CN105466909A - Method for fast quantitative analysis for six-element content in powder metallurgy - Google Patents
Method for fast quantitative analysis for six-element content in powder metallurgy Download PDFInfo
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Abstract
A method for a fast quantitative analysis for six-element content in powder metallurgy comprises sample deoiling, reagent preparing, test material weighing, front processing dissolving, diluting, wavelength selecting, serial standard solution preparing, fast detection by an inductive coupling plasma atomic emission spectrometry and calculating of an analysis result and precision. The method solves the technical problem of the fast quantitative analysis for the content of six elements of copper, tin, zinc, lead, cobalt and chrome in the powder metallurgy, establishes the inductive coupling plasma atomic emission spectrometry to detect the content of the six elements of copper, tin, zinc, lead, cobalt and chrome in the powder metallurgy, ensures the product quality, improves the production efficiency and reduces the production cost.
Description
Technical field
The present invention relates to hexa-atomic cellulose content quick quantitative analytic method in a kind of powder metallurgy, particularly the inductively coupled plasma atomic emission spectrum quick quantitative analytic method of copper, tin, zinc, lead, cobalt, chromium amount in a kind of powder metallurgy.
Background technology
Powder metallurgy refers to metal powder (or potpourri of metal powder and non-metal powder) as raw material, through being shaped and sintering the technological process manufacturing metal material, compound substance and all kinds goods.Powder metallurgy is very widely in the scope of solution Material Field problem.Powder metallurgy has superiority technically and economically, and the application risen in national economy is more and more wider.Can say do not have now which industrial sector not use powder metallurgy and goods.Through consulting, there are GB/T4309-2009 powdered metallurgical material classification and trade mark method for expressing, GB/T2688-2012 sliding bearing sintered metal powder bearing technical conditions.There is the content regulation of the chemical composition such as chemical combination C, total C, Cu, Sn, Zn, Pb in GB/T2688-2012, also specify oil content simultaneously.Its content is (%): chemical combination C0 ~ 1.0; Total C0 ~ 3.5; Cu0 ~ 40.0; Sn1.5 ~ 10.5; Zn≤7.0; Pb2 ~ 5.Specify the methods analyst that its chemical composition specifies according to GB/T223.But, carry out the problem detected after whether deoiling, do not describe clear in its technical conditions, also not mentioned in GB/T223 standard method of analysis.In addition, in GB/T223, measurement range: Cu0.005% ~ 2.63%, Sn0.0009% ~ 0.20%, Zn0.0005% ~ 0.05%, Pb0.0005% ~ 0.25%, Co0.010% ~ 30.00%, can not meet the quick testing requirement of multielement content in powder metallurgy (Cu1.00% ~ 40.00%, Sn1.00% ~ 15.00%, Zn1.00% ~ 7.00%, Pb1.00% ~ 8.00%, Co0.50% ~ 10.00%).Do not find hexa-atomic cellulose content quick quantitative analytic method in powder metallurgy.In addition, in company standard method, do not find relevant applicable detection method yet.At present, as the exploitation of copper, tin, zinc, lead, cobalt, chromium content quick quantitative analytic method in powder metallurgy, still belong to blank.
Summary of the invention
Object of the present invention is exactly the deficiency in order to overcome above-mentioned background technology, hexa-atomic cellulose content quick quantitative analytic method in a kind of powder metallurgy is provided, in the method, test portion is after oil removing, hydrochloric acid solution and salpeter solution or cosolvent solution, mixture of sulfuric phosphoric acid solubilize, certain volume is diluted to secondary and other water of higher level, on inductively coupled plasma atomic emission spectrometer, measure the emitted luminescence intensity of element to be measured in test solution in recommended wavelength or other suitable wavelength places, calculated the massfraction of element to be measured by calibration curve.
Hexa-atomic cellulose content quick quantitative analytic method in a kind of powder metallurgy of the present invention, comprises sample oil removing, preparation of reagents, test portion takes, pre-treatment is dissolved, dilutes, wavelength chooses, series standard solution preparation, ICP-AES detect fast, the calculating of analysis result and precision.
Beneficial effect of the present invention:
In a kind of powder metallurgy of the present invention, hexa-atomic cellulose content quick quantitative analytic method has following features:
1. establish the quick quantitative analytic method of ICP-AES to copper, tin, zinc, lead, cobalt, chromium amount in powder metallurgy;
2. measurement range (without oil base):
Element | Massfraction w B/% | Element | Massfraction w B/% |
Cu | 1.00~40.00 | Pb | 1.00~8.00 |
Sn | 1.00~15.00 | Co | 0.50~10.00 |
Zn | 1.00~7.00 | Cr | 0.50~5.00 |
Specify that the massfraction of element to be measured be with oil removing after butt be as the criterion and carry out calculating.
3. precision:
Accompanying drawing explanation
Fig. 1 is the sample solution constitutional diagram after pre-treatment of the present invention;
Fig. 2 is the instrument and equipment figure of use of the present invention.
Embodiment
Below with reference to drawings and Examples, the present invention is described in detail.
Embodiment
Hexa-atomic cellulose content quick quantitative analytic method in a kind of powder metallurgy involved by the present embodiment, its step is as follows:
Step one: oil removing
The oil removing of parts lab scale exemplar, that parts lab scale exemplar to be placed in temperature be that the high temperature resistance furnace calcination 1h of 600 DEG C is to eliminating oily substance, or the appropriate powder metallurgy sample bits shape sample drilled through is placed in 250mL beaker, about 2h is soaked with absolute ethyl alcohol or acetone or ether equal solvent, and shake up at any time, after using up solvent, with low-temperature furnace heating, drying, be cooled to room temperature;
Step 2: pre-treatment
With ten thousand/electronic balance, take 0.1000g test portion, be placed in 150mL conical flask, in the conical flask being loaded with powder metallurgy test portion, add 15mL hydrochloric acid solution, 15mL salpeter solution or 2mL cosolvent solution, 10mL mixture of sulfuric phosphoric acid solution, low-temperature heat to test portion dissolves completely, then be heated to emit sulfuric acid cigarette, drip about 2mL nitric acid immediately, with destructive Carbide, take off cooling, be dissolved in water and be cooled to room temperature, the sample solution of room temperature will be cooled to after pre-treatment dissolution process, be transferred in 100mL volumetric flask, in transfer process, insert in volumetric flask with a glass bar, conical flask bottleneck tilts near glass bar, solution is slowly flowed into along glass bar, glass bar lower end will near bottleneck inwall, but not too close bottleneck, in order to avoid there is solution to overflow, after solution stream is complete, by conical flask along glass bar slightly toward on carry, simultaneously upright, a solution of attachment conical flask oral area is made to flow back in beaker, remain in a little solution in conical flask, with other washing of a small amount of secondary higher level 3 ~ 4 times, cleansing solution is transferred in volumetric flask as stated above, after solution proceeds to volumetric flask, add other water of secondary higher level, be diluted to about 3/4 volume time, volumetric flask yawing (is sure not reversing shake) several times, do preliminary mixing, then continue to add other water of secondary higher level, dropwise add carefully during nearly graticule, until the lower meniscus of solution and graticule tangent till, cover tightly glass stopper,
Left index finger pins stopper, and right hand finger tip withstands a bottle feather edge, and, then, make bubble rise to top the other way around the other way around by volumetric flask and wholely to swing, 10 times so repeatedly ~ 15 times, can mix, the sample solution state after pre-treatment as shown in Figure 1;
Step 3: instrument condition of work is optimized
The instrument and equipment used as shown in Figure 2, is optimized instrument condition of work according to instrument instructions, selects suitable measuring condition, as argon pressure, observed altitude, analytical line, flush time, integral time etc.;
Utilize PridigyXP type inductively coupled plasma atomic emission spectrometer, the optimization measuring condition of selection is as recommended work parameter:
RF power: 1.1kW; Atomization gas pressure: 0.2MPa (30PSI); Cooling gas flow: 20L/min; Plasmatorch observed altitude: 15mm; Flush time: 30s; Integral time: 10s; Purity of argon: be not less than 99.99%;
Step 4: determined wavelength is selected
After instrument condition of work being optimized according to instrument instructions, in element determination wavelength spectral line, consider according to sensing range, linear relationship, the recovery, testing result accuracy, select suitable mensuration wavelength; Selected mensuration wavelength is:
Element | Wavelength/nm | Element | Wavelength/nm |
Cu | 324.754;224.700 | Pb | 220.353;217.000 |
Sn | 189.991;235.484 | Co | 228.615;236.379 |
Zn | 213.856;206.200 | Cr | 206.149;267.716 |
Step 5: testing result is collected
Operate according to PridigyXP type inductively-coupled plasma spectrometer working specification, detect the content of element to be measured in sample solution; Record testing result, carries out next step analysis;
Step 6: addition method is verified
According to the analytical approach optimal conditions selected, according to standard addition method, make recovery test;
Step 7: synthetic standard sample is verified
(1) synthetic standard sample
The synthetic standard sample element addition of 3 powder metallurgy is in table 1:
Table 1 synthetic standard sample element addition
(2) calibration curve preparation
In calibration curve solution, the content outline of element to be measured is higher than the content of this element in sample.The quantity of calibration curve solution is determined by precision requirement, and general (3 ~ 5) are individual, draws the standard solution of calibration curve in table 2:
The standard solution of calibration curve drawn by table 2
(3) measure
A. instrument prepares
Open ICP spectrometer, more than preheating 2h;
According to instrument instructions, instrument condition of work is optimized, selects suitable measuring condition, as argon pressure, observed altitude, analytical line, flush time, integral time etc.;
Prepare the softwares such as calibration curve drafting, measurement and statistical computation;
Click plasmatorch is lighted a fire, and confirms that instrument operational factor is in normal range after igniting, atomization system and plasma torch working properly, stablize more than 15min;
B. the measurement of series of calibration curve solution and the drafting of calibration curve
On inductive coupling plasma emission spectrograph, measure the spectral intensity of serial calibration curve solution beryllium, each solution duplicate measurements 2 times ~ 3 times, calculates its mean value; Deduct zero-dose spectral intensity mean value for ordinate with each spectral intensity mean value, the concentration of series of calibration curve solution is horizontal ordinate, draws the calibration curve of beryllium respectively;
Calculate the related coefficient of calibration curve, related coefficient should be greater than more than 0.999;
C. the mensuration of sample solution
Measure the spectral intensity in sample solution, duplicate measurements 2 times ~ 3 times, calculates its mean value; The mean value that its spectral intensity mean value deducts blank solution spectral intensity is clean spectral intensity;
(4) calculating of analysis result
According to calibration curve, clean spectral intensity is converted into the mass concentration of element to be measured in sample solution, represents with mg/mL;
In test portion, copper, tin, zinc, lead, cobalt, chromium amount are with massfraction w
bmeter, calculates by formula (1):
In formula:
ρ
b---the numerical value of the mass concentration of element to be measured in test solution, unit is milligram every milliliter (mg/mL);
The numerical value that V---tested liquid is long-pending, unit is milliliter (mL);
M---the numerical value of test portion quality, unit is gram (g);
Step 8: content inspection
1. for the standard addition method inspection of low content
According to the optimal conditions selected, according to standard addition method, make recovery test, the recovery=(measuring resultant-test portion content)/addition × 100%; General provision requires that the recovery is 95% ~ 105%, and the present embodiment recovery is 98.50% ~ 102.0%, see table 3, this detection method measurement result is described accurately and reliably;
Table 3 recovery test result
2. for the synthetic standard sample inspection of high-load
Carry out verification operation (iron-holder is 0.1000g) by the mode synthetic standard sample of implementation step seven, its evaluation, in table 4, illustrates this detection method measurement result accurately and reliably;
Table 4 synthetic standard sample evaluation
3. produce examination and analyses result
Utilize hexa-atomic cellulose content quick quantitative analytic method in a kind of powder metallurgy, carried out detection and precision test to sample to be tested, it produces examination and analyses result see table 5, and from table 5, analysis result of the present invention accurately and reliably.
Examination and analyses result produced by table 5
The present embodiment shows that method of the present invention solves the fast quantitative analysis technical matters of 6 constituent contents such as the plumbous cobalt chromium of Cu-Sn-Zn in powder metallurgy, establishes ICP-AES and to detect in powder metallurgy 6 constituent contents such as the plumbous cobalt chromium of Cu-Sn-Zn; For the further research of powder metallurgy novel product in the industry fields such as machinery, to improve the quality of products in process of production, production efficiency, reduction production cost, provide solid foundation; For the quick and precisely quantitative test of 6 constituent contents such as the plumbous cobalt chromium of Cu-Sn-Zn in powder metallurgy, provide foundation; Reach the deposit object of chemical fundamentals detection technique exploitation, also can be used as the technical support that new standard is formulated simultaneously.
Claims (1)
1. a hexa-atomic cellulose content quick quantitative analytic method in powder metallurgy, its step is as follows:
Step one: oil removing
The oil removing of parts lab scale exemplar, that parts lab scale exemplar to be placed in temperature be that the high temperature resistance furnace calcination 1h of 600 DEG C is to eliminating oily substance, or the appropriate powder metallurgy sample bits shape sample drilled through is placed in 250mL beaker, about 2h is soaked with absolute ethyl alcohol or acetone or ether equal solvent, and shake up at any time, after using up solvent, with low-temperature furnace heating, drying, be cooled to room temperature;
Step 2: pre-treatment
With ten thousand/electronic balance, take 0.1000g test portion, be placed in 150mL conical flask, in the conical flask being loaded with powder metallurgy test portion, add 15mL hydrochloric acid solution, 15mL salpeter solution or 2mL cosolvent solution, 10mL mixture of sulfuric phosphoric acid solution, low-temperature heat to test portion dissolves completely, then be heated to emit sulfuric acid cigarette, drip about 2mL nitric acid immediately, with destructive Carbide, take off cooling, be dissolved in water and be cooled to room temperature, the sample solution of room temperature will be cooled to after pre-treatment dissolution process, be transferred in 100mL volumetric flask, in transfer process, insert in volumetric flask with a glass bar, conical flask bottleneck tilts near glass bar, solution is slowly flowed into along glass bar, glass bar lower end will near bottleneck inwall, but not too close bottleneck, in order to avoid there is solution to overflow, after solution stream is complete, by conical flask along glass bar slightly toward on carry, simultaneously upright, a solution of attachment conical flask oral area is made to flow back in beaker, remain in a little solution in conical flask, with other washing of a small amount of secondary higher level 3 ~ 4 times, cleansing solution is transferred in volumetric flask as stated above, after solution proceeds to volumetric flask, add other water of secondary higher level, be diluted to about 3/4 volume time, volumetric flask yawing (is sure not reversing shake) several times, do preliminary mixing, then continue to add other water of secondary higher level, dropwise add carefully during nearly graticule, until the lower meniscus of solution and graticule tangent till, cover tightly glass stopper,
Left index finger pins stopper, and right hand finger tip withstands a bottle feather edge, and, then, make bubble rise to top the other way around the other way around by volumetric flask and wholely to swing, 10 times so repeatedly ~ 15 times, can mix, the sample solution state after pre-treatment as shown in Figure 1;
Step 3: instrument condition of work is optimized
According to instrument instructions, instrument condition of work is optimized, selects suitable measuring condition, as argon pressure, observed altitude, analytical line, flush time, integral time etc.;
Utilize PridigyXP type inductively coupled plasma atomic emission spectrometer, the optimization measuring condition of selection is as recommended work parameter:
RF power: 1.1kW; Atomization gas pressure: 0.2MPa (30PSI); Cooling gas flow: 20L/min; Plasmatorch observed altitude: 15mm; Flush time: 30s; Integral time: 10s; Purity of argon: be not less than 99.99%;
Step 4: determined wavelength is selected
After instrument condition of work being optimized according to instrument instructions, in element determination wavelength spectral line, consider according to sensing range, linear relationship, the recovery, testing result accuracy, select suitable mensuration wavelength; Selected mensuration wavelength is:
Step 5: testing result is collected
Operate according to PridigyXP type inductively-coupled plasma spectrometer working specification, detect the content of element to be measured in sample solution; Record testing result, carries out next step analysis;
Step 6: addition method is verified
According to the analytical approach optimal conditions selected, according to standard addition method, make recovery test;
Step 7: synthetic standard sample is verified
(1) synthetic standard sample
The synthetic standard sample element addition of 3 powder metallurgy is in table 1:
Table 1 synthetic standard sample element addition
(2) calibration curve preparation
In calibration curve solution, the content outline of element to be measured is higher than the content of this element in sample.The quantity of calibration curve solution is determined by precision requirement, and general (3 ~ 5) are individual, draws the standard solution of calibration curve in table 2:
The standard solution of calibration curve drawn by table 2
(3) measure
A. instrument prepares
Open ICP spectrometer, more than preheating 2h;
According to instrument instructions, instrument condition of work is optimized, selects suitable measuring condition, as argon pressure, observed altitude, analytical line, flush time, integral time etc.;
Prepare the softwares such as calibration curve drafting, measurement and statistical computation;
Click plasmatorch is lighted a fire, and confirms that instrument operational factor is in normal range after igniting, atomization system and plasma torch working properly, stablize more than 15min;
B. the measurement of series of calibration curve solution and the drafting of calibration curve
On inductive coupling plasma emission spectrograph, measure the spectral intensity of serial calibration curve solution beryllium, each solution duplicate measurements 2 times ~ 3 times, calculates its mean value; Deduct zero-dose spectral intensity mean value for ordinate with each spectral intensity mean value, the concentration of series of calibration curve solution is horizontal ordinate, draws the calibration curve of beryllium respectively;
Calculate the related coefficient of calibration curve, related coefficient should be greater than more than 0.999;
C. the mensuration of sample solution
Measure the spectral intensity in sample solution, duplicate measurements 2 times ~ 3 times, calculates its mean value; The mean value that its spectral intensity mean value deducts blank solution spectral intensity is clean spectral intensity;
(4) calculating of analysis result
According to calibration curve, clean spectral intensity is converted into the mass concentration of element to be measured in sample solution, represents with mg/mL;
In test portion, copper, tin, zinc, lead, cobalt, chromium amount are with massfraction w
bmeter, calculates by formula (1):
In formula:
ρ
b---the numerical value of the mass concentration of element to be measured in test solution, unit is milligram every milliliter (mg/mL);
The numerical value that V---tested liquid is long-pending, unit is milliliter (mL);
M---the numerical value of test portion quality, unit is gram (g);
Step 8: content inspection
1. for the standard addition method inspection of low content
According to the optimal conditions selected, according to standard addition method, make recovery test, the recovery=(measuring resultant-test portion content)/addition × 100%; General provision requires that the recovery is 95% ~ 105%, and the present embodiment recovery is 98.50% ~ 102.0%, see table 3, this detection method measurement result is described accurately and reliably;
Table 3 recovery test result
2. for the synthetic standard sample inspection of high-load
Carry out verification operation (iron-holder is 0.1000g) by the mode synthetic standard sample of implementation step seven, its evaluation, in table 4, illustrates this detection method measurement result accurately and reliably;
Table 4 synthetic standard sample evaluation
3. produce examination and analyses result
Utilize hexa-atomic cellulose content quick quantitative analytic method in a kind of powder metallurgy, carried out detection and precision test to sample to be tested, it produces examination and analyses result see table 5, and from table 5, analysis result of the present invention accurately and reliably.
Examination and analyses result produced by table 5
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CN106596516A (en) * | 2016-11-09 | 2017-04-26 | 重庆长安工业(集团)有限责任公司 | Method of measuring trace lead content of tin bronze by means of standard addition-ICP atomic emission spectrometer |
CN108375640A (en) * | 2018-05-03 | 2018-08-07 | 北京农业质量标准与检测技术研究中心 | A method of heavy metal chromium form in mushroom is extracted based on tube furnace |
CN108918508A (en) * | 2018-07-25 | 2018-11-30 | 重庆长安工业(集团)有限责任公司 | The measuring method of high content iron in a kind of tin bronze |
CN110823867A (en) * | 2019-10-14 | 2020-02-21 | 重庆长安工业(集团)有限责任公司 | Analysis method for multi-element content in tin-lanthanum-cerium intermediate alloy |
CN110823865A (en) * | 2019-10-12 | 2020-02-21 | 重庆长安工业(集团)有限责任公司 | Method for measuring high-content antimony in tin foil |
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CN106596516A (en) * | 2016-11-09 | 2017-04-26 | 重庆长安工业(集团)有限责任公司 | Method of measuring trace lead content of tin bronze by means of standard addition-ICP atomic emission spectrometer |
CN108375640A (en) * | 2018-05-03 | 2018-08-07 | 北京农业质量标准与检测技术研究中心 | A method of heavy metal chromium form in mushroom is extracted based on tube furnace |
CN108375640B (en) * | 2018-05-03 | 2021-05-25 | 北京农业质量标准与检测技术研究中心 | Method for extracting form of heavy metal chromium in mushroom based on tube furnace |
CN108918508A (en) * | 2018-07-25 | 2018-11-30 | 重庆长安工业(集团)有限责任公司 | The measuring method of high content iron in a kind of tin bronze |
CN110823865A (en) * | 2019-10-12 | 2020-02-21 | 重庆长安工业(集团)有限责任公司 | Method for measuring high-content antimony in tin foil |
CN110823867A (en) * | 2019-10-14 | 2020-02-21 | 重庆长安工业(集团)有限责任公司 | Analysis method for multi-element content in tin-lanthanum-cerium intermediate alloy |
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