CN110514645A - The method of impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES - Google Patents
The method of impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract
The method that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES, is related to constituent content field of measuring technique in silicon bronze.The invention aims to solve the problem of that ICP-AES instrument is lower for shortwave Element sensitivity in the prior art can not accurately calculate impurity element As, Sb content in silicon bronze.Method: ultraviolet purging is carried out to light room, the standard specimen respectively containing As, Sb is exposed；In light room, after adjustment parameter, draws the standard curve of various concentration and select one group of optimal standard curve, by the parameter setting of the standard curve into inductively-coupled plasma spectrometer；Sample introduction needle is inserted into prepare liquid, prepare liquid is measured with ICP-AES, is calculated according to measurement result, obtains the content of impurity element As, Sb in silicon bronze.The present invention can get the method that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES.
Description
Technical field
The present invention relates to constituent content field of measuring technique in silicon bronze, and in particular to miscellaneous in the accurate measurement silicon bronze of one kind
The method of prime element As, Sb content.
Background technique
Main raw material(s) of the silicon bronze as bearing retainer plays a very important role during Production of bearing.
The performance of material itself is such as organized, hardness, is occurred with the variation with environment is easy under the variation of applying working condition
Change, but for material at be grouped as be will not be changed with variation such as temperature of environment etc..Component content
Whether it is strict controlled in acceptability limit, whether Element detection result is accurate, can directly trace legal liabilities.Therefore raw material member
The accurate measurement of element, the factory for finished product is very necessary.
For impurity element As, Sb in retainer material silicon bronze, both elements are shortwave element, and content is special
It is not low, provide that chemical component, the content of the two elements are≤0.002 according to the standard in ZZT03-YS-046.Because of content
Too low, general detecting instrument detection limit is too high, is unable to satisfy the accurate measurement of trace element, therefore using ICP-AES to two
A element measures, but ICP-AES lower for the sensitivity of shortwave element, and especially content is especially few, more difficult
Identify the presence of both elements, qualitative limitation more can not accurately calculate content.Therefore right during detection
The parameter of ICP-AES instrument is strictly adjusted.
Summary of the invention
It is lower for shortwave Element sensitivity the invention aims to solve ICP-AES instrument in the prior art, it can not
The problem of accurately calculating impurity element As, Sb content in silicon bronze, and provide and accurately measure impurity in silicon bronze with ICP-AES
The method of elements A s, Sb content.
The method that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES is completed according to the following steps:
One, light room is handled: using elder generation high frequency 30min~60min, again by the way of low frequency 60min~120min, to light room into
The ultraviolet purging of row；
Two, it exposes: the standard specimen containing As and the standard specimen containing Sb is exposed；
Three, parameter setting: in light room, to inductively-coupled plasma spectrometer progress parameter setting: incident power is
1.0kW~1.2kW, cooling gas flow are 18L/min~20L/min, and secondary air amount is 0.3L/min~0.4L/min, atomization
Throughput is 32L/min~34L/min, and peristaltic pump is 1.3mL/min~1.4mL/min, and Vertical Observation mode is observed；
Four, standard curve is chosen:
1., in the concentration of As be the As solution that various concentration is configured within the scope of 0.08mg/L~2.40mg/L, different dense
5 kinds or 5 kinds or more are chosen according to increasing concen-trations form in the As solution of degree and is used as 1 group of As standard curve sample, choose at least 4 groups
As standard curve sample is tested every group of As standard curve sample respectively, is tested according to the parameter that step 3 is set
Curve is evenly distributed situation one group of optimal test curve of selection as As standard song according to absorption peak in all test curves
Line, and by the parameter setting of the As standard curve into inductively-coupled plasma spectrometer；
2., in the concentration of Sb be the Sb solution that various concentration is configured within the scope of 0.08mg/L~2.40mg/L, different dense
5 kinds or 5 kinds or more are chosen according to increasing concen-trations form in the Sb solution of degree and is used as 1 group of Sb standard curve sample, choose at least 4 groups
Sb directrix curve sample is marked, according to the parameter that step 3 is set, every group of Sb standard curve sample is tested respectively, is tested
Curve is evenly distributed situation one group of optimal test curve of selection as Sb standard song according to absorption peak in all test curves
Line, and by the parameter setting of the Sb standard curve into inductively-coupled plasma spectrometer；
Five, measure content: sample introduction needle is inserted into prepare liquid, with inductively-coupled plasma spectrometer to prepare liquid into
Row measurement, is calculated according to measurement result, obtains the content of impurity element As, Sb in silicon bronze.
Beneficial effects of the present invention:
The method that the present invention accurately measures impurity element As, Sb content in silicon bronze with ICP-AES, by improving silicon bronze
Sampler-dissolving method, optimization instrument parameter, improve sensitivity of the instrument to both elements, therefore being capable of Accurate Determining bearing retainer
The constituent content of material silicon bronze impurity element As, Sb.The detection method is respectively as follows: the detection limit of two elements the detection of As
The detection for being limited to 0.0088, Sb is limited to 0.0119；The minimum constituent content of corresponding A s is that the minimum constituent content of 0.000051%, Sb is
0.00007%, it is seen that effectively increase sensitivity.The rate of recovery for the As element of determinand is 104.75%~124.95%
Between；Sb is between 92.8%~122%, and the rate of recovery is higher, be can be applied in production detection.
The present invention can get the method that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES.
Detailed description of the invention
When Fig. 1 is that the time for exposure is 20s in embodiment one, the bright degree image of hot spot is shown under As, Sb wavelength calibration；
When Fig. 2 is that the time for exposure is 30s in embodiment one, the bright degree image of hot spot is shown under As, Sb wavelength calibration；
When Fig. 3 is that the time for exposure is 40s in embodiment one, the bright degree image of hot spot is shown under As, Sb wavelength calibration；
When Fig. 4 is that the time for exposure is 50s in embodiment one, the bright degree image of hot spot is shown under As, Sb wavelength calibration；
When Fig. 5 is that the time for exposure is 60s in embodiment one, the bright degree image of hot spot is shown under As, Sb wavelength calibration；
When Fig. 6 is that the time for exposure is 80s in embodiment one, the bright degree image of hot spot is shown under As, Sb wavelength calibration；
When Fig. 7 is that the time for exposure is 120s in embodiment one, the bright degree image of hot spot is aobvious under As, Sb wavelength calibration
Show；
Fig. 8 is the linear rule figure of group 1. elements A s in one comparative experiments of embodiment；
Fig. 9 is the linear rule figure of group 2. elements A s in one comparative experiments of embodiment；
Figure 10 is the linear rule figure of group 3. elements A s in one comparative experiments of embodiment；
Figure 11 is the linear rule figure of group 4. elements A s in one comparative experiments of embodiment；
Figure 12 is the linear rule figure of group 1. element sb in one comparative experiments of embodiment；
Figure 13 is the linear rule figure of group 2. element sb in one comparative experiments of embodiment；
Figure 14 is the linear rule figure of group 3. element sb in one comparative experiments of embodiment；
Figure 15 is the linear rule figure of group 4. element sb in one comparative experiments of embodiment；
Figure 16 is the canonical plotting for optimizing the elements A s under technique in embodiment one；
Figure 17 is the canonical plotting for optimizing the element sb under technique in embodiment one.
Specific embodiment
Specific embodiment 1: present embodiment accurately measures impurity element As, Sb content in silicon bronze with ICP-AES
Method is completed according to the following steps:
One, light room is handled: using elder generation high frequency 30min~60min, again by the way of low frequency 60min~120min, to light room into
The ultraviolet purging of row；
Two, it exposes: the standard specimen containing As and the standard specimen containing Sb is exposed；
Three, parameter setting: in light room, to inductively-coupled plasma spectrometer progress parameter setting: incident power is
1.0kW~1.2kW, cooling gas flow are 18L/min~20L/min, and secondary air amount is 0.3L/min~0.4L/min, atomization
Throughput is 32L/min~34L/min, and peristaltic pump is 1.3mL/min~1.4mL/min, and Vertical Observation mode is observed；
Four, standard curve is chosen:
1., in the concentration of As be the As solution that various concentration is configured within the scope of 0.08mg/L~2.40mg/L, different dense
5 kinds or 5 kinds or more are chosen according to increasing concen-trations form in the As solution of degree and is used as 1 group of As standard curve sample, choose at least 4 groups
As standard curve sample is tested every group of As standard curve sample respectively, is tested according to the parameter that step 3 is set
Curve is evenly distributed situation one group of optimal test curve of selection as As standard song according to absorption peak in all test curves
Line, and by the parameter setting of the As standard curve into inductively-coupled plasma spectrometer；
2., in the concentration of Sb be the Sb solution that various concentration is configured within the scope of 0.08mg/L~2.40mg/L, different dense
5 kinds or 5 kinds or more are chosen according to increasing concen-trations form in the Sb solution of degree and is used as 1 group of Sb standard curve sample, choose at least 4 groups
Sb directrix curve sample is marked, according to the parameter that step 3 is set, every group of Sb standard curve sample is tested respectively, is tested
Curve is evenly distributed situation one group of optimal test curve of selection as Sb standard song according to absorption peak in all test curves
Line, and by the parameter setting of the Sb standard curve into inductively-coupled plasma spectrometer；
Five, measure content: sample introduction needle is inserted into prepare liquid, with inductively-coupled plasma spectrometer to prepare liquid into
Row measurement, is calculated according to measurement result, obtains the content of impurity element As, Sb in silicon bronze.
Specific embodiment 2: the differences between this implementation mode and the specific implementation mode are that: using first in the step 1
The mode of high frequency 30min, again low frequency 60min carry out ultraviolet purging to light room.
Other steps are same as the specific embodiment one.
Specific embodiment 3: present embodiment is with specific embodiment one or two differences: will in the step 2
Standard specimen containing As and the standard specimen containing Sb carry out the exposure of 80s~120s.
Other steps are the same as one or two specific embodiments.
Specific embodiment 4: one of present embodiment and specific embodiment one to three difference are: the step 2
The middle exposure that the standard specimen containing As and the standard specimen containing Sb are carried out to 80s.
Other steps are identical as specific embodiment one to three.
Specific embodiment 5: one of present embodiment and specific embodiment one to four difference are: institute in step 5
The prepare liquid stated is prepared according to the following steps:
Nitric acid/hydrochloric acid mixed solution is added into conical flask, silicon bronze sample is placed in nitric acid/hydrochloric acid mixed solution,
It is then heated to 20 DEG C~40 DEG C, and insulated and stirred 30min~50min at 20 DEG C~40 DEG C, then molten to nitric acid/mixed in hydrochloric acid
Nitric acid solution to solution is added dropwise in liquid to clarify, is finally cooled to room temperature, is settled to 50mL with hydrochloric acid solution, shake up standing, obtain
Prepare liquid, the quality of the silicon bronze sample and the ratio of nitric acid/hydrochloric acid mixed solution volume are (0.85g~1g): (20mL~
30mL), nitric acid solution and the volume ratio of hydrochloric acid solution are 1:4 in the nitric acid/hydrochloric acid mixed solution, in the nitric acid solution
HNO3Mass fraction be 66%~68%, the mass fraction of HCL is 36%~38% in the hydrochloric acid solution.
Other steps are identical as specific embodiment one to four.
Specific embodiment 6: one of present embodiment and specific embodiment one to five difference are: the step 4
The middle content with impurity element As, Sb in ICP-AES measurement silicon bronze, is observed using Vertical Observation mode.
Other steps are identical as specific embodiment one to five.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one: the method that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES, according to the following steps
It completes:
One, light room is handled: being optimized by many experiments, finally by the way of high frequency 30min, low frequency 60min, to light room
Carry out ultraviolet purging；
Two, it weighs 0.1gCu to fuse into 25mL hydrochloric acid solution, the As standard liquid constant volume of certain volume is then added to 250mL's
It in volumetric flask, then weighs 0.1gCu and fuses into 25mL hydrochloric acid solution, the Sb standard liquid constant volume of certain volume is added to the capacity of 250mL
In bottle, two standard specimens containing As, Sb respectively are obtained；
Exposure: the length of time for exposure equally restricts the accurate measurement of As, Sb element, and the time for exposure affects element
It is special should be able to grade point position identification, the sensitivity of Element detection is affected, because shortwave element is anti-in corresponding energy level point
It answers sensitivity relatively low, therefore is exposed the parameter optimization of time to As, Sb sample, respectively by the standard specimen containing As, Sb
Successively carry out the exposure of 20s, 30s, 40s, 50s, 60s, 80s and 120s；
As shown in Fig. 1~7, for the standard specimen containing As, Sb is successively carried out 20s, 30s, 40s, 50s, 60s, 80s and 120s
Exposure, the bright degree image of the hot spot under the wavelength calibration of As, Sb after exposure shows；Pass through the wave of different exposure time
It can be seen that after time for exposure 80s in long calibration figure, hot spot brightness is significantly improved, it is seen that the time for exposure of 80s can have
Effect identifies corresponding element and without the interference of other elements hot spot, can effectively identify corresponding element, and can be accurate right
The brightness size of element is answered effectively to carry out quantitative analysis to element.
Three, preparation process:
(1) equivalent Cu is dissolved, constant volume is used as blank solution in the volumetric flask of 250mL；
(2) nitric acid/hydrochloric acid mixed solution is added into conical flask, 0.85g silicon bronze sample is placed in 20mL nitric acid/hydrochloric acid
In mixed solution, it is then heated to 35 DEG C, and the insulated and stirred 30min at 35 DEG C, then be added dropwise into nitric acid/hydrochloric acid mixed solution
Nitric acid solution to solution is clarified, and is finally cooled to room temperature, is settled to 50mL with hydrochloric acid solution, shake up standing, obtains prepare liquid, institute
Stating nitric acid solution and the volume ratio of hydrochloric acid solution in nitric acid/hydrochloric acid mixed solution is 1:4, HNO in the nitric acid solution3Quality
Score is 66%~68%, and the mass fraction of HCL is 36%~38% in the hydrochloric acid solution；
Four, parameter setting: in light room, parameter setting is carried out to inductively-coupled plasma spectrometer: adjusting plasma
Body parameter, incident power 1.2kW, cooling gas flow 20L/min, secondary air amount 0.4L/min, atomization gas flow are
34L/min, peristaltic pump 1.4mL/min are observed using Vertical Observation mode；
Four, standard curve is chosen:
1., in the concentration of As be the As solution that various concentration is configured within the scope of 0.08mg/L~2.40mg/L, different dense
5 kinds are chosen according to increasing concen-trations form in the As solution of degree and is used as 1 group of As standard curve sample, choose 4 groups of As standard curve examinations
Sample tests every group of As standard curve sample respectively, obtains test curve according to the parameter that step 4 is set, all
One group of optimal test curve is chosen as As standard curve according to the absorption peak situation that is evenly distributed in test curve, and by the As
The parameter setting of standard curve is into inductively-coupled plasma spectrometer；
2., in the concentration of Sb be the Sb solution that various concentration is configured within the scope of 0.08mg/L~2.40mg/L, different dense
5 kinds are chosen according to increasing concen-trations form in the Sb solution of degree and is used as 1 group of Sb standard curve sample, choose 4 groups of mark Sb directrix curve examinations
Sample tests every group of Sb standard curve sample respectively, obtains test curve according to the parameter that step 4 is set, all
One group of optimal test curve is chosen as Sb standard curve according to the absorption peak situation that is evenly distributed in test curve, and by the Sb
The parameter setting of standard curve is into inductively-coupled plasma spectrometer；
The selection of standard curve concentration gradient:
Impurity content is lower in silicon bronze, it is desirable to effectively drafting standard curve, and concentration gradient is effectively ensured
Linear rule meets bright rich Beer law, and guarantees that the surveyed concentration of sample just falls in standard curve center, mentions as far as possible
The accuracy of high sample detection, it is therefore desirable to the standard curve for meeting both element linear rules of As, Sb with experimental verification, because
This has done comparative experiments as shown in table 3 below respectively, and obtained linear rule figure is as shown in Fig. 8~15:
Table 3
| Group | S0 | S1(mg/L) | S2(mg/L) | S3(mg/L) | S4(mg/L) | S5(mg/L) |
| ① | 0 | 0.24 | 0.32 | 0.40 | 0.48 | 0.56 |
| ② | 0 | 0.32 | 0.40 | 0.48 | 0.56 | 0.64 |
| ③ | 0 | 0.08 | 0.16 | 0.24 | 0.48 | 0.56 |
| ④ | 0 | 0.40 | 0.80 | 1.20 | 1.60 | 2.40 |
As shown in Fig. 8~15, from the linear rule of As, Sb element under each concentration gradient, hence it is evident that find out same concentration
Under the peak intensity of Sb be substantially better than As element, it is also seen that the method is better than As to the sensitivity of Sb, and detection limit is wanted
Better than elements A s.Compare the linear rule under the different gradients under same element, it can be seen that the linear rule of group 2. is brighter
It is aobvious, therefore under the concentration gradient of group 2. in the case where the solidification of other techniques must be asked, obtained linear rule such as Figure 16~17 institute
Show, hence it is evident that find out solidify under technique the sensitivity of As significantly improve, and the intensity at peak effectively enhances under identical conditions, and
And background reduces, and is linearly obviously improved, therefore the concentration gradient is most preferably to meet the concentration gradient of linear rule.
Measurement content: sample introduction needle is inserted into prepare liquid, prepare liquid is carried out with inductively-coupled plasma spectrometer
Measurement, is converted into degree according to the concentration value of measurement result, obtains the content of impurity element As, Sb in silicon bronze.
Table 1 is prepare liquid sample introduction parameter；
Table 1
Under different capacity and the flow of different cooling airs, detection limit is lower, and it is the 6th group that peak intensity is higher, power
For 1.2kW and sample introduction parameter that cooling gas flow is 20LPM is the parameter values for detection optimized.
Table 2 is optimum optimization parameter；
Table 2
Five, before sample amounts analysis, preanalysis (SemiQuant) is carried out to unknown sample, determines element in sample
Type and substantially content, the disturbed condition of element wavelength surrounding to be measured is differentiated according to qualitative analysis.According to national standard GB/
The analytical line recommended in T5121.27-2008 is As:189.042r；Sb:206.83.It is detected around the two spectral lines without dry
Disturb the presence of spectral line.
Six, detection limit:
Detection limit refer to generate one can reliably be detected analysis signal required for certain element Cmin or
Content can distinguish over the concentration limit of noise,
It takes 10 parts of blank to be measured, by 3 times of standard deviations (S) and slope (K), calculates detection limit (3S/K), as a result such as
Shown in the following table 4:
Table 4
| Group | 1 | 2 | 3 | 4 | 5 | Average value | Detection limit |
| As | -0.0003 | 0.0027 | 0.0014 | 0.0040 | 0.0055 | 0.0025 | 0.0088 |
| Sb | -0.0082 | -0.0055 | -0.0068 | -0.0117 | -0.0177 | -0.0122 | 0.0119 |
| Group | 6 | 7 | 8 | 9 | 10 | SD | |
| As | -0.0019 | 0.0077 | -0.0012 | 0.0049 | 0.0019 | 0.0029 | |
| Sb | -0.0157 | -0.0149 | -0.0156 | -0.0114 | 0.0115 | 0.0040 |
The detection that the detection of As is limited to 0.0088, Sb as can be seen from Table 4 is limited to 0.0119, and corresponding A s is minimum, and element contains
It is 0.00007% that amount, which is the minimum constituent content of 0.000051%, Sb,.It can be seen that the method is to the sensitive of the two elements
Degree is very high, can accurately measure the As of low content in silicon bronze, the constituent content of Sb.
Seven, data process&analysis:
(1) precision
1) repeated
Ten arithmetic mean of instantaneous values and standard deviation for calculating separately AS, Sb are continuously surveyed to sample J4-12, J4-21 with this method
Difference and relative standard deviation the data obtained are as shown in table 5 below, according to standard
Table 5
2) accuracy
It is measured with standard liquid of this method to preparation, the result of measurement is as shown in table 6 below:
Table 6
(2) calculating of the rate of recovery
The rate of recovery is the extent of damage for reflecting determinand in sample analysis, and fewer rate of recovery of loss is higher.It can demonstrate,prove
Whether bright molten sample is complete, if there is loss, whether method conditional coefficient is reasonable.
Recovery of standard addition=(standardized sample measured value-Specimen Determination value)/scalar quantity * 100%
Scalar quantity cannot be excessive, generally the 0.5~2 of determinand content times, and the total content after mark-on is no more than side
The determination of the upper limit of method.
1) blank recovery of standard addition
Table 7
| Group | Mark-on blank determination value | Blank determination value | Mark-on value | Rate of recovery % |
| 1 | 0.3267 | 0.0074 | 0.32 | 99.78 |
| 2 | 0.3994 | 0.0074 | 0.40 | 98.00 |
| 3 | 0.5648 | 0.0074 | 0.56 | 99.54 |
| 4 | 0.6419 | 0.0074 | 0.64 | 99.14 |
Four groups of blank standardized samples have been surveyed respectively, and the obtained rate of recovery is as shown above, average recovery rate 99.12%.
Because, it can be said that bright, within the scope of systematic error, can be used as graticule makes measured value there are certain systematic error
With.
2) sample recovery of standard addition
Table 8
20 groups of experiments are done to As, Sb respectively, the gained rate of recovery is as shown above, and average recovery rate is respectively that As exists
Between 104.75%~124.95%；Sb is again between 92.80%~122%.
Eight, effect (integrated structure feature):
It is capable of the constituent content of Accurate Determining bearing holder material silicon bronze impurity element As, Sb using this method, it should
The detection that detection method is limited to 0.0088, Sb for the detection that the detection limit of two elements is respectively as follows: As is limited to 0.0119.Corresponding A s
Minimum constituent content is that the minimum constituent content of 0.000051%, Sb is 0.00007%.It can be seen that effectively increasing sensitivity.For
The rate of recovery of the As element of determinand is between 104.75%~124.95%；Sb be 92.8%~122% between, the rate of recovery compared with
Height can be applied in production detection.
Claims (6)
1. accurately measuring the method for impurity element As, Sb content in silicon bronze with ICP-AES, it is characterised in that this method is by following
Step is completed:
One, light room is handled: using first high frequency 30min~60min, again by the way of low frequency 60min~120min, carrying out purple to light room
Outer purging；
Two, it exposes: the standard specimen containing As and the standard specimen containing Sb is exposed；
Three, in light room, parameter setting: incident power 1.0kW parameter setting: is carried out to inductively-coupled plasma spectrometer
~1.2kW, cooling gas flow are 18L/min~20L/min, and secondary air amount is 0.3L/min~0.4L/min, atomization air flow
Amount is 32L/min~34L/min, and peristaltic pump is 1.3mL/min~1.4mL/min, and Vertical Observation mode is observed；
Four, standard curve is chosen:
1., As concentration be 0.08mg/L~2.40mg/L within the scope of configure various concentration As solution, in various concentration
5 kinds or 5 kinds or more are chosen according to increasing concen-trations form in As solution and is used as 1 group of As standard curve sample, choose at least 4 groups of As marks
Directrix curve sample tests every group of As standard curve sample according to the parameter that step 3 is set respectively, and it is bent to obtain test
Line is evenly distributed situation one group of optimal test curve of selection as As standard song according to absorption peak in all test curves
Line, and by the parameter setting of the As standard curve into inductively-coupled plasma spectrometer；
2., Sb concentration be 0.08mg/L~2.40mg/L within the scope of configure various concentration Sb solution, in various concentration
5 kinds or 5 kinds or more are chosen according to increasing concen-trations form in Sb solution and is used as 1 group of Sb standard curve sample, choose at least 4 groups of mark Sb
Directrix curve sample tests every group of Sb standard curve sample according to the parameter that step 3 is set respectively, and it is bent to obtain test
Line is evenly distributed situation one group of optimal test curve of selection as Sb standard song according to absorption peak in all test curves
Line, and by the parameter setting of the Sb standard curve into inductively-coupled plasma spectrometer；
Five, it measures content: sample introduction needle being inserted into prepare liquid, prepare liquid is surveyed with inductively-coupled plasma spectrometer
Amount, is calculated according to measurement result, obtains the content of impurity element As, Sb in silicon bronze.
2. the method according to claim 1 that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES,
It is characterized in that in the step 1 carrying out ultraviolet purging to light room using first high frequency 30min, again by the way of low frequency 60min.
3. the method according to claim 1 that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES,
It is characterized in that the standard specimen containing As and the standard specimen containing Sb are carried out to the exposure of 80s~120s in the step 2.
4. the method according to claim 3 that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES,
It is characterized in that the standard specimen containing As and the standard specimen containing Sb are carried out to the exposure of 80s in the step 2.
5. the method according to claim 1 that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES,
It is characterized in that in the step 3 that incident power is 1.2kW, cooling gas flow 20L/min, secondary air amount 0.4L/min,
Atomization gas flow is 34L/min, peristaltic pump 1.4mL/min.
6. the method according to claim 1 that impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES,
It is characterized in that prepare liquid described in step 5 is prepared according to the following steps:
Nitric acid/hydrochloric acid mixed solution is added into conical flask, silicon bronze sample is placed in nitric acid/hydrochloric acid mixed solution, then
It is heated to 20 DEG C~40 DEG C, and insulated and stirred 30min~50min at 20 DEG C~40 DEG C, then into nitric acid/hydrochloric acid mixed solution
Nitric acid solution to solution is added dropwise to clarify, is finally cooled to room temperature, is settled to 50mL with hydrochloric acid solution, shake up standing, obtain to be measured
Liquid, the quality of the silicon bronze sample and the ratio of nitric acid/hydrochloric acid mixed solution volume are (0.85g~1g): (20mL~
30mL), nitric acid solution and the volume ratio of hydrochloric acid solution are 1:4 in the nitric acid/hydrochloric acid mixed solution, in the nitric acid solution
HNO3Mass fraction be 66%~68%, the mass fraction of HCL is 36%~38% in the hydrochloric acid solution.
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