CN107917907A - Micro- detection method in chromium powder - Google Patents
Micro- detection method in chromium powder Download PDFInfo
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Abstract
The invention discloses detection method micro- in a kind of chromium powder, on inductively coupled plasma atomic emission spectrometer, selects micro- optimal detection condition and best detection wavelength to be measured, detection chromium matrix standard serial solution obtains standard working curve；By standard serial solution testing conditions and each micro- best detection wavelength, sample solution is detected, obtains corresponding the intensity of spectral line of trace element to be measured in sample solution；The micronutrient levels to be measured in sample solution is determined according to corresponding the intensity of spectral line of trace element to be measured in the standard working curve and sample solution of acquisition.The detection method can measure the content of various trace elements in chromium powder at the same time, and use chromium Matrix Match standard working curve method, both spectra1 interfer- of the main amount matrix of chromium to determination of trace element had been eliminated, has also eliminated the influence of hydrochloric acid solution matrix, Results of Trace Element Detection accuracy is high.
Description
Technical field
The invention belongs to the technical field of analytical chemistry quantitative analysis, and in particular to micro- detection in a kind of chromium powder
Method.
Background technology
Chromium powder (Cr) is mainly used in wlding, and vacuum coating, plasma spraying, high temperature insostatic pressing (HIP) chromium target raw material also can conduct
The additive of hard alloy, diamond tool, stainless steel or ceramics, can increase surface corrosion resistance, addition is a small amount of also can conduct
Grain growth inhibitor.Being directed to the detection method of micro impurity element in chromium powder has ICP-MS determination methods, atomic absorption light
Spectrometry, titration, spectrophotometry, polarography and gravimetric method, the deficiency of these detection methods are：
Patent《The ICP-MS assay methods of micro- impurity in High Pure Chromium》(patent (publication) 104597110A), relates to
And the test of ICP-MS methods the high-purity chromium powder for being purity more than 99.99% in phosphorus, copper, lead, tin, bismuth, antimony, arsenic, use
The molten sample of hydrochloric acid, Standard entertion mass spectrography are tested.This method only relates to micro in high-purity chromium powder of the purity more than 99.99%
Phosphorus, copper, lead, tin, bismuth, antimony, arsenic measure, and hydrochloric acid solution therein will cause very big mass spectrum to disturb, and be not particularly suited for ICP-
MS is tested, and influences micro- test accuracy.The mass spectrum interference for eliminating hydrochloric acid is usually steamed using chromatography (microtrabeculae) separation, electric heating
The resolution ratio sectorial magnetic field ICP-MS of hair or selection costly, this makes the operation of this method sufficiently complex, does not apply to professional technique
General analysis person's operation beyond member, analysis cost is high, is not suitable for manufacturing enterprise's batch detection analysis and promotes and applies.
Document《Micro Ni, Cu, Mn, Fe, Pb, Sb, Zn, Ca, Mg in Standard entertion atomic absorption method METHOD FOR CONTINUOUS DETERMINATION chromium powder
Content》(《Natural science edition》, 2006,19 (4)：465-466), although the atomic absorption spectrography (AAS) being related to is tested 9 in chromium powder
A impurity element, but often one impurity element of survey must all replace hollow cathode lamp, calibration curve solution of reperformance test
And sample solution, the measure cycle is longer, cumbersome；
Document《The research of Fe (III) in automatic reference flow injection analysis measure chromium powder》(《Leather science and work
Journey》, 2004,14 (2)：15-17), titration, spectrophotometry, polarography and the gravimetric method being related to determine respectively iron, aluminium,
Silicon, lead, tin, bismuth, stilba prime element, each element chemistry processing method are different, it is necessary to and sample is handled respectively to be tested, sample
Process cycle is longer, and process is cumbersome, is not suitable for rapid batch production analysis.
Document《The measure disodium ethylene diamine tetraacetate drop of GB/T 4702.4-2008 crome metal chemical analysis method iron contents
Determine method and flame atomic absorption spectrometry》With《GB/T 4702.5-2008 crome metal chemical analysis method aluminum content tests second
Edetate disodium titration and flame atomic absorption spectrometry》, the impurity element Monitoring lower-cut being related to is higher, ethylenediamine tetraacetic
Acetic acid disodium titration and Flame Atomic Absorption Spectrometry Determination iron, aluminium, Monitoring lower-cut 0.10%；Documentation standards add atom
The content of micro Ni, Cu, Mn, Fe, Pb, Sb, Zn, Ca, Mg do not write test limit in absorption process METHOD FOR CONTINUOUS DETERMINATION chromium powder.
At present, the document of impurity element or patent in chromium powder is measured using inductively coupled plasma emission spectrography to have no
Report.
The content of the invention
Present invention aim to address the above problem, there is provided it is a kind of it is easy to operate, detection cycle is short, suitable for batch detection
Micro- detection method in chromium powder.
In order to solve the above technical problems, the technical scheme is that：Micro- detection method in a kind of chromium powder,
On inductively coupled plasma atomic emission spectrometer, the matching detection condition of selection criteria serial solution and each
Micro- matching detection wavelength to be measured, detection contain micro- chromium matrix standard serial solution to be measured, obtain to be measured
The standard working curve of microelement concentration-the intensity of spectral line；
On inductively coupled plasma atomic emission spectrometer, by standard serial solution matching detection condition and respectively treat
The matching detection wavelength of micrometer secondary element, detects sample solution, obtains corresponding the intensity of spectral line of trace element to be measured in sample solution；
Determine that sample is molten according to corresponding the intensity of spectral line of trace element to be measured in the standard working curve and sample solution of acquisition
Micronutrient levels to be measured in liquid.
Micro- detection method in above-mentioned chromium powder, sample solution dissolve by heating chromium powder sample preparation by hydrochloric acid and form.
Micro- detection method, specifically includes following steps in above-mentioned chromium powder：
S1：Draw standard working curve
S11：Prepare chromium matrix standard serial solution
Weigh high-purity 0.1~0.4g of chromium powder, add 20~40mL of hydrochloric acid, heated under the conditions of 200~400 DEG C of temperature, it is high
After pure chromium powder is completely dissolved, cooling, adds each micro- normal storage solution to be measured, solution is diluted to volumetric flask with water
Scale, is configured to the chromium matrix standard serial solution that each trace element to be measured is respectively provided with appropriate gradient；
S12：Detect chromium matrix standard serial solution
Open inductively coupled plasma atomic emission spectrometer, the matching detection condition of selection criteria serial solution and each
Micro- matching detection wavelength to be measured, micro- spectral line to be measured is strong in sequentially determining chromium matrix standard serial solution
Degree；
S13：Obtain standard working curve
Standard working curve is drawn according to each micro- concentration to be measured, the intensity of spectral line automatically by computer software, and
Carry out background correction；
S2：Measure micronutrient levels to be measured
S21：Prepare sample solution
Weigh chromium powder 0.1~0.4g of sample, add 20~40mL of hydrochloric acid, heated under the conditions of 200~400 DEG C of temperature, chromium
After powder sample is completely dissolved, cooling, is diluted with water to volumetric flask scale, is configured to sample solution；
S22：Detect sample solution
Under the operating condition identical with drawing standard working curve, each micro- spectrum to be measured in determination sample solution
Line strength, computer automatically determine each micro- content to be measured in sample solution according to standard working curve.
Micro- detection method in above-mentioned chromium powder, the hydrochloric acid are top grade pure hydrochloric acid, and the water is pure water.
Micro- detection method in above-mentioned chromium powder, micro- normal storage solution to be measured include by nickel, manganese,
The standard solution 1 and/or stored up by iron, aluminium, vanadium single element standard that zinc, calcium, magnesium, titanium, cobalt single element normal storage solution are configured to
Deposit the standard solution 2 that solution is configured to.Found through inventor's many experiments, iron, aluminium, foreign matter of vanadium content are inclined in chromium powder used in production
Height, more than more than 1000ppm, other impurity are relatively low, less than 300ppm, thus are configured with the hybrid standard storage of two sets of various concentrations
Standby liquid, is prepared for the standard working curve of various concentrations scope, to ensure sample defects inspecting accuracy.
Micro- detection method in above-mentioned chromium powder, it is described it is to be measured trace element include nickel, manganese, iron, zinc, calcium, magnesium,
Aluminium, titanium, vanadium, cobalt.In the prior art, there is presently no a kind of inductively coupled plasma atomic emission spectrometry quickly to measure chromium
The detection method of nickel, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, cobalt in powder.In inductively coupled plasma atomic emission spectrometry
In, the scope of Detection wavelength can have accuracy of detection fairly obvious influence, discovery largely be tested by the present inventor, when each
Micro- Detection wavelength to be measured is：Nickel is 216.556nm, manganese 257.610nm, iron 259.940nm, zinc are
213.856nm, calcium 184.006nm, magnesium 279.553nm, aluminium 167.079nm, titanium 337.280nm, vanadium are
292.402nm, cobalt 230.786nm, foregoing micro- testing result error to be detected is small, and accuracy of detection is high, with regard to iron, aluminium
Detection elements lower limit 0.1% can reduce by 100 times than what is mentioned in existing literature.
Micro- detection method in above-mentioned chromium powder, the inductively coupled plasma atomic emission spectrometer, detection
Condition is：Using horizontal observed pattern, RF incident powers are 1150~1350W, nebulizer gas 0.2~1.5L/min of flow,
It is 50~100rpm to rinse pump speed and analysis pump speed, and washing time is 10~40s, and secondary air speed is 0.5~1.5L/min,
Flow rate of carrier gas is 0.5~1.0L/min, and the long and short ripple time of integration is 5~30s, and integral number of times is 2~4 times, and spectrum room temperature is
37.9~38.1 DEG C.Further preferred testing conditions are the optimum level observed pattern of use, and RF incident powers are 1150W, mist
Change device gas flow 0.6L/min, it is 50rpm to rinse pump speed and analysis pump speed, washing time 30s, and secondary air speed is
0.5L/min, the long wave time of integration are 5s, and the shortwave time of integration is 10s, and integral number of times is 2 times, and spectrum room temperature is 38 DEG C.Need
It is noted that the purpose of setting testing conditions is in order to be measured to the working curve solution and sample solution of preparation,
The design parameter of the detection of inductively coupled plasma atomic emission spectrometer can be set according to conventional detection condition, however it is not limited to
Aforementioned parameters.It is detected when under testing conditions provided by the invention, testing result is more stable, and error is small.
Micro- detection method in above-mentioned chromium powder, background correction can use conventional standard addition method, matrix
With standard working curve method, internal standard method etc..The specific method and step of background correction are carried out according to custom requirements.In this hair
In bright, adjusted or cast out by the big back of the body of Matrix effects using Matrix Match standard working curve method and spectrogram or so background positions
The method of scape carries out background correction, does the matrix of standard working curve using High Pure Chromium first, with test sample Matrix Match, disappears
Except sample and standard working curve baseline lamination；Then after standard working curve is tested, each survey is opened respectively
The spectrogram of element is tried, situation is disturbed according to background, left and right background positions is adjusted or casts out the big background of Matrix effects to realize
Background correction.
The raw material such as the hydrochloric acid and water that are arrived involved in the present invention, can be bought by market and obtained, had no specifically limited.
Micro- detection method has the advantages that in chromium powder provided by the invention：
(1) chromium Matrix Match standard working curve method is used, had both eliminated light of the main amount matrix of chromium to determination of trace element
Spectrum interference, also eliminates the influence of hydrochloric acid solution matrix, and Results of Trace Element Detection accuracy is high；
(2) chromium powder sample is once dissolved, the content of various trace elements can be measured at the same time, does not limit to chromium powder purity, inspection
The survey cycle is short, scope is wide, and analysis method is rapidly and efficiently；
(3) sample dissolving is saved testing cost, is reduced chemical levels with sour species is few, dosage is small, beneficial to environmental protection and
Operator's health；
(4) sample handling processes are easy, and instrumentation is simple, except the general analysis operative employee of professional technique an ancient official title also can use
The detection method carries out the detection that batch multielement quickly produces analysis, and strong applicability, is worth popularization in the field of business.
Brief description of the drawings
Fig. 1 is nickel standard working curve in the embodiment of the present invention：
Fig. 2 is manganese standard working curve in the embodiment of the present invention；
Fig. 3 is iron standard working curve in the embodiment of the present invention；
Fig. 4 is zinc standard working curve in the embodiment of the present invention；
Fig. 5 is standard calcium working curve in the embodiment of the present invention；
Fig. 6 is magnesium standard working curve in the embodiment of the present invention；
Fig. 7 is aluminium standard working curve in the embodiment of the present invention；
Fig. 8 is titanium standard working curve in the embodiment of the present invention；
Fig. 9 is vanadium standard working curve in the embodiment of the present invention；
Figure 10 is cobalt standard working curve in the embodiment of the present invention；
Figure 11 is spectrogram before ferro element or so background correction；
Figure 12 is spectrogram after the left background correction of ferro element.
Embodiment
Technical scheme is described further with reference to specific embodiment, further to show this hair
The advantages of bright：
It is in the examples below that the reagent used and instrument is as follows：
1st, reagent
Hydrochloric acid (top pure grade)；
Quartz beaker and the quartz surfaces ware (200mL) that matches；
Glass or polypropylene volumetric flask (100mL)；
Polytetrafluoroethylene (PTFE) reagent bottle (100mL)；
High-purity argon gas (>=99.99%)；
High-purity chromium powder (>=99.99%)；
Single element normal storage solution：For national standard solution, nickel, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, cobalt, concentration
It is 1000 μ g/mL；
Standard solution 1：(medium：It is acid) with automatic liquid-transfering gun point take single element standard reserving solution nickel, manganese, zinc, calcium, magnesium,
Each 5.00mL of titanium, cobalt is diluted with water so far at the scale of volumetric flask in same 100mL volumetric flasks, is mixed；One is transferred to gather
Stored in tetrafluoroethene reagent bottle, it is respectively 50 μ g/mL to mix nickel, manganese, zinc, calcium, magnesium, titanium, cobalt concentration in standard liquid；
Standard solution 2：(medium：It is acid) with automatic pipettor point take iron, aluminium, vanadium single element standard reserving solution each
20.00mL is diluted with water so far at the scale of volumetric flask in same 100mL volumetric flasks, is mixed.It is transferred to a polytetrafluoroethyl-ne
Stored in alkene reagent bottle, it is respectively 200 μ g/mL to mix iron, aluminium, vanadium concentration in standard liquid.
2nd, instrument
Electronic balance：D=0.1mg；
U.S.'s thermoelectricity icp6300 types inductively coupled plasma atomic emission spectrometer (matches somebody with somebody central tube, the mist of quartz material
Change room and atomizer)；
Temperature controllable electric hot plate (room temperature~450 DEG C).
Micro- detection method, comprises the following steps that in chromium powder provided by the invention：
S1：Draw standard working curve
S11：Prepare chromium matrix standard serial solution
It is parallel to weigh four parts of the high-purity chromium powders of 0.1~0.4g, it is respectively placed in four 200mL quartz beakers, addition 20~
40mL hydrochloric acid, covers quartz surfaces ware, is dissolved on 200~400 DEG C of electric hot plates；Sample dissolving is complete, removes, and is rushed with a small amount of water
Wall of cup and surface plate inner wall are washed, is diluted to 20~40mL, cap upper surface ware, 1 is boiled in heating on 200~400 DEG C of electric hot plates~
3min, removes cooling, test solution is transferred to respectively in four 100mL volumetric flasks, then is divided with automatic liquid-transfering gun in four volumetric flasks
0~4mL standard solution 1 and standard solution 2 are not added not respectively, are diluted with water to scale, are shaken up；
S12：Detect chromium matrix standard serial solution
Open inductively coupled plasma atomic emission spectrometer, the optimal detection condition of selection criteria serial solution and each
The best detection wavelength of trace element (nickel, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, cobalt) to be measured, sequentially determining chromium matrix standard
Each micro- the intensity of spectral line to be measured in serial solution, according to each micro- concentration to be measured, the intensity of spectral line by computer
Software draws standard working curve automatically, and carries out background correction, as shown in Fig. 1-Figure 10, be respectively nickel, manganese, iron, zinc, calcium,
Magnesium, aluminium, titanium, vanadium, cobalt, concentration unit are the standard working curve of μ g/100mL；
S2：Measure micronutrient levels to be measured
S21：Prepare sample solution
0.1~0.4g hafnium metal powfer samples are weighed, are placed in 200mL quartz beakers, 20~40mL hydrochloric acid is added, covers stone
English surface plate, dissolves on 200~400 DEG C of electric hot plates；Sample dissolving is complete, removes, and wall of cup and surface plate are rinsed with a small amount of water
Inner wall, is diluted to 20~40mL, and cap upper surface ware, boils 1~3min in heating on 200~400 DEG C of electric hot plates, remove cooling,
Dissolved samples solution is transferred in 100mL volumetric flasks, is diluted with water to scale, is shaken up；
S22：Detect sample solution
Under the operating condition identical with drawing standard working curve, each micro- spectrum to be measured in determination sample solution
Line strength, computer automatically determine each micro- content to be measured in sample solution according to standard working curve.
The testing conditions of inductively coupled plasma atomic emission spectrometer are：
Using horizontal observed pattern, RF incident powers are 1150~1350W, nebulizer gas 0.2~1.5L/min of flow,
It is 50~100rpm to rinse pump speed and analysis pump speed, and washing time is 10~40s, and secondary air speed is 0.5~1.5L/min,
Flow rate of carrier gas is 0.5~1.0L/min, and the long and short ripple time of integration is 5~30s, and integral number of times is 2~4 times, and spectrum room temperature is
37.9~38.1 DEG C.
In the present embodiment, background correction comprises the following steps that：After testing standard working curve, each is opened respectively
The spectrogram of test elements, situation is disturbed according to background, adjusts left and right background, and left and right background baseline answers horizontal not appearance, energy
Than substantially suitable, to having Interference Peaks at the background positions of left and right, by moving horizontally background positions or adjustment background pixel width
To eliminate interference of the Interference Peaks to left and right background；Adjustment can not eliminate interference, take the mode for deleting left background or right background
Carry out background correction.By taking ferro element as an example, as shown in FIG. 11 and 12, before background correction is carried out, ferro element detection spectrogram is left
Background is disturbed peak influence, and apparently higher than right background, this experiment use first moves right left background one pixel position energy ratio
Put, then left background is adjusted to a pixel by two pixels, make left background baseline and right background baseline values, eliminate the left back of the body
Scape interference problem.
Embodiment 1
Detect nickel in No. 1 chromium powder sample, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, the method for cobalt and trace element inspection to be measured
Survey wavelength, method detection limit, sample detection lower limit.
S1：Draw standard working curve
S11：Prepare chromium matrix standard serial solution
It is parallel to weigh four parts of the high-purity chromium powder matrixes of 0.1000g, it is respectively placed in four 200mL quartz beakers, adds 20mL
Hydrochloric acid, covers quartz surfaces ware, is dissolved on 250 DEG C of electric hot plates, and sample dissolving is complete, removes, with a small amount of water rinse wall of cup and
Surface plate inner wall, is diluted to about 30mL, cap upper surface ware, boils 1min in heating on 250 DEG C of electric hot plates, remove cooling, will try
Liquid is transferred in four 100mL volumetric flasks respectively, then is separately added into standard solution 1 and mark in four volumetric flasks with automatic liquid-transfering gun
Quasi- solution 2；Wherein：First part is blank solution, and the addition of standard solution 1 and standard solution 2 is 0；Second part of standard is molten
The addition of liquid 1 and standard solution 2 is 0.2mL；3rd part of standard solution 1 and 2 addition of standard solution is 0.5mL；4th
The standard solution 1 of part and the addition of standard solution 2 are 1.0mL；Then scale is diluted with water to, is shaken up to be measured.
S12：Detect chromium matrix standard serial solution
Open inductively coupled plasma atomic emission spectrometer, the optimal detection condition of selection criteria serial solution and each
The best detection wavelength of trace element (nickel, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, cobalt) to be measured, sequentially determining chromium matrix standard
Each micro- the intensity of spectral line to be measured in serial solution；
S13：Obtain standard working curve
Using micro- concentration to be measured as abscissa, the intensity of spectral line is ordinate, by the computer testing of instrument configuration
Software draws standard working curve automatically, and carries out background correction.
S2：Measure micronutrient levels to be measured
S21：Prepare sample solution
Precise 0.1000g hafnium metal powfers, are placed in 200mL quartz beakers, add 20mL hydrochloric acid, cover quartz surfaces
Ware, dissolves on 250 DEG C of electric hot plates, and sample dissolving is complete, removes, and rinses wall of cup and surface plate inner wall with a small amount of water, is diluted to
About 30mL, cap upper surface ware, boils 1min in heating on 250 DEG C of electric hot plates, removes cooling, dissolved samples solution is transferred to
In 100mL volumetric flasks, scale is diluted with water to, is shaken up to be measured.
S22：Detect sample solution
Under the operating condition identical with drawing standard working curve, each micro- spectrum to be measured in determination sample solution
Line strength, computer automatically determine each micro- content to be measured in sample solution according to standard working curve.
The testing conditions of inductively coupled plasma atomic emission spectrometer are：Using horizontal observed pattern, RF incidence work(
Rate is 1150W, nebulizer gas flow 0.6L/min, rinses pump speed and analysis pump speed is 50rpm, washing time 30s, auxiliary
It is 0.5L/min to help gas velocity, and the long wave time of integration is 5s, and the shortwave time of integration is 10s, and integral number of times is 2 times, spectrum room temperature
Spend for 38 DEG C.
Table 1：Trace element detection wavelength to be measured in embodiment 1：
By blank solution METHOD FOR CONTINUOUS DETERMINATION 10 times, 3 calculating are multiplied by with the standard deviation average values of 10 measure, obtain treating micrometer
The method detection limit of secondary element is as shown in table 2：
Table 2：Trace element method detection limit to be measured in embodiment 1
Sample detection lower limit=method detection limit+blank content, only when micronutrient levels to be measured etc. in blank solution
When 0, sample detection lower limit is equal to method detection limit, if micronutrient levels to be measured is not equal to 0 in blank solution, sample detection
Lower limit detects limit for height with regard to ratio method.
The selection criteria addition method in test software, four parts of standard working curve solution are tested respectively, measure sky
Micronutrient levels to be measured in white solution：
Table 3：Micronutrient levels to be measured in 1 blank solution of embodiment
Table 4：Trace element detection lower limit to be measured in embodiment 1
Known by table 4：Iron tramp Monitoring lower-cut is 8.79ppm, i.e., 0.0009% in this method chromium powder, aluminium defects inspecting lower limit
For 4.85ppm, i.e., 0.0005%, more than 100 times are reduced than document report iron, aluminium element Monitoring lower-cut 0.10%, detection spirit
Sensitivity is considerably higher.
Embodiment 2
Detect nickel in No. 1 chromium powder sample, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, the method for cobalt and trace element inspection to be measured
Survey wavelength, method detection limit, sample detection lower limit.
S1：Draw standard working curve
S11：Prepare chromium matrix standard serial solution
It is parallel to weigh four parts of the high-purity chromium powder matrixes of 0.2000g, it is respectively placed in four 200mL quartz beakers, adds 30mL
Hydrochloric acid, covers quartz surfaces ware, is dissolved on 300 DEG C of electric hot plates, and sample dissolving is complete, removes, with a small amount of water rinse wall of cup and
Surface plate inner wall, is diluted to about 30mL, cap upper surface ware, boils 1min in heating on 300 DEG C of electric hot plates, remove cooling, will try
Liquid is transferred in four 100mL volumetric flasks respectively, then is separately added into standard solution 1 and mark in four volumetric flasks with automatic liquid-transfering gun
Quasi- solution 2；Wherein：First part is blank solution, and the addition of standard solution 1 and standard solution 2 is 0；Second part of standard is molten
The addition of liquid 1 and standard solution 2 is 0.5mL；3rd part of standard solution 1 and 2 addition of standard solution is 1.0mL；4th
The standard solution 1 of part and the addition of standard solution 2 are 2.0mL；Then scale is diluted with water to, is shaken up to be measured.
S12：Detect chromium matrix standard serial solution
Open inductively coupled plasma atomic emission spectrometer, the optimal detection condition of selection criteria serial solution and each
The best detection wavelength of trace element (nickel, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, cobalt) to be measured, sequentially determining chromium matrix standard
Each micro- the intensity of spectral line to be measured in serial solution；
S13；Obtain standard working curve
Using micro- concentration to be measured as abscissa, the intensity of spectral line is ordinate, draws standard working curve, and carry out
Background correction；
S2：Measure micronutrient levels to be measured
S21：Prepare sample solution
Precise 0.2000g hafnium metal powfers, are placed in 200mL quartz beakers, add 30mL hydrochloric acid, cover quartz surfaces
Ware, dissolves on 300 DEG C of electric hot plates, and sample dissolving is complete, removes, and rinses wall of cup and surface plate inner wall with a small amount of water, is diluted to
About 30mL, cap upper surface ware, boils 1min in heating on 300 DEG C of electric hot plates, removes cooling, dissolved samples solution is transferred to
In 100mL volumetric flasks, scale is diluted with water to, is shaken up to be measured.
S22：Detect sample solution
Under the operating condition identical with drawing standard working curve, each micro- spectrum to be measured in determination sample solution
Line strength, computer automatically determine each micro- content to be measured in sample solution according to standard working curve.
The testing conditions of inductively coupled plasma atomic emission spectrometer are：Using horizontal observed pattern, RF incidence work(
Rate is 1150W, nebulizer gas flow 0.6L/min, rinses pump speed and analysis pump speed is 50rpm, washing time 30s, auxiliary
It is 0.5L/min to help gas velocity, and the long wave time of integration is 5s, and the shortwave time of integration is 10s, and integral number of times is 2 times, spectrum room temperature
Spend for 38 DEG C.
Table 5：Trace element detection wavelength to be measured in embodiment 2：
By blank reagent solution METHOD FOR CONTINUOUS DETERMINATION 10 times, 3 calculating are multiplied by with the standard deviation average values of 10 measure, are treated
The method detection limit of micrometer secondary element is as shown in table 6：
Table 6：Trace element detection limit to be measured in embodiment 2
Sample detection lower limit=method detection limit+blank content, only when micronutrient levels to be measured etc. in blank solution
When 0, sample detection lower limit is equal to method detection limit, if micronutrient levels to be measured is not equal to 0 in blank solution, sample detection
Lower limit detects limit for height with regard to ratio method.
The selection criteria addition method in test software, four parts of standard working curve solution are tested respectively, measure sky
Micronutrient levels to be measured in white solution：
Table 7：Micronutrient levels to be measured in 2 blank solution of embodiment
Table 8：Trace element detection lower limit to be measured in embodiment 2
Known by table 8：Iron tramp Monitoring lower-cut is 8.93ppm, i.e., 0.0009% in this method chromium powder, aluminium defects inspecting lower limit
For 4.97ppm, i.e., 0.0005%, more than 100 times are reduced than document report iron, aluminium element Monitoring lower-cut 0.10%, detection spirit
Sensitivity is considerably higher.
Embodiment 3
Detect nickel in No. 1 chromium powder sample, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, the method for cobalt and trace element inspection to be measured
Survey wavelength, method detection limit, sample detection lower limit.
S1：Draw standard working curve
S11：Prepare chromium matrix standard serial solution
It is parallel to weigh four parts of the high-purity chromium powder matrixes of 0.4000g, it is respectively placed in four 200mL quartz beakers, adds 40mL
Hydrochloric acid, covers quartz surfaces ware, is dissolved on 300 DEG C of electric hot plates, and sample dissolving is complete, removes, with a small amount of water rinse wall of cup and
Surface plate inner wall, is diluted to about 30mL, cap upper surface ware, boils 1min in heating on 300 DEG C of electric hot plates, remove cooling, will try
Liquid is transferred in four 100mL volumetric flasks respectively, then is separately added into standard solution 1 and mark in four volumetric flasks with automatic liquid-transfering gun
Quasi- solution 2；Wherein：First part is blank solution, and the addition of standard solution 1 and standard solution 2 is 0；Second part of standard is molten
The addition of liquid 1 and standard solution 2 is 1.0mL；3rd part of standard solution 1 and 2 addition of standard solution is 2.0mL；4th
The standard solution 1 of part and the addition of standard solution 2 are 4.0mL；Then scale is diluted with water to, is shaken up to be measured.
S12：Detect chromium matrix standard serial solution
Open inductively coupled plasma atomic emission spectrometer, the optimal detection condition of selection criteria serial solution and each
The best detection wavelength of trace element (nickel, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, cobalt) to be measured, sequentially determining chromium matrix standard
Each micro- the intensity of spectral line to be measured in serial solution；
S13；Obtain standard working curve
Using micro- concentration to be measured as abscissa, the intensity of spectral line is ordinate, draws standard working curve, and carry out
Background correction；
S2：Measure micronutrient levels to be measured
S21：Prepare sample solution
Precise 0.4000g hafnium metal powfers, are placed in 200mL quartz beakers, add 40mL hydrochloric acid, cover quartz surfaces
Ware, dissolves on 300 DEG C of electric hot plates, and sample dissolving is complete, removes, and rinses wall of cup and surface plate inner wall with a small amount of water, is diluted to
About 30mL, cap upper surface ware, boils 1min in heating on 300 DEG C of electric hot plates, removes cooling, dissolved samples solution is transferred to
In 100mL volumetric flasks, scale is diluted with water to, is shaken up to be measured.
S22：Detect sample solution
Under the operating condition identical with drawing standard working curve, each micro- spectrum to be measured in determination sample solution
Line strength, computer automatically determine each micro- content to be measured in sample solution according to standard working curve.
The testing conditions of inductively coupled plasma atomic emission spectrometer are：Using horizontal observed pattern, RF incidence work(
Rate is 1150W, nebulizer gas flow 0.6L/min, rinses pump speed and analysis pump speed is 50rpm, washing time 30s, auxiliary
It is 0.5L/min to help gas velocity, and the long wave time of integration is 5s, and the shortwave time of integration is 10s, and integral number of times is 2 times, spectrum room temperature
Spend for 38 DEG C.
Table 9：Trace element detection wavelength to be measured in embodiment 2：
By blank reagent solution METHOD FOR CONTINUOUS DETERMINATION 10 times, 3 calculating are multiplied by with the standard deviation average values of 10 measure, are treated
The method detection limit of micrometer secondary element is as shown in table 10：
Table 10：Trace element method detection limit to be measured in embodiment 3
Sample detection lower limit=method detection limit+blank content, only when micronutrient levels to be measured etc. in blank solution
When 0, sample detection lower limit is equal to method detection limit, if micronutrient levels to be measured is not equal to 0 in blank solution, sample detection
Lower limit detects limit for height with regard to ratio method.
The selection criteria addition method in test software, four parts of standard working curve solution are tested respectively, measure sky
Micronutrient levels to be measured in white solution：
Table 11：Micronutrient levels to be measured in 3 blank solution of embodiment
Table 12：Trace element detection lower limit to be measured in embodiment 3
Known by table 12：Iron tramp Monitoring lower-cut is 9.08ppm, i.e., 0.0009% in this method chromium powder, under aluminium defects inspecting
5.20ppm, i.e., 0.0005% are limited to, reduces more than 100 times than document report iron, aluminium element Monitoring lower-cut 0.10%, detection
Sensitivity is considerably higher.
Embodiment 4
Precision test
Five parts of No. 2 each 0.2000g of chromium powder sample of parallel weighing, handle No. 2 samples by 2 method and step of embodiment, carry out essence
Density Detection, detection data are as shown in table 13：
Table 13：4 Precision Experiment of embodiment detects data
Embodiment 5
Mark-on reclaims are tested
No. 2 chromium powder samples are selected, are quantitatively adding standard solution to be measured, carry out mark-on reclaims experiment, testing result is shown in Table 14
It is shown：
Table 14：Recovery testu testing result in implementing 5
It was found from table 13 and table 14：Detection method provided by the invention, precision and the rate of recovery are good, meet detection and analysis
It is required that with higher practicality and it is widely applied prospect.
In general, the inductively coupled plasma emission spectrography measure chromium powder in nickel, manganese, iron, zinc, calcium, magnesium, aluminium,
Titanium, vanadium, the detection method of cobalt, easy, quick, easy to operate, the analysis suitable for batch production detects.
Those of ordinary skill in the art will understand that the embodiments described herein, which is to help reader, understands this hair
Bright principle, it should be understood that protection scope of the present invention is not limited to such special statement and embodiment.This area
Those of ordinary skill these disclosed technical inspirations can make according to the present invention and various not depart from the other each of essence of the invention
The specific deformation of kind and combination, these deform and combine still within the scope of the present invention.
Claims (9)
- A kind of 1. micro- detection method in chromium powder, it is characterised in that：On inductively coupled plasma atomic emission spectrometer, the matching detection condition of selection criteria serial solution and each to be measured The matching detection wavelength of trace element, detection contain micro- chromium matrix standard serial solution to be measured, obtain to be measured micro The standard working curve of concentration of element-the intensity of spectral line；On inductively coupled plasma atomic emission spectrometer, by standard serial solution matching detection condition and respectively treat micrometer The matching detection wavelength of secondary element, detects sample solution, obtains corresponding the intensity of spectral line of trace element to be measured in sample solution；Determined according to corresponding the intensity of spectral line of trace element to be measured in the standard working curve and sample solution of acquisition in sample solution Micronutrient levels to be measured.
- 2. micro- detection method in chromium powder according to claim 1, it is characterised in that：The sample solution is by salt Acid dissolves by heating chromium powder sample preparation and forms.
- 3. micro- detection method in chromium powder according to claim 1, it is characterised in that：Specifically include following step Suddenly：S1：Draw standard working curveS11：Prepare chromium matrix standard serial solutionWeigh high-purity 0.1~0.4g of chromium powder, add 20~40mL of hydrochloric acid, heated under the conditions of 200~400 DEG C of temperature, High Pure Chromium After powder is completely dissolved, cooling, adds micro- normal storage solution to be measured, solution is diluted to volumetric flask scale with water, It is configured to the chromium matrix standard serial solution that each trace element to be measured is respectively provided with appropriate gradient；S12：Detect chromium matrix standard serial solutionOpen inductively coupled plasma atomic emission spectrometer, the matching detection condition of selection criteria serial solution and each to be measured The matching detection wavelength of trace element, micro- the intensity of spectral line to be measured in sequentially determining chromium matrix standard serial solution；S13；Obtain standard working curveStandard working curve is drawn, and carries out background correction according to micro- concentration to be measured, the intensity of spectral line；S2：Measure micronutrient levels to be measuredS21：Prepare sample solutionWeigh chromium powder 0.1~0.4g of sample, add 20~40mL of hydrochloric acid, heated under the conditions of 200~400 DEG C of temperature, chromium powder sample After product are completely dissolved, cooling, is diluted with water to volumetric flask scale, is configured to sample solution；S22：Detect sample solutionUnder the operating condition identical with drawing standard working curve, micro- spectral line to be measured is strong in determination sample solution Degree, computer automatically determine micro- content to be measured in sample solution according to standard working curve.
- 4. micro- detection method in chromium powder according to claim 3, it is characterised in that：The hydrochloric acid is top pure grade Hydrochloric acid, the water are pure water.
- 5. according to detection method micro- in any chromium powders of claim 1-4, it is characterised in that：It is described to treat micrometer Secondary element includes nickel, manganese, iron, zinc, calcium, magnesium, aluminium, titanium, vanadium, cobalt.
- 6. micro- detection method in chromium powder according to claim 5, it is characterised in that：Micro- mark to be measured Quasi- storage solutions include the standard solution 1 that is configured to by nickel, manganese, zinc, calcium, magnesium, titanium, cobalt single element normal storage solution and/or The standard solution 2 being configured to by iron, aluminium, vanadium single element normal storage solution.
- 7. micro- detection method in chromium powder according to claim 5, it is characterised in that：It is selected each to be measured micro The matching detection wavelength of element is：Nickel is 216.556nm, manganese 257.610nm, iron 259.940nm, zinc 213.856nm, Calcium is 184.006nm, magnesium 279.553nm, aluminium 167.079nm, titanium 337.280nm, vanadium 292.402nm, cobalt are 230.786nm。
- 8. according to detection method micro- in any chromium powders of claim 1-4, it is characterised in that：The inductance coupling Plasma atomic emission spectrometer is closed, testing conditions are：Using horizontal observed pattern, RF incident powers are 1150~1350W, Nebulizer gas 0.2~1.5L/min of flow, it is 50~100rpm to rinse pump speed and analysis pump speed, washing time for 10~ 40s, secondary air speed are 0.5~1.5L/min, and flow rate of carrier gas is 0.5~1.0L/min, the long and short ripple time of integration for 5~ 30s, integral number of times are 2~4 times, and spectrum room temperature is 37.9~38.1 DEG C.
- 9. micro- detection method in chromium powder according to claim 8, it is characterised in that：Described inductive coupling etc. from Daughter atom emission spectrometer, testing conditions are：Using horizontal observed pattern, RF incident powers are 1150W, nebulizer gas stream 0.6L/min is measured, it is 50rpm to rinse pump speed and analysis pump speed, and washing time 30s, secondary air speed is 0.5L/min, long The ripple time of integration is 5s, and the shortwave time of integration is 10s, and integral number of times is 2 times, and spectrum room temperature is 38 DEG C.
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