CN109270051A - Use the method for Determination of Trace Boron in micro-wave digestion ICP-AES method analysis steel - Google Patents
Use the method for Determination of Trace Boron in micro-wave digestion ICP-AES method analysis steel Download PDFInfo
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Abstract
The present invention disclose it is a kind of analyze the method for Determination of Trace Boron in measurement steel using micro-wave digestion inductively coupled plasma emission spectrography and only use a small amount of hydrochloric acid, nitric acid, hydrofluoric acid and phosphoric acid, realize the complete decomposition of boron in steel, while the not loss of boron again.Entire Specimen eliminating process carries out in closed environment completely, easy to operate, small pollution of the environment.And by the way that a small amount of phosphoric acid is added in resolution acid, it is suppressed that the volatilization of boron increases the rate of recovery of boron, improves the precision and accuracy of analysis.
Description
Technical field
The invention belongs to iron and steel technical fields, are related to a kind of analysis method of iron and steel component, specifically trace in steel
Measure the measuring method of boron (mainly for mass fraction in 0.0002%-0.0005%).
Background technique
There is much the analysis method of Determination of Trace Boron in steel, there are three existing national standards analysis method is main: methanol distillation-ginger
Flavine photometry, abbreviation photometry (GB/T223.75-2008)；Spark discharge atomic emission spectrometry, abbreviation spark source-OES
Method (GB/T4336-2016)；Micro-wave digestion-inductively coupled plasma mass spectrometry, abbreviation ICP-MS method (GB/T 223.81-
2007).In these three methods, analyst coverage and analysis precision can satisfy the only GB/ of certain special steel grade technical requirements
T223.81-2007 can analyze boron mass fraction in 0.0002%-0.0005%, when boron mass fraction is 0.0002%
When, repeatability is 0.00009%, reproducibility 0.00025%.Although spark source-OES method can analyze 0.0001%-
0.0005% boron, but standard fails to provide its analysis precision within the scope of this contents level, the not only national standard in China
In this way, American Standard ASTM E415-17 and day mark JIS G 1253:2002 are also in this way, this uses limitation with spark source-OES method
It is related.Photometry can only analyze boron of the mass fraction 0.0005% or more.
Inductively coupled plasma atomic emission spectrometry, abbreviation ICP-AES method, China does not formulate relevant country at present
Standard method of analysis, there is boron quantitative approach-trimethylborate distillation and separation method in Japanese Industrial Standards, and standard No. is JIS G
1258-7:2007 uses ICP-AES analysis method, can be with mass fraction in quantitative analysis steel in 0.0001%-
Boron in 0.010% range, although method high sensitivity, whole process needs to carry out distillation separation using silica ware,
Operating process is complicated, and analysis process is long.
Summary of the invention
The object of the invention is that the shortcomings that overcoming the prior art, proposes that a kind of analysis measures the side of Determination of Trace Boron in steel
Method, this method be using in ICP-AES method measurement steel in Determination of Trace Boron, especially steel mass fraction in 0.0002%-
Boron in 0.0005% range, accuracy of analysis and precision reach the requirement of GB/T 223.81-2007, without using detection limit
Low but expensive ICP-MS instrument, without by complicated distillation separating step.This analysis method has analysis speed
Fastly, operating method is simple, and analysis detection limit is low, accuracy of analysis and the good advantage of precision.
The specific technical solution of the present invention is as follows:
A method of Determination of Trace Boron in measurement steel being analyzed using micro-wave digestion inductively coupled plasma emission spectrography,
It is characterized in that including the following steps:
(1) sample dissolves:
By hydrochloric acid, nitric acid and water, 1:1:2 is configured to mixed acid solution by volume, and 10ml mixing is added by every 0.5g sample
Sample to be tested, mixed acid solution, hydrofluoric acid, phosphoric acid are placed in closed by the ratio of acid solution, 0.5ml hydrofluoric acid, 1ml phosphoric acid
It is cleared up in microwave dissolver, selects Ramp to Temperature control model, temperature-rise period slowly carries out, point three steps,
The first step rises to 70 DEG C in 5 minutes, keeps the temperature 10 minutes, and second step rises to 100 DEG C in 5 minutes, keeps the temperature 10 minutes, third step
120 DEG C are risen in 5 minutes, keep the temperature 15 minutes；
(2) ICP is measured:
ICP-AES spectrometer selects 182.641nm as boron analytical line；
It is as follows that parameter is arranged in ICP-AES spectrometer plasma:
RF power: 1150-1350w；
Nebulizer gas flow: 0.5-0.6L/min；
Vertical Observation height: 10-12mm.
Preferably, ICP-AES spectrometer plasma setting parameter is as follows:
RF power: 1150w；
Nebulizer gas flow: 0.6L/min；
Vertical Observation height: 12mm.
The method that the present invention analyzes Determination of Trace Boron in steel using inductive coupling plasma emission spectrograph, this method are applied to
In iron and steel enterprise, make the analysis of Determination of Trace Boron in steel (mass fraction be lower than 0.0005%) realize it is quick, accurate, economical and
The feature of environmental protection is good, solves the problems, such as to measure Determination of Trace Boron in steel using ICP-AES method.
Firstly, this method uses microwave digestion technology, only with a small amount of hydrochloric acid, nitric acid, hydrofluoric acid and phosphoric acid (every 0.5g sample
Product correspond to total acid content about 6.5ml), the complete decomposition of boron in steel is realized, while the not loss of boron again.Entire Specimen eliminating mistake
Journey carries out in closed environment completely, easy to operate, small pollution of the environment.And heating for dissolving, the need of traditional open type
Acid amount to be used is at least 30ml, and to be smoldered and could decompose completely the boron in sample by sulfuric acid, smolder the time and
Temperature also wants strict control, and operating condition is harsh, is not easy to grasp, cause serious pollution to the environment.By being added on a small quantity in resolution acid
Phosphoric acid, it is suppressed that the volatilization of boron increases the rate of recovery of boron, improves the precision and accuracy of analysis.
Entire analytic process is not necessarily to complicated lock out operation, avoids using the higher a whole set of quartz still ware of price and big
Toxic methanol reagent is measured, analysis cost and the pollution to environment are reduced, reduces the Health cost to operator.
Furthermore this method uses the common inductively coupled plasma atomic emission spectrometer of iron and steel enterprise to survey as analysis
Amount equipment is realized to trace Boron nitrogen rings in steel, and analysis precision has reached the requirement of GB/T 223.81-2007, is without the use of
Expensive icp ms, reduce analysis cost, and analysis precision can satisfy production requirement.
Detailed description of the invention
Fig. 1 is trace B 182.641nm analytical line spectrogram in steel.
Fig. 2 is trace B analytic set curve in steel.
Specific embodiment
The method that the present invention measures Determination of Trace Boron in steel can be dissolved from sample and the ICP-AES method of sample measures in terms of two
To illustrate:
The dissolution of 1.1 samples
Boron mainly exists in steel with solid solution, moreover it is possible to form the borides such as boron nitride, boron oxide and iron carbon boron.Various shapes
The boron of state is extremely different to the stability of acid, this keeps the decomposition of boron-containing steel and measurement relatively difficult.Usually solid solution boron, boron oxide compound,
Iron carbon-boron compound can be decomposed by diluted acid, this part of boron is referred to as " acid molten boron " in analysis, but due to using acid type,
The difference of concentration and heating method often makes the analysis result of the molten boron of acid different.Boron nitride has the stability of height, cannot be by
This part of boron is known as " the insoluble boron of acid " in analysis by general diluted acid dissolution, and the decomposition of the insoluble boron of acid generally uses sodium carbonate
Fusion method.Containing elements such as niobium, tantalum, titanium, aluminium in general high-alloy steel, nickel base superalloy, boron is much larger than to the affinity of nitrogen, because
This seldom forms boron nitride, and full boron amount can be obtained after sulfuric acid is smoldered.And full boron amount can be obtained sometimes to carbon steel, middle-low alloy steel,
Sometimes between sour molten boron and full boron.
This method use microwave digestion technology, using mixing diluted acid sample dissolution, by adjusting mixing diluted acid type and
Proportion, and micro-wave digestion program is worked out, it finds out suitable mixed acid, concentration, with program is when cleared up, makes in steel sample
Boron can all dissolve and volatilization loss of the boron in digestion process.
1.1.1 the determination of dissolving acid.
Here mixing diluted acid is hydrochloric acid, nitric acid and water, volume ratio 1: 1: 2, the mixing diluted acid that every 0.5g sample is added
Amount is 10ml, to enable boron all to dissolve, 0.5ml hydrofluoric acid is added, fluorine ion and boron are complexed to form [BF4]-, boron is dissolved,
The phosphoric acid of 1ml is added to inhibit the volatilization loss of boron simultaneously
Use dilute hydrochloric acid nitric acid (HCl+HNO3+H2O=1+1+2) advantage is for clearing up middle-low alloy steel speed fastly and disappearing
Solution effect is good, and nitric acid content is excessively high, and oxidation rate is slow, and content of hydrochloric acid is excessively high, is unfavorable for the destruction of carbide, and this diluted acid matches
It is faster than concentrated acid reaction speed to clear up steel sample；Hydrofluoric acid addition is to form fluorine boron complex ion with boron using it, to promote the molten of boron
Solution, considers that the factor of reagent blank, hydrofluoric acid additional amount should not be added clear up sample boron completely；Consider simultaneously
To under the conditions of dilute acidic, fluorine boron complex ion is unstable, and temperature is more than 130 DEG C and easily resolves into boric acid, and boric acid is easily with vapor
Volatilization, causes the volatilization loss of boron；The difficult stable comple to volatilize can be generated since phosphoric acid is reacted with boron, phosphoric acid is added
It prevents boron from volatilizing, but since phosphoric acid toughness itself is strong, is not easy to be atomized, excessive addition can be such that nebulization efficiency reduces, experiment hair
The amount of existing 1.0ml is suitable.Comprehensively consider, present invention determine that mixed acid proportion, reagent blank is low, and nebulization efficiency is high, molten
Determination of Trace Boron speed is fast and thorough in Xie Gang, and volatilization loss is few, and the boron rate of recovery is high, and this law analysis is made to have high sensitivity.
1.1.2 the establishment of micro-wave digestion program.
Entire digestion process is carried out in closed digestion tank, is selected Ramp to Temperature (linear temperature increase)
Control model, temperature-rise period preferably slowly carry out, and point three steps, the first step rises to 70 DEG C in 5 minutes, keep the temperature 10 minutes, second step
100 DEG C are risen in 5 minutes, keeps the temperature 10 minutes, and third step rises to 120 DEG C in 5 minutes, keeps the temperature 15 minutes.
Substep heating is advantageous in that avoid reaction carries out excessively fierce in a short time, while can make entirely to disappear again
Solution reaction carries out sufficiently, and is conducive to control temperature in reactor tank within 130 DEG C, to prevent the volatilization loss of boron.
1.2ICP measurement
1.2.1 selection analysis line
The analytical line of boron there are commonly 182.591nm, 182.641nm, 208.959nm, 249.678n-m, 249.773nm,
Every analytical line superiority and inferiority is analyzed as follows:
249.773nm is most sensitive analysis line, but has the strong jamming peak of iron, the resolution ratio of instrument at 249.782nm
It is not enough to separate this two lines, is separated boron using complicated separation means, it can be with quantitative analysis boron to 0.0001%.
249.678nm is also more sensitive analytical line, but has the strong jamming peak of iron at 249.653nm, in 249.697nm
There are the Interference Peaks of niobium at place again, although the resolution ratio of instrument can separate the analytical line of boron and the analytical line of iron and niobium, by
Yu Tie, niobium analytical line be distributed across the analytical line two sides of boron, be superimposed upon in background, cause background correction difficult.If not carrying on the back
Scape correction, when doing calibration curve using series standard sample and use this calibrating curve measuring sample, when sample and standard sample
Or it will affect the precision and accuracy of analysis when difference occurs in matrix between standard specimen itself.
It is also higher that 208.959nm analyzes line sensitivity, but has the strong jamming peak of molybdenum, instrument at 208.952nm to the left
Device cannot separate the two.
This two analysis line sensitivities of 182.591nm and 182.641nm are not as good as above-mentioned analytical line (when being free of matrix), still
Other than having the interference of sulphur at 182.624nm, without other interference elements, instrumental resolution can by the interfering line of sulphur with
The analytical line of this two boron separates.In view of 182.641nm analytical line peak back ratio is more excellent, sensitivity is higher, therefore selects
182.641nm as boron analytical line.
1.2.2 parameter is arranged in instrument plasma
In ICP emission spectrographic analysis, the factor for influencing the intensity of spectral line mainly has output high frequency power, gas flow and light
Compose observed altitude.Wherein gas flow includes cooling air (plasma gas) flow, secondary air amount and carrier gas (atomizer gas again
Body) flow, wherein atomization gas flow effect is maximum.
The present invention mainly has studied output high frequency power (RF power), atomization gas flow and Vertical Observation height and exists to boron
182.641nm locating the influence of the intensity of spectral line.By change RF power (from 950w to 1350w), change atomization gas flow (from
0.50L/min to 0.70L/min) and change Vertical Observation height (from 8mm to 14mm), observe the intensity of spectral line and background intensity
Variation.
Experiment discovery, is more difficult excitation, that is, so-called hard spectrum due to atomic spectral line of the boron at 182.641nm
Line, therefore increase output high frequency power (RF power), reduce atomization gas flow and reduce Vertical Observation height, be conducive to increase spectrum
Line intensity.The present invention selects following parameter that parameter is arranged as plasma.
RF power: 1150-1350w
Nebulizer gas flow: 0.5-0.6L/min
Vertical Observation height: 10-12mm
Wherein for Vertical Observation height at 10mm, the intensity of spectral line is most strong, but background intensity also increases simultaneously.Comprehensively consider spectrum
Parameter is arranged as plasma in the signal-to-background ratio and stability of line, preferably following parameter:
RF power: 1150w
Secondary air amount: 0.5L/min
Nebulizer gas flow: 0.6L/min
Vertical Observation height: 12mm.
Embodiment one
1.1 test portion
1.1.1 instrument and reagent
Microwave digestion system: the closed microwave digestion system of MARS of CEM company production；
Full spectrum direct-reading ICP-AES spectrometer: the iCAP 6300 of U.S.'s thermoelectricity production；Hydrofluoric acid resistant solution atomization sample introduction system
System；
Dilute hydrochloric acid-nitric acid mixed acid: hydrochloric acid, nitric acid are all made of excellent pure grade, hydrochloric acid+nitric acid+water=1+1+2；
Phosphoric acid: excellent pure grade；
Hydrofluoric acid: excellent pure grade；
Boron standard solution: 100 μ g/ml are prepared using boric acid, used time dilution；
The not steel standard sample of boracic: known boron mass percent is below 0.00005%；
Steel standard sample containing Determination of Trace Boron.
1.1.2 the operating condition of instrument
1 iCAP-6300 spectrometer operating condition of table
1.1.3 experimental method
0.5000g sample is weighed, is placed in polytetrafluoroethylene (PTFE) high-pressure digestion tank, 10mL dilute hydrochloric acid-nitric acid mixed acid is added,
After reacting calmness, 0.5ml hydrofluoric acid and 1ml phosphoric acid are sequentially added, is closed the lid, is packed into according to the operating procedure of instrument micro-
Wave is cleared up in instrument, carries out micro-wave digestion according to the program that table 2 is set.After cooling, constant volume is in 100mL polyethylene volume bottle.?
In ICP-AES spectrometer, measured according to the operating condition of table 1.
1.1.4 working curve
6 parts of steel standard sample of not boracic are weighed, is placed in polytetrafluoroethylene (PTFE) high-pressure digestion tank, it is molten to sequentially add boron standard
Liquid (2.5 μ g/ml) 0ml, 0.50ml, 1.00ml, 1.50ml, 2.50ml, 4.00ml, corresponding boron mass fraction 0.00000%,
0.00025%, 0.00050%, 0.00075%, 0.00125%, 0.00200%.According to experimental method, resolution acid is added and carries out
After micro-wave digestion, constant volume, working curve is established in ICP-AES spectrometer, as shown in Figure 1, 2, to measure respective sample
Full boron mass fraction (different colours spectral line corresponds to different samples in Fig. 1).
1.2 results and discussion
1.2.1 the selection of micro-wave digestion condition
Need to select suitable condition when carrying out Specimen eliminating using microwave digestion system, micro-wave digestion condition include power,
Temperature, time select best micro-wave digestion condition, are shown in Table 2 according to the requirement of microwave digestion system specification.
2 micro-wave digestion operating condition of table
| Stage | Maximum power (w) | Heating-up time (minute) | Target temperature (DEG C) | Retention time (minute) after reaching temperature |
| 1 | 400 | 5 | 70 | 10 |
| 2 | 640 | 5 | 100 | 10 |
| 3 | 800 | 5 | 120 | 15 |
1.2.2 digestive reagent selects
Under the conditions of selected resolution, resolution test is carried out using different inorganic acid combinations, measures the content of boron in steel,
It the results are shown in Table 3.
3 digestive reagent Selection experiment result (%) of table
Seen from table 3, add a small amount of hydrofluoric acid and phosphoric acid using dilute hydrochloric acid nitric acid mixed acid, the resolution of boron is complete and lossless
It loses.Actually use dilute hydrochloric acid nitric acid mixed acid (hydrochloric acid+nitric acid+water=1+1+2) 10ml, hydrofluoric acid 0.5ml and phosphatase 11 ml conduct
Digestive reagent.
1.2.3 the detection limit and quantitative limit of method
It according to Such analysis condition, measures sample blank 10 times, obtaining standard deviation S is 0.00002%, 3 times of standard
Deviation is the detection limit of method, is determined as 0.00006%.10 times of standard deviation is the quantitative limit of method, is determined as
0.0002%.
1.2.4 the preci-sion and accuracy of method
It is repeatedly measured in different time using trace boron steel standard specimen of this method to different content, the knot obtained
Fruit, precision and accuracy are shown in Table 4, wherein critical difference CD0.95For the permission between the average value and standard value of 7 measurement results
Difference, mark be 1. according in GB/T223.81-2007 repeatability limit and reproducibility limit be calculated, marking 2. is basis
Repeatability limit and reproducibility limit in GB/T223.75-2008 are calculated；Allow it is critical it is very poor be according to repeatability limit multiplied by
1.5 times are calculated, 7 duplicate measurements it is very poor should be less than be equal to allow it is critical very poor, mark be 1. according to GB/T223.81-
Repeatability limit in 2007 is calculated, and marking 2. is calculated according to the repeatability limit in GB/T223.75-2008.
Table 4 analyzes result, precision and accuracy
By table 4 as it can be seen that boron content is within the scope of 0.0002%-0.0005%, this law analysis precision and accuracy meet GB/
T 223.81-2007 requirement, within the scope of 0.0005%-0.0020%, this law analysis precision and accuracy can expire boron content
Sufficient GB/T 223.81-2007 and GB/T 223.75-2008 requirement.
1.3 brief summary
Test result shows using closed microwave digestion system, and hydrochloric acid, nitric acid, hydrofluoric acid is used to add phosphoric acid as disappearing
Reagent is solved, by the way that best instrument parameter is arranged, may be implemented to exist to content to trace Boron nitrogen rings in steel using ICP-AES method
0.0004% boron, for relative standard deviation 8% or so, the precision of analysis and accuracy reach national standard.
This method is suitable for boron mass fraction and measures in the full boron of 0.0002% or more steel, can satisfy production and scientific research
It is required that.
Claims (5)
1. a kind of method for analyzing Determination of Trace Boron in measurement steel using micro-wave digestion inductively coupled plasma emission spectrography, special
Sign is to include the following steps:
(1) sample dissolves:
By hydrochloric acid, nitric acid and water, 1:1:2 is configured to mixed acid solution by volume, and it is molten that 10ml mixed acid is added by every 0.5g sample
Sample to be tested, mixed acid solution, hydrofluoric acid, phosphoric acid are placed in closed type micro-wave by the ratio of liquid, 0.5ml hydrofluoric acid, 1ml phosphoric acid
It is cleared up in resolution instrument, selects Ramp to Temperature control model, temperature-rise period slowly carries out, point three steps, and first
Step rises to 70 DEG C in 5 minutes, keeps the temperature 10 minutes, and second step rises to 100 DEG C in 5 minutes, keeps the temperature 10 minutes, third step is 5
120 DEG C are risen in minute, keep the temperature 15 minutes；
(2) ICP is measured:
ICP-AES spectrometer selects 182.641nm as boron analytical line；
It is as follows that parameter is arranged in ICP-AES spectrometer plasma:
RF power: 1150-1350w；
Nebulizer gas flow: 0.5-0.6 L/min；
Vertical Observation height: 10-12mm.
2. the method for Determination of Trace Boron in analysis measurement steel as described in claim 1, it is characterised in that ICP-AES spectrometer plasma
It is as follows that parameter is arranged in body:
RF power: 1150w；
Nebulizer gas flow: 0.6L/min；
Vertical Observation height: 12mm.
3. the method for Determination of Trace Boron in analysis measurement steel as described in claim 1, it is characterised in that micro- in the temperature-rise period first step
Wave digestion system maximum power is set as 400W；In second step, microwave digestion system maximum power is set as 640W；Third step
In, microwave digestion system maximum power is set as 800W.
4. the method for Determination of Trace Boron in analysis measurement steel as described in claim 1, it is characterised in that ICP-AES spectrometer is arranged such as
Lower parameter: nebulizer pressure 0.13Mpa, secondary air amount 0.5L/min, pump speed 50/rpm, long wave integrate 5s, shortwave integral
15s。
5. the method for Determination of Trace Boron in analysis measurement steel as described in claim 1, it is characterised in that by hydrochloric acid, nitric acid, water press than
Sample is put into mixed liquor, after reacting calmness, sequentially adds the hydrofluoric acid of corresponding proportion, phosphoric acid is configured to mix by example with postponing
Close acid solution.
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| CN114778240A (en) * | 2022-04-12 | 2022-07-22 | 宁波江丰电子材料股份有限公司 | Dissolving method of TaAl alloy |
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