CN113030065B - Method for detecting disodium tetraborate in oxide removing agent - Google Patents
Method for detecting disodium tetraborate in oxide removing agent Download PDFInfo
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Abstract
The invention provides a method for detecting disodium tetraborate in an oxide removing agent, which comprises the following steps of: (1) pretreating an oxide reagent sample; (2) preparing a sample test solution; (3) selecting element detection spectral lines; (4) drawing a standard curve; (5) and detecting the sample. The method solves the inapplicability of the national standard method to detecting the disodium tetraborate in the oxide removing agent by utilizing the inductively coupled plasma emission spectrum, has higher accuracy and precision, high standard adding recovery rate and good linear relation, and can meet the requirements of quick and accurate production detection.
Description
Technical Field
The invention belongs to the field of metallurgical analysis, and relates to a method for detecting disodium tetraborate in an oxide removing agent, in particular to a method for detecting disodium tetraborate in an oxide removing agent by utilizing inductively coupled plasma emission spectroscopy (ICP-AES).
Background
The oxide removing agent plays an important role in the rolling process of the steel pipe, has various types, and is a common type consisting of sodium sulfate, borax, sodium phosphate and sodium stearate. The current method for detecting disodium tetraborate in the oxide removing agent adopts the national standard GB/T537-2009. However, this standard is used for detecting borax raw materials with industrial purity, and is not applicable to detecting oxide agents with various material compositions. The reason for the inapplicability is mainly that the presence of sodium phosphate consumes sodium hydroxide solution, whereas the content of sodium phosphate in the oxide agent is rather high, leading to a final result that is far higher than practical. The oxidation removing agent is heated by water to be dissolved, but with the reduction of the temperature in the subsequent titration test process, a large amount of white insoluble matters are formed, and the active ingredients to be detected can be wrapped, so that the final analysis result is affected. Moreover, titration analysis is complicated, time-consuming and difficult to adapt to the faster and faster production pace.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for detecting disodium tetraborate in an oxide removing agent by utilizing an inductively coupled plasma emission spectrum, so as to solve the inapplicability of national standard GB/T537-2009 and rapidly and accurately detect the disodium tetraborate in the oxide removing agent.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a method for detecting disodium tetraborate in an oxide removing agent, which comprises the following steps of:
pretreatment of the oxide reagent sample: burning the sample of the oxide removing agent at 400-500 ℃ for 0.5-1 hour, cooling, dissolving with water, filtering, and fixing the volume to obtain a sample stock solution;
preparing a sample test solution: the nitric acid solution is used for fixing the volume of the sample stock solution to obtain a sample test solution;
selecting element detection spectral lines: selecting an optimal analysis spectral line according to interference conditions;
drawing a standard curve: drawing a standard curve by taking the gradient concentration of the boron standard solution as an abscissa and the intensity of emitted light as an ordinate;
detecting a sample: detecting the emitted light intensity of a sample solution by utilizing an inductively coupled plasma emission spectrum, and obtaining the percentage content of disodium tetraborate in the sample according to a standard curve;
the working conditions of the inductively coupled plasma emission spectrum are as follows: RF power 1150w, pump speed 50r/min, atomizer flow 0.6L/min, auxiliary air flow 0.5L/min, and viewing height 12cm.
Further, the optimal analytical line is 182.5nm.
Further, the oxide removing agent consists of sodium sulfate, borax, sodium phosphate and sodium stearate.
Further, the volume percentage concentration of the nitric acid solution is 0.5%.
Further, the oxide removing agent consists of 9.91-15.55% of sodium stearate, 12.63-29.98% of sodium sulfate, 26.99-34.94% of sodium phosphate and 19.87-30.05% of borax.
Further, the borax is anhydrous borax or decahydrate borax.
Further, the gradient concentration of the boron standard solution is 0mg/L, 10mg/L, 20mg/L and 30mg/L.
The beneficial effects of the invention are as follows:
the invention adopts the mode of burning for 0.5 to 1 hour at 400 to 500 ℃, cooling and dissolving with water, and can rapidly filter the burnt residues, the filtrate is clear and transparent, and the filtering and the washing are only needed for less than 1 hour; the content of disodium tetraborate in the oxide removing agent is detected by utilizing the inductively coupled plasma emission spectrum, the titration interference of sodium phosphate in the national standard method is overcome, the problem of difficult filtration in the sample dissolution process is solved, the analysis process is quick and simple, the result is accurate and reliable, and the production detection requirement of enterprises can be met.
Detailed Description
The invention is described in further detail below with reference to specific embodiments:
examples
1. Instrument and operating conditions
Instrument apparatus: ICAP 7200 inductively coupled plasma emission spectrum (sammer, inc.).
Working conditions: RF power 1150w, pump speed 50r/min, atomizer flow 0.6L/min, auxiliary air flow 0.5L/min, and viewing height 12cm.
2. Primary reagents and materials
Experimental water: ultrapure water;
nitric acid: ρ=1.12 g/mL, analytically pure;
anhydrous sodium sulfate: analytically pure;
borax decahydrate: high-grade purity;
anhydrous borax: is obtained by burning borax decahydrate at 500 ℃ until the quality is constant;
sodium phosphate: an industrial grade;
sodium stearate: analytically pure;
national standard boron solution: 1000mg/L;
since the oxide removing agent has no commercial standard substance, the standard oxide removing agent is self-prepared, and the specific composition is shown in table 1:
table 1 composition of standard oxide removal agent and treatment conditions
The borax used in the marks 1-3 is anhydrous borax, and the disodium tetraborate content can be directly obtained according to weighing calculation; borax used in the mark 4 and the mark 5 is borax decahydrate, and the disodium tetraborate content is obtained through conversion of chemical formula relation.
The containers used throughout the test were plastic containers.
3. Sample processing and detection
Weigh 5g of sample into corundum crucible. The firing temperatures and firing times used for marks 1-5 are shown in Table 1. After the burning is finished and cooled, the mixture is dissolved by water, filtered and washed into a 500mL volumetric flask, and the volume is fixed by water to obtain a sample stock solution. And transferring 2mL of the sample stock solution into a 100mL volumetric flask, and fixing the volume by using a nitric acid solution with the volume percentage concentration of 0.5% to obtain a sample test solution.
The optimal analysis spectral line is 182.5nm according to the interference condition. And drawing a standard curve by taking gradient concentrations of 0mg/L, 10mg/L, 20mg/L and 30mg/L of boron standard solution as an abscissa and the emitted light intensity as an ordinate. The linear correlation coefficient of the obtained standard curve was 0.999948. And detecting the emission light intensity of the obtained sample solution by utilizing the inductively coupled plasma emission spectrum, and obtaining the content of disodium tetraborate in the sample according to a standard curve. The conversion formula is as follows:
w 1 : the boron content is read out according to a standard curve, mg/L;
M 1 : the relative atomic mass, g/mol, of boron;
M 2 : relative molecular mass, g/mol, of disodium tetraborate;
V 1 : the volume of the sample stock solution, L;
V 2 : the volume of the removed sample stock solution is L;
V 3 : the volume of the sample solution L;
m: sample mass, g.
The mass percentage results of the disodium tetraborate obtained by the method are shown in table 2.
4. Accuracy and precision
Table 2 accuracy and precision results
By comparing the disodium tetraborate contents of sample nos. 1 to 5 in tables 1 and 2, it can be seen that the disodium tetraborate content obtained by the method is very close to the disodium tetraborate content obtained by weighing calculation, and the difference is only 0.16% at minimum. This shows that the use of inductively coupled plasma emission spectroscopy to detect the disodium tetraborate content in the oxide removal agent has a high degree of accuracy.
As can be seen from the relative standard deviation data in Table 2, the relative standard deviation of each of the marks 1 to 5 is less than 0.39%, which indicates that the method has higher precision in detecting the disodium tetraborate content in the oxide removing agent.
5. Recovery rate
The production sample L1 was subjected to a labeled recovery test. L1 was treated in the same manner as in standard 2, with the addition of standard boron solution, scalar addition and results as shown in Table 3.
TABLE 3 recovery results
As can be seen from Table 3, the labeled recovery result is between 99.6 and 103 percent, which shows that the sample composition has no obvious effect on the detection of the disodium tetraborate in the method, and also shows that the method for detecting the disodium tetraborate in the oxide removing agent has higher accuracy.
Comparative example
The standard 4 sample is detected according to the method of national standard GB/T537-2009, the result is 29.45%, and compared with 20.06% obtained by weighing calculation and 20.41% obtained by the method, the national standard method has lower accuracy. This is mainly due to the presence of sodium phosphate, the sodium hydroxide solution consumed, and thus the measurement results are much higher than the actual value. Therefore, the method is more suitable for detecting the disodium tetraborate in the oxide removing agent.
In addition, it was found by test that the oxide-removing agent is not easily dissolved in water at normal temperature. After heating to dissolve, white insoluble matters appear along with the reduction of the temperature in the subsequent experimental process; if the solution is directly introduced into ICP-AES, the sampling system is blocked and cannot be detected. The solution was filtered, but there was difficulty in filtration. Filtered and washed clean, requiring at least one day. When the temperature of 300 ℃ is adopted for burning, the filtrate is brownish black, and if the filtrate is introduced into a spectrometer, interference can be brought, and the filtering and washing time is long, namely about 3 hours. When the temperature is 600 ℃, the sample is melted and firmly attached to the bottom of the crucible after being cooled, and the sample cannot be dissolved and transferred.
The test data show that the method for detecting the disodium tetraborate in the oxide removing agent can solve the inapplicability of detecting the disodium tetraborate in the oxide removing agent by utilizing the inductively coupled plasma emission spectrum, has higher accuracy and precision, high standard adding recovery rate and good linear relation, and can meet the requirements of rapid and accurate production detection.
Claims (6)
1. A method for detecting disodium tetraborate in an oxidation inhibitor, comprising the steps of:
pretreatment of the oxide reagent sample: burning the sample of the oxide removing agent at 400-500 ℃ for 0.5-1 hour, cooling, dissolving with water, filtering, and fixing the volume to obtain a sample stock solution;
preparing a sample test solution: the nitric acid solution is used for fixing the volume of the sample stock solution to obtain a sample test solution;
selecting element detection spectral lines: selecting an optimal analysis spectral line according to interference conditions;
drawing a standard curve: drawing a standard curve by taking the gradient concentration of the boron standard solution as an abscissa and the intensity of emitted light as an ordinate;
detecting a sample: detecting the emitted light intensity of a sample solution by utilizing an inductively coupled plasma emission spectrum, and obtaining the percentage content of disodium tetraborate in the sample according to a standard curve;
the working conditions of the inductively coupled plasma emission spectrum are as follows: RF power is 1150w, pump speed is 50r/min, atomizer flow is 0.6L/min, auxiliary air flow is 0.5L/min, and observation height is 12cm;
the oxide removing agent consists of sodium sulfate, borax, sodium phosphate and sodium stearate.
2. A method of detecting disodium tetraborate in an oxidation inhibitor according to claim 1, wherein: the optimal analytical line was 182.5nm.
3. A method of detecting disodium tetraborate in an oxidation inhibitor according to claim 1, wherein: the volume percentage concentration of the nitric acid solution is 0.5%.
4. A method of detecting disodium tetraborate in an oxidation inhibitor according to claim 1, wherein: the deoxidizer consists of 9.91-15.55% of sodium stearate, 12.63-29.98% of sodium sulfate, 26.99-34.94% of sodium phosphate and 19.87-30.05% of borax for enabling the content of disodium tetraborate.
5. The method for detecting disodium tetraborate in an oxide removing agent according to claim 4, wherein: the borax is anhydrous borax or decahydrate borax.
6. A method of detecting disodium tetraborate in an oxidation inhibitor according to claim 1, wherein: the gradient concentration of the boron standard solution is 0mg/L, 10mg/L, 20mg/L and 30mg/L.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103033498A (en) * | 2012-12-21 | 2013-04-10 | 深圳市谱尼测试科技有限公司 | Method for simultaneously detecting substances of very high concern (SVHC) boric acid and borax of registration, evaluation, authorization and restriction of chemicals (REACH) law of European Union |
| CN104535709A (en) * | 2014-12-23 | 2015-04-22 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of sodium tetraborate in sintering promoting agent |
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| CN101846629B (en) * | 2010-04-30 | 2011-11-09 | 浙江出入境检验检疫局检验检疫技术中心 | Method for measuring boric acid and borate in cosmetics by microwave digestion -ICP-OES |
| CN109540804A (en) * | 2018-09-30 | 2019-03-29 | 大冶特殊钢股份有限公司 | The detection method of boron element in a kind of manganeisen |
| CN111504982A (en) * | 2020-04-23 | 2020-08-07 | 广州海关技术中心 | Method for measuring boron content in glass by inductively coupled plasma emission spectrometry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103033498A (en) * | 2012-12-21 | 2013-04-10 | 深圳市谱尼测试科技有限公司 | Method for simultaneously detecting substances of very high concern (SVHC) boric acid and borax of registration, evaluation, authorization and restriction of chemicals (REACH) law of European Union |
| CN104535709A (en) * | 2014-12-23 | 2015-04-22 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of sodium tetraborate in sintering promoting agent |
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