CN102661991A - Method for measuring content of acid-solvable boron in steel - Google Patents

Method for measuring content of acid-solvable boron in steel Download PDF

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CN102661991A
CN102661991A CN2012101559767A CN201210155976A CN102661991A CN 102661991 A CN102661991 A CN 102661991A CN 2012101559767 A CN2012101559767 A CN 2012101559767A CN 201210155976 A CN201210155976 A CN 201210155976A CN 102661991 A CN102661991 A CN 102661991A
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boron
acid
steel
solution
sample
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丁美英
石琳
田永生
刘淼
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Baotou Iron and Steel Group Co Ltd
Inner Mongolia Baotou Steel Union Co Ltd
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Baotou Iron and Steel Group Co Ltd
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Abstract

The invention provides a method for measuring the content of acid-solvable boron in steel, belonging to the technical field of analytical chemistry. The method comprises the following steps of: dissolving a sample with sulfuric acid with the concentration of 5 mol/L at a low temperature in the absence of an oxidant; diluting until a ruled volume is reached; and measuring acid-solvable boron by using an inductive coupling plasma mass spectrometer. With the adoption of the method provided by the invention, the content of the acid-solvable boron in the steel is measured in an accurate, rapid, simply and conveniently operated, and non-pollution manner.

Description

Boron Determination on content method is dissolved in acid in a kind of steel
One, technical field
The invention belongs to technical field of analytical chemistry, relate to the quantitative analysis tech of the molten boron of acid in a kind of steel.
Two, background technology
Since 20 beginnings of the century found that the adding boron element can improve quenching degree in the steel, boron had carried out a large amount of research and application as micro alloying element in HSLA, structural carbon steel, stainless steel, heat-resisting steel and high temperature alloy.The superiority that boron-containing steel had is very obvious, boron aboundresources, low price and also in steel content few, in supply, do not have problems; Particularly under the high background of global financial crisis, steel industry over capacity, homogeneity intensified competition, resources costs, but in order to replacing the not only pressure of alleviate resource supply of valuable alloying element, and also worthwhile economically; The production of boron steel, application, research work also will constantly develop, enlarge.The molten boron of acid is one of project of analyzing usually in the metallurgical analysis in the steel, at present, and the existing GB of the mensuration of the molten boron of acid in the steel; But limit for height under this methods analyst long flow path, trivial operations, the analysis, and adopt objectionable impurities such as methyl alcohol, therefore use be absolutely unsafe, convenient; We have invented this method through experiment, and this method accurately, fast; Easy and simple to handle, safety have reduced the analysis lower limit.
Three, summary of the invention
The objective of the invention is to disclose the molten boron Determination on content method of acid in a kind of steel, utilize this method can measure the content of the molten boron of acid in the steel safely, fast and accurately.
At first, confirm the span of correlation parameter through experiment and to the influence factor of assay method.
1, Instrument working parameter
Instrument title: ELAN DRC-e ICP-MS mass spectrometer (U.S. PE manufactured)
The running parameter of ICP-MS mass spectrometer instrument is single charge ion intensity and multi-atomic ion intensity such as the oxide that possibly produce interference, sulfide of influence element to be measured directly.For this reason, before measuring, the Mg, In, Ba, Ce, U mixed standard solution (tuning solution) that at first adopts 10 μ g/mL carries out to mass spectrometer that parameters such as mass calibration, resolution are tuning, the correction of lens voltage detecting device are selected, correction work.Utilize the Tuning and the Optimize function of instrument, be optimized and obtain Instrument working parameter, see table 1.
Table 1: Instrument working parameter
2, the selection of instrument test condition
With the mixed standard solution of multiple elements such as the iron matrix that contains micro-sulfuric acid, boron, carry out the condition test of power, atomizer flow, secondary air amount etc. successively, the result shows:
1) along with the increase (increasing to 1300W from 900W) of power, line strength of boron increases, and power is when 1050W～1200W, and it is maximum that the intensity of boron reaches.
2) plasma gas flow rate increases to 18L/min from 11L/min, and line strength of boron does not have significant change;
3) the atomizer flow increases to 1.10L/min from 0.70L/min, and the intensity of boron also changes thereupon, and is interval at 0.80L/min～0.95L/min, and the response of boron is maximum;
4) the secondary air amount increases to 1.7L/min from 0.8L/min, and line strength of boron does not have significant change.
According to power, atomizer flow, secondary air amount, plasma gas flow rate experiment; It is test condition that this method is selected the related data that line strength is big, background is low; The result is: power 1200W, atomizer flow 0.85L/min, secondary air amount 1.2L/min, plasma gas flow rate 15L/min.
3, isotopic selection
The coordination of boron have 10B, 11B is in mensuration 11Therefore the stable and good linearity of B measured value is selected 11B is an analytical line.
4, the interference of iron-based body
In the standard solution of some parts of boron, add 0 respectively, the high purity iron mark liquid of 0.2g/mL, 0.4mg/mL, 0.6mg/mL, 0.8mg/mL, 1mg/mL, adopt the plasma mass spectrometer to measure, the result sees table 2.
Table 2: the iron-based body influence %
Figure BDA0000165805972
It is thus clear that the recovery of tested element is in 95～105% scopes, promptly the iron-based body below the 1mg/mL does not have remarkable interference to measuring element in the mensuration system,
5, dissolve appearance acid
The GB regulation, the boron of measuring gained with about 5mol/L sulfuric acid low-temperature decomposition under the situation that does not have oxidant to exist is that boron is dissolved in acid.This method adopts the sulfuric acid 20mL of (1+3), is heated to sample in the boiling water bath and dissolves fully.
6, the selection of sample weighting amount
Because the ICP-MS mass spectrometer should not use a large amount of sulfuric acid; Therefore adopting the increase sample weighting amount to be diluted to certain volume again measures; Make the residual quantity of sulfuric acid in the mensuration system very low; Do not influence the mass spectrometric normal use of ICP-MS, the content of boron is claimed 0.5000g less than 0.020% in this method regulation steel; The content of boron is claimed 0.1000g～0.2000g greater than 0.020% in the steel.Pipette test solution, the constant volume of certain volume, the ICP-MS mass spectrometer is measured.
7, coexistence elements interference experiment
In the presence of iron-based, the boron of different content is marked the interference measurement that liquid carries out Mn, V, Ni, Mo, Cr, Ti, Cu, RE, the result is following: Mn≤3.00%, Cr, Ni, V≤1.00%, Ti, Mo≤2.00%, Cu, RE≤0.2% is interference measurement not, sees table 3.
Table 3: coexistence elements influence %
Figure BDA0000165805973
But when facile hydrolysis elements such as containing niobium, tungsten in the solution exists, must do the filtration back and measure, be prone to stifled sampling system and measured value instability because of fine particle is arranged.
8, the detection limit of working curve, related coefficient, method
In 7 100mL volumetric flasks; Pipetting concentration respectively is boron standard solution 0,1.00,2.50,5.00,10.00,5.00mL (the boron standard solution of 1 μ g/mL), the 10.00mL (the boron standard solution of 1 μ g/mL) of 0.1 μ g/mL, adds the sulfuric acid 0.5mL of ρ 1.84g/mL, is diluted with water to scale and shakes up; With the beryllium is internal standard element; The employing icp ms is measured, the automatic drawing curve of instrument, and its related coefficient is more than 0.999.Measure by 11 parts of blank solutions of experimental technique preparation, basis of calculation deviation, 3 times standard deviation is the detection limit of measuring element, and 10 times detection limit is the detection lower limit.Be limited under the detection of the molten boron of acid: 0.0001%.
Result according to above-mentioned experiment obtains is applied to the molten boron Determination on content method of acid in the steel with the related parameter of confirming that has.The technical scheme that realizes this method is such, and (content of boron was claimed 0.1000g～0.2000g) greater than 0.020% o'clock in the steel to take by weighing sample 0.5000g; In the quartz beaker of 150mL, add the sulfuric acid of 20mL (1+3), make sample dissolution in the boiling water bath; Take off; Move in the volumetric flask of 100mL,, shake up with the water constant volume; Pipette 1mL～20mL solution in the volumetric flask of 100mL, constant volume in company with the band reagent blank, is an internal standard element with the beryllium, adopts icp ms to measure.
The drafting of working curve
In 7 100mL volumetric flasks; Pipetting concentration respectively is boron standard solution 0,1.00,2.50,5.00,10.00,5.00mL (the boron standard solution of 1 μ g/mL), the 10.00mL (the boron standard solution of 1 μ g/mL) of 0.1 μ g/mL; Adding the sulfuric acid 0.5mL of ρ 1.84g/mL, be diluted with water to scale and shake up, is internal standard element with the beryllium; The employing icp ms is measured, the automatic drawing curve of instrument.
Computing formula is: W ( M ) % = 10 - 9 × V × ( C - C 0 ) m × 100
W in the formula (M)-represent acid to dissolve the massfraction of boron, %;
The concentration numerical value of boron in C-sample solution, ng/mL;
C 0The concentration numerical value of boron in the-blank solution, ng/mL;
The numerical value of V-test solution volume, mL;
The quality numerical value of m-sample, g.
Outstanding advantage of the present invention is to have set up the molten boron Determination on content method of acid in a kind of steel, and this method is accurate, quick, pollution-free.
Four, embodiment:
Below in conjunction with embodiment the present invention is done further description.
Embodiment 1
Take by weighing 0.5000g GBW01327 low alloy steel, in the quartz beaker of 150mL, add the sulfuric acid of 20mL (1+3), make sample dissolution in the boiling water bath, take off, move in the volumetric flask of 100mL,, shake up with the water constant volume; Pipette 20mL solution in the volumetric flask of 100mL, constant volume in company with the band reagent blank, is an internal standard element with the beryllium, adopts icp ms to measure, and the result sees table 4.
The drafting of working curve
In 7 100mL volumetric flasks; Pipetting concentration respectively is boron standard solution 0,1.00,2.50,5.00,10.00,5.00mL (the boron standard solution of 1 μ g/mL), the 10.00mL (the boron standard solution of 1 μ g/mL) of 0.1 μ g/mL; Adding the sulfuric acid 0.5mL of ρ 1.84g/mL, be diluted with water to scale and shake up, is internal standard element with the beryllium; The employing icp ms is measured, the automatic drawing curve of instrument.
Computing formula is: W ( M ) % = 10 - 9 × V × ( C - C 0 ) m × 100
W in the formula (M)-represent acid to dissolve the massfraction of boron, %;
The concentration numerical value of boron in C-sample solution, ng/mL;
C 0The concentration numerical value of boron in the-blank solution, ng/mL;
The numerical value of V-test solution volume, mL;
The quality numerical value of m-sample, g.
Embodiment 2
Take by weighing 0.5000g GBW01325 low alloy steel, in the quartz beaker of 150mL, add the sulfuric acid of 20mL (1+3), make sample dissolution in the boiling water bath, take off, move in the volumetric flask of 100mL,, shake up with the water constant volume; Pipette 10mL solution in the volumetric flask of 100mL, constant volume in company with the band reagent blank, is an internal standard element with the beryllium, adopts icp ms to measure, and computing formula is with embodiment 1, and the result sees table 4.
The drafting of working curve
In 7 100mL volumetric flasks; Pipetting concentration respectively is boron standard solution 0,1.00,2.50,5.00,10.00,5.00mL (the boron standard solution of 1 μ g/mL), the 10.00mL (the boron standard solution of 1 μ g/mL) of 0.1 μ g/mL; Adding the sulfuric acid 0.5mL of ρ 1.84g/mL, be diluted with water to scale and shake up, is internal standard element with the beryllium; The employing icp ms is measured, the automatic drawing curve of instrument.
Embodiment 3
Take by weighing 0.5000g GBW01322 low alloy steel, in the quartz beaker of 150mL, add the sulfuric acid of 20mL (1+3), make sample dissolution in the boiling water bath, take off, move in the volumetric flask of 100mL,, shake up with the water constant volume; Pipette 5mL solution in the volumetric flask of 100mL, constant volume in company with the band reagent blank, is an internal standard element with the beryllium, adopts icp ms to measure, and computing formula is with embodiment 1, and the result sees table 4.
The drafting of working curve
In 7 100mL volumetric flasks; Pipetting concentration respectively is boron standard solution 0,1.00,2.50,5.00,10.00,5.00mL (the boron standard solution of 1 μ g/mL), the 10.00mL (the boron standard solution of 1 μ g/mL) of 0.1 μ g/mL; Adding the sulfuric acid 0.5mL of ρ 1.84g/mL, be diluted with water to scale and shake up, is internal standard element with the beryllium; The employing icp ms is measured, the automatic drawing curve of instrument.
Embodiment 4
Take by weighing 0.2000g GBW01312 low alloy steel, in the quartz beaker of 150mL, add the sulfuric acid of 20mL (1+3), make sample dissolution in the boiling water bath, take off, move in the volumetric flask of 100mL,, shake up with the water constant volume; Pipette 5mL solution in the volumetric flask of 100mL, constant volume in company with the band reagent blank, is an internal standard element with the beryllium, adopts icp ms to measure, and computing formula is with embodiment 1, and the result sees table 4.
The drafting of working curve
In 7 100mL volumetric flasks; Pipetting concentration respectively is boron standard solution 0,1.00,2.50,5.00,10.00,5.00mL (the boron standard solution of 1 μ g/mL), the 10.00mL (the boron standard solution of 1 μ g/mL) of 0.1 μ g/mL; Adding the sulfuric acid 0.5mL of ρ 1.84g/mL, be diluted with water to scale and shake up, is internal standard element with the beryllium; The employing icp ms is measured, the automatic drawing curve of instrument.
Table 4: measure % as a result
Figure BDA0000165805976

Claims (2)

1., boron Determination on content method is dissolved in acid in a kind of steel, it is characterized in that sample processes bits appearance, determination step is following:
1) (content of boron was claimed 0.1000g～0.2000g), in the quartz beaker of 150mL greater than 0.020% o'clock in the steel, to take by weighing sample 0.5000g; The sulfuric acid that adds 20mL (1+3) makes sample dissolution in the boiling water bath, take off; Move in the volumetric flask of 100mL,, shake up with the water constant volume; Pipette 1mL～20mL solution in the volumetric flask of 100mL, constant volume in company with the band reagent blank, is an internal standard element with the beryllium, adopts icp ms to measure;
2), the drafting of working curve
In 7 100mL volumetric flasks; Pipetting concentration respectively is boron standard solution 0,1.00,2.50,5.00,10.00,5.00mL (the boron standard solution of 1 μ g/mL), the 10.00mL (the boron standard solution of 1 μ g/mL) of 0.1 μ g/mL; Adding the sulfuric acid 0.5mL of ρ 1.84g/mL, be diluted with water to scale and shake up, is internal standard element with the beryllium; The employing icp ms is measured, the automatic drawing curve of instrument;
Computing formula is: W ( M ) % = 10 - 9 × V × ( C - C 0 ) m × 100
W in the formula (M)-represent acid to dissolve the massfraction of boron, %;
The concentration numerical value of boron in C-sample solution, ng/mL;
C 0The concentration numerical value of boron in the-blank solution, ng/mL;
The numerical value of V-test solution volume, mL;
The quality numerical value of m-sample, g.
2. boron Determination on content method is dissolved in acid in the steel according to claim 1, it is characterized in that the sulfuric acid of 20mL (1+3), makes sample dissolution in the boiling water bath, is diluted to certain volume, measures with icp ms.
CN2012101559767A 2012-05-18 2012-05-18 Method for measuring content of acid-solvable boron in steel Pending CN102661991A (en)

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CN103018222A (en) * 2012-12-14 2013-04-03 天津师范大学 Internal standard method for gas sampling non-dispersive atomic fluorescence detection of transitional and precious metal elements
CN103868978A (en) * 2014-02-24 2014-06-18 天津钢管集团股份有限公司 Method for determining acid-solvable boron in middle-low alloy steel by inductively coupled plasma source mass spectrometer
CN114166827A (en) * 2021-11-05 2022-03-11 本钢板材股份有限公司 Method for detecting boron in steel

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102928501A (en) * 2012-11-16 2013-02-13 内蒙古包钢钢联股份有限公司 Measuring method of solid-solution boron content in steel
CN103018222A (en) * 2012-12-14 2013-04-03 天津师范大学 Internal standard method for gas sampling non-dispersive atomic fluorescence detection of transitional and precious metal elements
CN103018222B (en) * 2012-12-14 2015-03-25 天津师范大学 Internal standard method for gas sampling non-dispersive atomic fluorescence detection of transitional and precious metal elements
CN103868978A (en) * 2014-02-24 2014-06-18 天津钢管集团股份有限公司 Method for determining acid-solvable boron in middle-low alloy steel by inductively coupled plasma source mass spectrometer
CN114166827A (en) * 2021-11-05 2022-03-11 本钢板材股份有限公司 Method for detecting boron in steel

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