples, in step S20, acid is removed by heating.
The samarium oxide sample solution is treated with acid, so that the consumption of ammonia water for subsequent pH value adjustment can be reduced, and the sample pretreatment time is shortened.
In some examples, step S20 further includes a step of diluting the samarium oxide sample solution with water before the step of adjusting the pH of the samarium oxide sample solution to 9 to 11 with ammonia water.
It can be understood that the samarium oxide sample solution is diluted by water and then the pH value is adjusted by ammonia water.
It can be understood that when the calcium oxide content in the samarium oxide sample is calculated subsequently, the calculation is carried out according to the dilution factor.
In some specific examples, in step S20, the samaric oxide sample solution is treated with acid-removing treatment, diluted with water, and adjusted to pH with ammonia water.
It can be understood that the speed of centrifugation does not need to be strictly controlled, and the samarium hydroxide can be settled to the bottom.
In some examples, in step S20, the centrifugation speed is 3000 r/min-5000 r/min, and the centrifugation time is 1 min-60 min.
In some specific examples, in step S20, the speed of centrifugation is 4000r/min and the time is 10min.
The centrifugal method is adopted to realize rapid separation of the samarium hydroxide and the calcium ion solution, so that the calcium pollution caused by filtering by using filter paper is effectively avoided, and the problem of penetration caused by the slow filtering speed of the samarium hydroxide is solved, thereby further improving the accuracy of the measurement result.
Step S30: providing a plurality of calcium ion standard solutions with different calcium ion concentrations, and respectively measuring the emission intensity of calcium ions in the plurality of calcium ion standard solutions by adopting ICP-OES to obtain a standard curve equation of the emission intensity and the calcium ion concentration.
It will be appreciated that the standard curve is usually made at 4 to 6 points, so 4 to 6 standard solutions of calcium at different concentrations are provided. It is also understood that the plurality of calcium ion standard solutions having different calcium ion concentrations are not limited to 4 to 6 different concentrations.
In some specific examples, in step S30, a plurality of calcium ion standard solutions with different calcium ion concentrations may be configured as follows:
providing a calcium ion concentration of C 0 Respectively taking standard solution AM 1 Volume, M 2 Volume, M 3 Volume, M 4 Volume, M 5 Putting other volumes such as the volume and the like into different volumetric flasks with the same volume respectively, and adding water to the volume to obtain calcium ion concentrations C 1 、C 2 、C 3 、C 4 、C 5 Etc. other concentrationThe calcium standard solution of (1).
In some examples, in step S30, the step of measuring the emission intensity of calcium ions in the plurality of calcium ion standard solutions by using ICP-OES further includes the step of adding ammonia water to the plurality of calcium ion standard solutions.
It can be understood that, when the emission intensity of the samarium oxide sample solution is measured by the ICP-OES in the step S20, the samarium oxide sample solution contains ammonium ions, and the influence of the ammonium ions on the measurement of calcium ions is small; and ammonia water is added into various calcium ion standard solutions respectively, so that the influence of ammonium ions on calcium ion determination can be further completely eliminated.
It is also understood that, in the step of preparing the calcium standard solution, the amount of ammonia water added is in accordance with the amount of ammonia water used in step S20.
In some examples, in step S30, the standard curve equation of the emission intensity versus the calcium ion concentration is:
Y＝k·X+b
wherein Y is the emission intensity; x is the concentration of calcium ions in the test solution, and the unit is mg/L; k and b are both constants.
It is to be understood that steps S10 to S20 and S30 are not in sequence, and that steps S10 to S20 may be performed first and then step S30 may be performed, step S30 may be performed first and then steps S10 to S20 may be performed, or steps S10 to S20 and step S30 may be performed simultaneously.
It can also be understood that the parameters of the ICP-OES instrument may be self-determined according to the instrument condition, and it is sufficient to ensure that the parameters in the ICP-OES measurement in step S20 and step S30 are consistent.
In some examples, in the method for determining the content of calcium oxide in samarium oxide, the operating conditions of ICP-OES may be:
the emission power is 0.5 kW-2.0 kW;
the flow rate of the plasma gas is 10.0L/min-20.0L/min;
the auxiliary gas flow is 1L/min-2L/min;
the pressure of the atomizer is 100KPa to 300KPa;
the observation height is 5 mm-20 mm;
the reading time for one time is 2 s-10 s;
the stable delay time of the instrument is 10 s-20 s;
the sample introduction time delay is 20-40 s;
the pump speed is 10 r/min-20 r/min;
the cleaning time is 5 s-20 s.
In some specific examples, in the method for determining the content of calcium oxide in samarium oxide, the operating conditions of ICP-OES are as follows: the emission power is 1.0kW, the plasma gas flow is 15.0L/min, the auxiliary gas flow is 1.50L/min, the atomizer pressure is 200KPa, the observation height is 10mm, the one-time reading time is 5s, the instrument stability time delay is 15s, the sample injection time delay is 30s, the pump speed is 15r/min, and the cleaning time is 10s.
In some specific examples, the wavelength of the calcium oxide in the samarium oxide is selected from the group consisting of Ca 396.847nm.
Step S40: and calculating to obtain the content of calcium oxide in the samarium oxide sample according to a standard curve equation.
It can be understood that the emission intensity Y of the samarium oxide sample is measured in the step S20, and the calcium ion concentration X in the samarium oxide sample is calculated according to the standard curve equation Y = k · X + b; then the calcium oxide content in the samarium oxide sample is obtained by calculation according to the formula W% = 1.3992X (X.dilution multiple)/m X100; wherein W is the mass fraction of calcium oxide in a samarium oxide sample; x is the concentration of calcium ions in the test solution, and the unit is mg/L; and m is the weighing amount of the samarium oxide sample.
It is understood that X.dilution factor is the mass of calcium ion, and 1.3992 × (X.dilution factor) is the mass of calcium oxide.
In some examples, the method for determining the content of calcium oxide in samarium oxide further comprises a step of performing a blank test.
In some of these examples, the blank test comprises the steps of:
adding acid liquor which is equal to the sample of the dissolved samarium oxide to drive acid; adding ammonia water which is equal to the amount of the sample group to obtain a blank solution;
emission intensity of the blank solution was measured using ICP-OES.
It can be understood that the standard curve squareIn the process Y = step S20, the emission intensity Y of the samarium oxide sample is measured 1 Emission intensity Y measured in blank test 2 。
It can be further understood that by performing a blank test, the influence of the reagent, water, environment and the like on the calcium ion measurement can be eliminated.
The method for measuring the content of calcium oxide in the samarium oxide adopts an ICP-OES method to obtain a standard curve equation of emission intensity and calcium ion concentration, adopts the ICP-OES method to measure the emission intensity of the samarium oxide sample, and calculates the content of calcium oxide in the samarium oxide sample according to the standard curve equation. After the samarium oxide sample is dissolved by the acid solution, the obtained samarium oxide sample solution is adjusted to a specific pH value by using ammonia water, and the effects that the samarium matrix is completely precipitated and the calcium ion is not precipitated can be basically realized under the condition of the specific pH value due to the large difference of solubility products of the samarium hydroxide and the calcium hydroxide, so that the interference of the samarium matrix on the matrix for calcium ion determination is effectively solved, and the accuracy of the determination result is effectively improved.
Furthermore, the centrifugal method is adopted to realize rapid separation of the samarium hydroxide and the calcium ion solution, so that the problems of calcium pollution caused by filtering by using filter paper and penetration caused by low filtering speed of the samarium hydroxide are effectively avoided, and the accuracy of a measurement result is further improved.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Hereinafter, the method for measuring the content of calcium oxide in samarium oxide according to the present invention is exemplified, and it is understood that the method for measuring the content of calcium oxide in samarium oxide according to the present invention is not limited to the following examples.
Example 1
1. The main apparatus is as follows: ICP-OES, a graphite furnace and a centrifugal machine;
2. reagent: nitric acid (1 +1, GR), ammonia water (1 +5, GR), C (Ca) =1000 mug/mL standard stock solutions, and experimental water are all ultrapure water;
3. procedure of the test
3.1. Weighing 0.2500g (accurate to 0.0001 g) of samarium oxide, wetting with a small amount of water, adding 2mL (1+1) of nitric acid, heating to nearly dry, transferring the solution with the size of the rest mung bean into a 50mL volumetric flask after cooling, adding 40mL of water and 4mL (1+5) of ammonia water, metering to a scale, and measuring by a pH meter, wherein the pH of the samarium oxide sample solution is 9.5;
3.2. transferring the samarium oxide sample solution to a centrifugal tube, setting the rotating speed to be 4000r/min, centrifuging for 10min, and transferring the supernatant to a clean cup to be tested;
along with the blank test and the parallel test, the blank solution was prepared as follows:
adding 2mL of nitric acid (58.33%) into plastic Wang Beizhong, heating to be nearly dry, transferring the solution with the size of the mung beans to a 50mL volumetric flask after cooling, adding 40mL of water and 4mL of (1+5) ammonia water, and fixing the volume to the scale;
3.3. preparing a standard solution: diluting a standard stock solution of C (Ca) =1000 mug/mL into a standard stock solution A of C (Ca) =10 mug/mL, respectively taking 0.25mL, 1mL, 2mL and 10mL of standard preparation solutions, respectively placing the standard preparation solutions in a 50mL volumetric flask, adding 4mL of ammonia water (1+5), and fixing the volume to a scale by using ultrapure water, wherein the concentrations of the standard series solutions are respectively 0.050mg/L,0.20mg/L,0.40mg/L,1.00mg/L and 10mg/L;
icp-OES test, instrument: ICP-0ES700 model full spectrum direct reading inductively coupled plasma emission spectrometer (Agilent);
the working conditions are as follows: the emission power is 1.0kW, the plasma gas flow is 15.0L/min, the auxiliary gas flow is 1.50L/min, the pressure of an atomizer is 200KPa, the observation height is 10mm, the one-time reading time is 5s, the instrument stability time delay is 15s, the sample introduction time delay is 30s, the pump speed is 15r/min, and the cleaning time is 10s;
after the ignition of the instrument is stable, sequentially measuring the series of standard solutions, selecting the wavelength of Ca 396.847nm, and drawing a standard curve as shown in figure 1; the standard curve equation is Y =7979.1X +465.64; r 2 ＝0.9996；
3.5. Measuring the emission intensity of the sample solution as Y 1 Emission intensity of blank solution is Y 2 Will delta Y (= Y) 1 -Y 2 ) Substituting the standard curve equation into the solution to be detected to calculate the concentration X of calcium ions in the solution to be detected, and calculating according to the formula W% = 1.3992X (X dilution times)/mx 100 to obtain the content of calcium oxide in the samarium oxide; wherein W is the mass fraction of calcium oxide in a samarium oxide sample; x is calcium ion in the test liquidSub-concentrations in mg/L; and m is the weighing amount of the samarium oxide sample.
4. As a result, the
And (3) testing accuracy: taking 3 parts of practical samarium oxide samples No. 1, no. 2, no. 3 and No. 4, and respectively detecting the content of calcium oxide in the samarium oxide samples by using GB/T12690.15-2018 and the measuring method of the embodiment 1, wherein the results are shown in a table 1.
TABLE 1
And (3) testing precision: 11 parallel samples were weighed and tested, and the RSD of the measurement results was calculated, and the results are shown in Table 2.
TABLE 2
| Sample numbering | RSD |
| Samarium oxide sample No. 1 | 3.32 |
| Samarium oxide sample No. 2 | 2.37 |
| Samarium oxide sample No. 3 | 2.21 |
As can be seen from tables 1 and 2, the precision and accuracy of the determination method in example 1 both meet the requirements of Standard GB/T27404-2008 "laboratory quality control Specification food physicochemical detection", and the determination accuracy is high.
Example 2
The method is substantially the same as in example 1 except that in step 3.1 of example 2, the pH of a sample solution of samarium oxide is 10.
Blank and parallel tests were performed.
And (3) testing accuracy: the content of calcium oxide in the samarium oxide sample is detected by the measuring method of the embodiment 2 by taking practical samarium oxide samples 1#, 2#, and 3#, and the results are compared with the results of the measuring method of GB/T12690.15-2018, and are shown in the table 3.
TABLE 3
Example 3
The method is basically the same as the method in the embodiment 1, and is different from the method in the embodiment 3 in that the step 3.2 is as follows:
and (4) filtering the samarium oxide sample solution prepared in the step (3.1) by adopting rapid quantitative filter paper, and taking a filtrate to be tested.
Blank and parallel tests were performed.
And (3) testing accuracy: the calcium oxide content in the samarium oxide sample is measured by taking practical samarium oxide samples 1# and 4# and respectively using GB/T12690.15-2018 and the measuring method of example 3, and the results are shown in Table 4.
TABLE 4
As can be seen from table 4, it is shown that for trace calcium, the use of centrifugation introduces less contamination, and centrifugation is more suitable for detection of trace calcium than filtration with filter paper.
Comparative example 1
Essentially the same as example 1, except that comparative example 1, step 3.1, was as follows:
3.1. weighing 0.2500g (accurate to 0.0001 g) of samarium oxide, wetting with a small amount of water, adding 2mL (1+1) of nitric acid, heating to be nearly dry, transferring the solution with the size of the rest mung bean into a 50mL volumetric flask after cooling, adding 40mL of water and 3mL (1+5) of ammonia water, fixing the volume to the scale, and measuring by a pH meter, wherein the pH of the samarium oxide sample solution is 8.3.
Blank and parallel tests were performed.
And (3) testing accuracy: and (3) taking practical samarium oxide samples No. 1 and No. 2, detecting the content of calcium oxide in the samarium oxide sample by using the detection method of the comparative example 1, and comparing the content with the results of the detection methods of the example 1 and GB/T12690.15-2018, wherein the results are shown in a table 5.
TABLE 5
As can be seen from Table 5, compared with example 1, the measurement result of comparative example 1 is greatly different from the measurement result of GB/T12690.15-2018, and the interference of the samarium oxide matrix on the calcium ion measurement cannot be eliminated.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, which is convenient for specific and detailed understanding of the technical solutions of the present invention, but the present invention should not be construed as being limited to the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. It should be understood that the technical solutions provided by the present invention, which are obtained by logical analysis, reasoning or limited experiments, are within the scope of the appended claims. Therefore, the protection scope of the present invention should be subject to the content of the appended claims, and the description and the drawings can be used for explaining the content of the claims.
Claims (10)
1. A method for measuring the content of calcium oxide in samarium oxide is characterized by comprising the following steps:
providing a samarium oxide sample, and dissolving the samarium oxide sample by using acid liquor to obtain a samarium oxide sample solution;
adjusting the pH value of the samarium oxide sample solution to 9-11 by adopting ammonia water, carrying out solid-liquid separation, taking supernatant, and measuring the emission intensity of calcium ions in the supernatant by adopting ICP-OES (inductively coupled plasma-optical emission spectrometry);
providing a plurality of calcium ion standard solutions with different calcium ion concentrations, and respectively measuring the emission intensity of calcium ions in the plurality of calcium ion standard solutions by adopting ICP-OES (inductively coupled plasma-optical emission spectrometry) to obtain a standard curve equation of the emission intensity and the calcium ion concentration;
and calculating to obtain the content of calcium oxide in the samarium oxide sample according to the standard curve equation.
2. The method of claim 1, in which the solid-liquid separation is performed by centrifugation.
3. The method for measuring the content of calcium oxide in samarium oxide according to claim 1, wherein the acid solution is at least one selected from the group consisting of nitric acid, hydrochloric acid and perchloric acid.
4. The method of claim 3, in which the acid solution is nitric acid.
5. The method for determining the content of calcium oxide in samarium oxide according to claim 1, wherein the acid solution comprises 30 to 60% by weight.
6. The method for measuring the content of calcium oxide in samarium oxide of claim 1, wherein the ammonia is present in an amount ranging from 10% to 50% by weight.
7. The method for determining the content of calcium oxide in samarium oxide according to any of claims 1 to 6, wherein the standard curve equation of the emission intensity and the calcium ion concentration is as follows:
Y＝k·X+b
wherein Y is the emission intensity; x is the concentration of calcium ions in the test solution, and the unit is mg/L; k and b are both constants.
8. The method of measuring the content of calcium oxide in samarium oxide according to any of claims 1 to 6, further comprising a step of removing an acid from the sample solution of samarium oxide before the step of adjusting the pH of the sample solution of samarium oxide to 9 to 11 with aqueous ammonia.
9. The method of measuring the content of calcium oxide in samarium oxide according to any of claims 1 to 6, further comprising a step of diluting the samarium oxide sample solution with water before the step of adjusting the pH of the samarium oxide sample solution to 9 to 11 with aqueous ammonia.
10. The method of measuring the content of calcium oxide in samarium oxide according to any of claims 1 to 6, further comprising a step of adding ammonia water to each of the plurality of the calcium ion standard solutions in the step of measuring the emission intensity of calcium ions in each of the plurality of the calcium ion standard solutions by ICP-OES.
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