CN1900698A - Method for analyzing flexible line components - Google Patents
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- CN1900698A CN1900698A CN 200510046889 CN200510046889A CN1900698A CN 1900698 A CN1900698 A CN 1900698A CN 200510046889 CN200510046889 CN 200510046889 CN 200510046889 A CN200510046889 A CN 200510046889A CN 1900698 A CN1900698 A CN 1900698A
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Abstract
Characters of the method are that first removing organic substances; next, using aqua regia to dissolve sample of material processed above; then, driving away acids in low melting point; using method of inductive coupling plasma atomic emission spectroscopy (ICP-AES) to analyze other components in the solution processed above. Features are: high adaptability less investment, easy of analysis, high accuracy.
Description
The technical field is as follows:
the invention relates to material science, and particularly provides a component analysis method for a flexible wire.
Background art:
flexible wire is an important material for spray coating soft strips, and therefore, accurate analysis of the composition of such materials is of considerable necessity and importance. Such materials include metal components (metal powder) and non-metal components (organic forming agents), and currently, there is no good analysis method in the prior art, and a corresponding flexible wire analysis method with low investment, simple and convenient analysis and accurate result is desired.
The invention content is as follows:
the invention aims to provide a component analysis method for a flexible wire.
The invention discloses a method for analyzing components of a flexible wire, which is characterized by comprising the following steps: firstly, removing organic substances (because a sample contains metal powder and an organic forming agent, in order to facilitate accurate analysis, organic components and inorganic components must be effectively separated), then dissolving the material sample subjected to the treatment by using aqua regia, then removing low-melting-point acid, and analyzing other components in the solution subjected to the treatment by using an inductively coupled plasma atomic emission spectrometry (ICP-AES method): and testing the treated sample by using an inductively coupled plasma emission spectrometer, measuring the spectral line intensity of each element to be tested, and fitting according to the relation between the spectral line intensity and the element content to obtain the element content to be tested.
The invention relates to a component analysis method of a flexible wire, which is characterized by comprising the following steps: the flexible wire (which is a mixed material composed of organic matters and inorganic matters) comprises the following two components in parts by weight:
the first material: the flexible wire material is composed of a certain amount of organic forming agent (the mass percentage content range of the organic forming agent in the total mass of the flexible wire material is usually 7-15%, and the preferable range is 8-12%) and Ni, Al, Cr, W, synthetic ruby, Mo, Ti, Co and Cu, wherein the relative mass parts of the other components except the organic forming agent are as follows: ni: 27 to 33; al: 8.0-13.0; cr is less than or equal to 1.5; w is less than or equal to 1.5; synthesizing ruby: 39.0 to 44.0; total amount of Mo, Ti, Co, Cu: less than or equal to 5; wherein the contents of Mo, Ti, Co and Cu are actually measured;
the second material: the flexible wire material is composed of a certain amount of organic forming agent (the mass percentage content range of the organic forming agent in the total mass of the flexible wire material is usually 7-15%, and the preferable range is 8-12%) and Ni, Al, Cr, W, Mo, Ti, Co and Cu, wherein the relative mass content parts of the other components except the organic forming agent are as follows: ni: 52-57; al: 15.0 to 18.0; w is less than or equal to 2.0; total amount of Cr, Mo, Ti, Co, Cu: less than or equal to 8; wherein the contents of Cr, Mo, Ti, Co and Cu are measured.
The invention relates to a component analysis method of a flexible wire, which is characterized by comprising the following steps: the method for removing the organic matters comprises the steps of adding concentrated sulfuric acid into a sample, and heating at a low temperature until the sample is carbonized and decomposed. The carbonization property of concentrated sulfuric acid can be utilized to separate organic matters from inorganic matters. The reaction formula is as follows:
in the carbonization of the organic forming agent, the degree of heating with sulfuric acid was tested:
adding equal amount of concentrated sulfuric acid into four equal amount of samples, heating in an electric furnace, adding aqua regia for dissolution, and analyzing the data of the synthesized ruby by specific temperature, time, dissolution condition and weight method as shown in Table 1:
TABLE 1 influence of heating degree of sulfuric acid
| Serial number | Heating of Temperature of | Degree of heating | Adding aqua regia for dissolution | Synthetic Hongbao Stone% | Al(％) | Cr(％) |
| 1 | Low temperature | Removing the tobacco when smoking a little smoke | Excessive organic floating matter after sample dissolution | 43.0 | 10.84 | 1.25 |
| 2 | Low temperature | Removing the smoke when the dense smoke is emitted | Less organic floating substances after the sample is dissolved | 42.6 | 11.09 | 1.27 |
| 3 | High temperature | Removing the tobacco when smoking a little smoke | Due to the high temperature, the sampleThe cigarette is quickly smoked, and the smoke is quickly smoked, presence of bulk sample | |||
| 4 | High temperature | Removing the smoke when the dense smoke is emitted | No organic floating matter after the sample is dissolved | 33.4 | 19.71 | 2.30 |
The above experimental phenomena and analytical data illustrate that: under the high temperature state, the smoke with concentrated sulfuric acid (338 ℃) decomposes partial synthesized ruby, the analysis result is obviously lower, and the micro smoke sample can not be decomposed completely; only low temperature fuming had little effect on the analysis results.
The invention relates to a component analysis method of a flexible wire, which is characterized by comprising the following steps:
the process of dissolving the flexible wire by the aqua regia is as follows:
the aqua regia used for dissolving the flexible wire rod is mixed with concentrated hydrochloric acid and concentrated nitric acid in a ratio of (1-5) to 1. The preferred scheme is as follows: firstly, dissolving a sample subjected to organic matter removal treatment in hydrochloric acid, and then adding nitric acid into the solution; the preferred range of the aqua regia ratio is concentrated hydrochloric acid to concentrated nitric acid (2-4) to 1.
A comparative test was performed for dissolution of the following samples: the sample subjected to organic matter removal treatment was dissolved by adding appropriate amounts of hydrochloric acid, nitric acid, and aqua regia (each amount is 10ml, each 0.1g) to 3 portions, respectively. The details are shown in Table 2:
TABLE 2 dissolution of sample
| Serial number | Reagent | Dissolution behavior | Dissolved sample All have pink color Appearance of insoluble matter |
| 1 | Hydrochloric acid | Slow dissolution | |
| 2 | Nitric acid | Slow dissolution | |
| 3 | Aqua regia (3+1) | Rapidly decompose |
As can be seen from the above table, the addition of aqua regia can rapidly decompose the decomposed sample, but the hydrochloric acid should be slowly added first, and then the nitric acid should be added, so as to avoid violent reaction overflow.
The invention relates to a component analysis method of a flexible wire, which is characterized by comprising the following steps: after the material is dissolved by aqua regia and before low-melting-point acid is driven to the full, hydrofluoric acid is added into the solution to remove silicon, so that the interference of silicon in the sample is eliminated, and the subsequent measurement of various alloy elements to be measured is conveniently carried out. Silicon with SiF4Gaseous stateThe form was drained off, separated from the solution phase.
Influence of organic Forming Agents:
because the organic forming agent contains a small amount of silicon besides organic components, the silicon is often formed into a silicic acid colloid in the synthetic ruby precipitate in the sulfuric acid carbonization and fuming processes, and silicon dioxide is formed after ashing, so that the synthetic ruby result is obviously higher. The effect is now eliminated by adding hydrofluoric acid to gasify the silica. The reaction equation is as follows:
the specific operation is shown in table 3:
TABLE 3 hydrofluoric acid addition Table
| Medium | Container with a lid | Synthetic ruby |
| H2SO4HF5ml is added during carbonization | Polytetrafluoroethylene beaker | 39.3 |
| HF5ml is added in the dissolving process of aqua regia | 39.8 | |
| Adding 1ml H after ashing2SO4+HF5ml | Platinum crucible | 38.2 |
In concentrated sulfuric acid fuming medium, hydrofluoric acid can decompose part of synthesized ruby, so that the analysis result is lower. Therefore, hydrofluoric acid should be added during the dissolution of aqua regia and removed after slight smoking, and the result is satisfactory.
The invention relates to a component analysis method of a flexible wire, which is characterized by comprising the following steps: after dissolving the material with aqua regia and before driving off the low melting acid, phosphoric acid was added to the solution to complex W. Because the sample contains a small amount of tungsten element, tungstic acid precipitation is easily generated in a concentrated acid state, and the analysis results of tungsten and synthetic ruby are influenced, so a small amount of phosphoric acid is added to complex the tungsten element after the sample is dissolved by aqua regia. The following is the effect of phosphoric acid on the results of the tungsten element analysis, as shown in table 4:
TABLE 4 influence of the addition of phosphoric acid on the results of the analysis of the tungsten element
| Dissolution process | Analysis result of W | Synthetic ruby |
| After the sample was dissolved, 1ml of phosphoric acid and fuming sulfuric acid were added. | 0.53 | 39.1 |
| After the sample is dissolved, no phosphoric acid is added, and slight smoke of sulfuric acid is generated. | 0.10 | 43.0 |
The above table shows that the addition of phosphoric acid can make the analysis result of tungsten accurate.
The invention relates to a component analysis method of a flexible wire, which is characterized by comprising the following steps: filtering the first material before removing the low-melting-point acid to obtain a solid precipitate with synthetic ruby as a main component; the obtained precipitate is washed until the filtrate is neutral, then the precipitate is placed in a crucible (preferably a crucible which is resistant to a high temperature of 1000 ℃ or higher, preferably a porcelain crucible of constant weight in advance), ashed in a high temperature furnace at about 800 ℃ or higher (preferably 1000 ℃) to eliminate the influence of the filter paper, then washed again, taken out, placed in a dryer, cooled and weighed.
Because the main component of the synthetic ruby is α alumina, which contains a small amount of chromium metal and is chemically inert and almost non-reactive with all reagents, the synthetic ruby can be analyzed by weight (weighing after solid-liquid separation) using this property.
In the formula, G: the sample is heavy; g1: the crucible is heavy; g2: the crucible and the precipitate are heavy.
The invention relates to a component analysis method of a flexible wire, which is characterized by comprising the following steps: the process for driving off the low-melting-point acid is as follows: phosphoric acid was added to the solution and heated until slight smoke was emitted. Since phosphoric acid has a strong dissolving power at a high temperature and can dissolve many substances which have been considered to be insoluble in acid, controlling the temperature after adding phosphoric acid is of great significance for the analysis result. The media were added according to the following table and the analytical results are shown in table 5:
TABLE 5 influence of phosphoric acid addition sequence on analysis results
| Serial number | Media addition sequence | Synthetic Red Gem (Gem) | Al | Cr | W |
| 1 | Sulfuric acid + phosphoric acid, fuming, adding Aqua regia and fuming | 41.6 | 11.84 | 1.38 | 0.50 |
| 2 | Sulfuric acid, fuming, adding aqua regia, fuming, boiling with phosphoric acid | 42.6 | 11.72 | 1.28 | 0.49 |
| 3 | Sulfuric acid, fuming, adding aqua fortis + Phosphoric acid, fuming | 42.4 | 10.84 | 1.28 | 0.50 |
| 4 | Sulfuric acid, fuming, adding aqua regia, fuming | 43.2 | 10.78 | 1.27 | 0.23 |
The above analysis results show that the synthetic ruby is decomposed by phosphoric acid in a fuming state of sulfuric acid for a long time, and the analysis results of aluminum,chromium and synthetic ruby are affected. Therefore, in order to keep the medium consistent and completely complex with tungsten, after the phosphoric acid is added, the medium is heated until the medium emits micro smoke and is taken down, and the analysis result is not influenced.
The invention relates to a component analysis method of a flexible wire, which is characterized by comprising the following steps: the analysis of other components in the solution after the above treatment by inductively coupled plasma atomic emission spectrometry (ICP-AES method) was carried out by: and testing the treated sample by using an inductively coupled plasma emission spectrometer, measuring the spectral line intensity of each element to be tested, and fitting according to the relation between the spectral line intensity and the element content to obtain the element content to be tested.
Adjusting the instrument according to the working condition of the instrument, measuring the spectral intensity of the element to be measured in each solution after the instrument is stable, and performing linear fitting by using a computer according to the relation between the spectral line intensity and the element content to measure the content of the element to be measured. Calculating the content of the element (M) to be detected according to the following formula:
M(％)＝kI+b
wherein k-represents the slope of the calibration curve; b-intercept of the working curve; i, measuring the signal intensity of the element to be measured.
ICP analysis of interference test among elements of Ni, Al, Cr, W, Mo, Ti, Co and Cu in two flexible wires
Ion solutions of different elements are prepared respectively, scanning is carried out on analysis spectral lines of different elements, and the results are shown in table 6:
TABLE 6 INTER-ELEMENT INTERFERENCE CONDITION TABLE
From the above data, it can be seen that there is no mutual interference between the spectral lines of the above elements. The spectral lines are the most sensitive analytical lines of the elements and do not interfere with each other. Therefore, the above spectral lines were selected as the analysis lines of the respective elements.
The method comprises the following steps of precision analysis:
the two flexible wires were analyzed for each analytical element as described above, and the results of six measurements are shown in table 7 (precision table):
| material | Element(s) | Results | Mean value of | RSD％ |
| First one Material | Ni | 32.68、32.78、32.51 32.77、32.65、32.55 | 32.66 | 0.34 |
| Cr | 1.27、1.27、1.27 1.28、1.28、1.27 | 1.27 | 0.39 | |
| Al | 11.34、11.19、11.41 11.25、11.36、11.74 | 11.38 | 1.67 | |
| W | 0.48、0.47、0.49 0.48、0.49、0.48 | 0.48 | 1.56 | |
| Mo | 0.39、0.39、0.39 0.40、0.40、0.39 | 0.39 | 1.28 | |
| Ti | 0.33、0.31、0.30 0.30、0.31、0.30 | 0.31 | 3.87 | |
| Co | 0.43、0.43、0.44 0.43、0.43、0.44 | 0.43 | 1.21 |
| Cu | 0.021、0.020、0.019 0.019、0.020、0.019 | 0.020 | 4.00 | |
| Synthesis of Red wine Treasure Stone (stone) | 39.6、39.4、39.8 39.2、39.7、39.5 | 39.5 | 0.55 | |
| Second kind Material | Ni | 62.02、62.34、62.18 62.25、62.30、62.11 | 62.20 | 0.19 |
| Cr | 2.50、2.53、2.49 2.51、2.50、2.53 | 2.51 | 0.67 | |
| Al | 21.01、20.95、21.03 20.98、20.94、21.04 | 20.99 | 0.20 | |
| W | 0.97、0.98、1.00 0.98、0.98、0.99 | 0.98 | 1.02 | |
| Mo | 0.73、0.72、0.72 0.73、0.74、0.73 | 0.73 | 1,03 | |
| Ti | 0.44、0.45，0.45 0.46、0.45、0.46 | 0.45 | 1.67 | |
| Co | 0.70、0.69、0.70 0.71、0.68、0.71 | 0.70 | 1.71 | |
| Cu | 0.04、0.04、0.05 0.04、0.04、0.05 | 0.04 | 4.5 |
Because the analysis methods of the alloy elements in the two alloy soft strips corresponding to the key points of the invention are the same, only the sample treated by the first material is subjected to the labeling test, the recovery rate is measured, and the results are shown in the table 8:
TABLE 8 recovery case
| Element(s) | The addition amount% | Results as% | The recovery rate is high |
| Ni | 10 | 42.58 | 99.2 |
| Al | 5 | 16.32 | 98.4 |
| Cr | 0.5 | 1.79 | 102.0 |
| Mo | 0.2 | 0.60 | 103.4 |
| Ti | 0.2 | 0.50 | 96.4 |
| Co | 0.3 | 0.72 | 96.7 |
| W | 0.3 | 0.77 | 100.2 |
| Cu | 0.03 | 0.05 | 101.3 |
As can beseen from tables 7 and 8, in the analysis range of the method, the relative standard deviation of other elements is less than 3% except that the content of copper is low and the deviation is less than 5%, and the recovery rate is between 96 and 104%, which indicates that the accuracy and precision of the method meet the requirements.
The inductively coupled plasma atomic emission spectrometry (ICP-AES) method is adopted to measure the nickel, aluminum, chromium, tungsten, molybdenum, titanium, cobalt and copper elements in the flexible wire rod, the method is good in accuracy and high in precision, and the requirements of production and scientific research can be met. The invention has strong adaptability, less investment, simple and convenient analysis and accurate result.
The specific implementation mode is as follows:
firstly, designing requirements (the embodiment is mentioned on the premise that the estimated values of the contents of the components meet the following conditions):
the first material consists of a certain amount of organic forming agent (the mass percentage content range of the organic forming agent in the total mass of the alloy wire material is 7-15%, and the preferable range is 8-12%) and Ni, Al, Cr, W, synthetic ruby, Mo, Ti, Co and Cu, wherein the relative mass content of other components except the organic forming agent is as follows: ni: 27 to 33; al: 8.0-13.0; cr is less than or equal to 1.5; w is less than or equal to 1.5; synthesizing ruby: 39.0 to 44.0; total amount of Mo, Ti, Co, Cu: less than or equal to 5; wherein the contents of Mo, Ti, Co and Cu are actually measured;
the second material: the alloy wire material consists of a certain amount of organic forming agent (the mass percentage content of the organic forming agent in the total mass of the alloy wire material is 7-15%, and the preferable range is 8-12%) and Ni, Al, Cr, W, Mo, Ti, Co and Cu, wherein the relative mass content of other components except the organic forming agent is as follows: ni: 52-57; al: 15.0 to 18.0; w is less than or equal to 2.0; total amount of Cr, Mo, Ti, Co, Cu: less than or equal to 8; wherein the contents of Cr, Mo, Ti, Co and Cu are actually measured;
II, test materials:
main materials: the two flexible wires;
auxiliary materials: sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, hydrofluoric acid, chromium, nickel, cobalt, molybdenum, tungsten, aluminum, titanium and copper standard solution (note: all the reagents used above are analytical reagents)
Wherein: hydrochloric acid: rho 1.19mg/ml
Nitric acid: rho is 1.42mg/ml
Phosphoric acid: rho 1.70mg/ml
Sulfuric acid: rho 1.84mg/ml
Chromium standard solution: 1mg/ml
Nickel standard solution: 1mg/ml
Cobalt standard solution: 1m/ml
Molybdenum standard solution: 1mg/ml
Tungsten standard solution: 1mg/ml
Aluminum standard solution: 1mg/ml
Titanium standard solution: 1mg/ml
Copper standard solution: 1mg/ml
Note: during the test, the above standard solution can be diluted appropriately according to the specific content of the analytical element.
Thirdly, equipment (I): JY70-PLUS inductively coupled plasma emission spectrometer
(II) the working conditions of the instrument:
high-frequency: 40.68 MHZ;
generator power: 1000W
Carrier gas flow: 0.5L/min;
carrier gas pressure: 0.3 MPa;
cooling air flow: 16L/min;
sheath gas flow rate: 0.2L/min;
observation height: 15 mm;
lifting amount of solution: 1.5 ml/min;
the analysis mode is as follows: multiple Cr channels: 267.716nm
Fe：259.940nm
Co：228.616nm
Ni：231.604nm
Mo：202.032nm
W：207.911nm
Al：396.152nm
Ti：337.279nm
Example 1 analysis of a first Material as a constituent analysis object
The first material consists of: a certain amount of organic forming agent (the mass percentage content range of the organic forming agent in the total mass of the alloy wire material is 7-15%, and the preferable range is 8-12%) and Ni, Al, Cr, W, synthetic ruby, Mo, Ti, Co and Cu; wherein the relative mass contents of other components except the organic forming agent are as follows: ni: 27 to 33; al: 8.0-13.0; cr is less than or equal to 1.5; w is less than or equal to 1.5; synthesizing ruby: 39.0 to 44.0; wherein the contents of Mo, Ti, Co and Cu are actually measured;
preparation of a test solution: accurately weighing 0.1000g of a sample in a 200ml polytetrafluoroethylene beaker, adding about 10ml of concentrated sulfuric acid, heating the sample on an electric furnace at a low temperature until the sample is carbonized and decomposed, taking down and cooling. Then, according to the aqua regia ratio, concentrated hydrochloric acid and concentrated nitric acid are (1-5) to 1; (preferably concentrated hydrochloric acid: concentrated nitric acid (2-4: 1)) is dissolved, hydrochloric acid is slowly added, and nitric acid is added after violent reaction; wherein the amount of nitric acid added is about 3 ml. Adding nitric acid, and heating in an electric furnace at low temperature until the sample is completely dissolved. Then dropping hydrofluoric acid 1ml and phosphoric acid 1ml, heating until slight smoke is produced, cooling, and adding water to dissolve salt.
Filtering the solution in a 100ml volumetric flask by using slow-speed filter paper; and washing with hot water for 5-8 times, then diluting the filtrate to scale, and shaking up to be tested. (the precipitate was stored for analytical synthesis of ruby).
Analysis of the content of synthetic ruby: and (3) continuously washing the precipitate remained in the process until the filtrate is neutral, then placing the precipitate into a ceramic crucible or a platinum crucible with constant weight in advance, ashing the precipitate in a high-temperature furnace at about 1000 ℃, then taking out the precipitate after washing again, placing the precipitate into a dryer, cooling and weighing. The content of the synthesized ruby was calculated as follows
In the formula: g-sample weight; g1-the weight of the crucible; g2Crucible and precipitation weight.
The analysis of other components in the solution after the above treatment by inductively coupled plasma atomic emission spectrometry (ICP-AES method) was carried out by: and testing the treated sample by usingan inductively coupled plasma emission spectrometer, measuring the spectral line intensity of each element to be tested, and fitting according to the relation between the spectral line intensity and the element content to obtain the element content to be tested.
Establishing an analysis curve: respectively adding Ni, Al, Cr, W, Mo, Ti, Co and Cu standard solutions into five volumetric flasks, wherein the specific contents of analytical curves are shown in Table 1; then adding 10ml of sulfuric acid and about 1ml of phosphoric acid, diluting with water to a scale mark, and shaking up for later use.
TABLE 9 Standard Curve
| Serial number | Ni | Cr | Al | Co | W | Mo | Ti | Cu |
| 1 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| 2 | 28 | 1 | 8 | 0.3 | 0.3 | 0.2 | 0.2 | 0.02 |
| 3 | 33 | 2 | 12 | 0.6 | 0.6 | 0.4 | 0.4 | 0.04 |
| 4 | 38 | 3 | 16 | 0.9 | 0.9 | 0.6 | 0.6 | 0.06 |
Adjusting the instrument according to the working condition of the instrument, measuring the spectral intensity of the element to be measured in each solution after the instrument is stabilized, and measuring the content of the element to be measured by performing linear fitting once by using the relation between the spectral line intensity and the element content through a computer to obtain the analysis curve of the content of each element in the standard solution to be measured.
Calculating an analysis result: the content of the element (M) to be measured was calculated as follows
M(％)＝kI+b
Wherein k-represents the slope of the calibration curve; b-intercept of the working curve; i, measuring the signal intensity of the element to be measured.
Example 2 analysis of a second Material as a constituent analysis object
The second material: the alloy wire material consists of a certain amount of organic forming agent (the mass percentage content of the organic forming agent in the total mass of the alloy wire material is 7-15%, and the preferable range is 8-12%) and Ni, Al, Cr, W, Mo, Ti, Co and Cu, wherein the relative mass content of other components except the organic forming agent is as follows: ni: 52-57; al: 15.0 to 18.0; w is less than or equal to 2.0; wherein the contents of Cr, Mo, Ti, Co and Cu are actually measured;
preparationof a test solution: accurately weighing 0.1000g of a sample in a 200ml polytetrafluoroethylene beaker, adding about 10ml of concentrated sulfuric acid, heating the sample on an electric furnace at a low temperature until the sample is carbonized and decomposed, taking down and cooling. Then, the aqua regia is prepared from the following components in percentage by weight: concentrated hydrochloric acid and concentrated nitric acid are (1-5) to 1; (preferably concentrated hydrochloric acid: concentrated nitric acid (2-4: 1)) is dissolved, hydrochloric acid is slowly added, and nitric acid is added after violent reaction; wherein the amount of nitric acid added is about 3 ml. Adding nitric acid, and heating in an electric furnace at low temperature until the sample is completely dissolved. Dropping hydrofluoric acid 1ml and phosphoric acid 1ml, heating until slight smoke is produced, cooling, and dissolving salt in water.
The analysis of other components in the solution after the above treatment by inductively coupled plasma atomic emission spectrometry (ICP-AES method) was carried out by: and testing the treated sample by using an inductively coupled plasma emission spectrometer, measuring the spectral line intensity of each element to be tested, and fitting according to the relation between the spectral line intensity and the element content to obtain the element content to be tested.
Establishing an analysis curve: respectively adding Ni, Al, Cr, W, Mo, Ti, Co and Cu standard solutions into five volumetric flasks, wherein the specific contents of analytical curves are shown in Table 1; then adding 10ml of sulfuric acid and about 1ml of phosphoric acid, diluting with water to a scale mark, and shaking up for later use.
TABLE 10 Standard Curve
| Serial number | Ni | Cr | Al | Co | W | Mo | Ti | Cu |
| 1 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| 2 | 28 | 1 | 8 | 0.3 | 0.3 | 0.2 | 0.2 | 0.02 |
| 3 | 33 | 2 | 12 | 0.6 | 0.6 | 0.4 | 0.4 | 0.04 |
| 4 | 38 | 3 | 16 | 0.9 | 0.9 | 0.6 | 0.6 | 0.06 |
Adjusting the instrument according to the working condition of the instrument, measuring the spectral intensity of the element to be measured in each solution after the instrument is stabilized, and measuring the content of the element to be measured by performing linear fitting once by using the relation between the spectral line intensity and the element content through a computer to obtain the analysis curve of the content of each element in the standard solution to be measured.
Calculating an analysis result:the content of the element (M) to be measured was calculated as follows
M(％)＝kI+b
Wherein k-represents the slope of the calibration curve; b-intercept of the working curve; i, measuring the signal intensity of the element to be measured.
Claims (10)
1. A flexible wire component analysis method is characterized in that: the organic matter was removed, the treated material sample was dissolved in aqua regia, low-melting acid was removed, and other components in the treated solution were analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES).
2. The method for analyzing the composition of a flexible wire according to claim 1, wherein: the flexible wire comprises the following two components in parts by weight:
the first material: the material consists of an organic forming agent and Ni, Al, Cr, W, synthetic ruby, Mo, Ti, Co and Cu, wherein the relative mass contents of other components except the organic forming agent are as follows: ni: 27 to 33; al: 8.0-13.0; cr is less than or equal to 1.5; w is less than or equal to 1.5; synthesizing ruby: 39.0 to 44.0; total amount of Mo, Ti, Co, Cu: less than or equal to 5;
the second material: the material consists of an organic forming agent and Ni, Al, Cr, W, Mo, Ti, Co and Cu, wherein the relative mass contents of other components except the organic forming agent are as follows: ni: 52-57; al: 15.0 to 18.0; w is less than or equal to 2.0; total amount of Cr, Mo, Ti, Co, Cu: less than or equal to 8.
3. The method for analyzing the composition of a flexible wire according to claim 2, wherein: the method for removing the organic matters comprises the steps of adding concentrated sulfuric acid into a sample, and heating at a low temperature until the sample is carbonized and decomposed.
4. The method for analyzing the composition of a flexible wire according to claim 2, wherein:
the aqua regia for dissolving the flexible wire rod is prepared from the following components in percentage by weight: concentrated hydrochloric acid and concentrated nitric acid are (1-5) to 1.
5. The method for analyzing the composition of a flexible wire according to claim 4, wherein: the process of dissolving the flexible wire by the aqua regia is as follows: firstly, dissolving a sample subjected to organic matter removal treatment in hydrochloric acid, and then adding nitric acid into the solution;
the aqua regia for dissolving the flexible wire rod is prepared from the following components in percentage by weight: concentrated hydrochloric acid and concentrated nitric acid are (2-4) to 1.
6. The method for analyzing the composition of a flexible wire according to claim 2, wherein: after dissolving the material with aqua regia and before driving off the low melting acid, hydrofluoric acid is added to the solution to remove silicon.
7. The method for analyzing the composition of a flexible wire according to claim 2, wherein: after dissolving the material with aqua regia and before driving off the low melting acid, phosphoric acid was added to the solution to complex W.
8. The method for analyzing the composition of a flexible wire according to any one ofclaims 2 to 7, wherein: filtering the first material before removing the low-melting-point acid to obtain a solid precipitate with synthetic ruby as a main component; washing the obtained precipitate until the filtrate is neutral, placing the precipitate in a crucible, ashing in a high temperature furnace to eliminate the influence of filter paper, cooling, and weighing.
9. The method for analyzing the composition of a flexible wire according to claim 2, wherein: the process for driving off the low-melting-point acid is as follows: phosphoric acid was added to the solution and heated until slight smoke was emitted.
10. The method for analyzing the composition of a flexible wire according to claim 1, wherein: the analysis of other components in the solution after the above treatment by inductively coupled plasma atomic emission spectrometry (ICP-AES method) was carried out by: and testing the treated sample by using an inductively coupled plasma emission spectrometer, measuring the spectral line intensity of each element to be tested, and fitting according to the relation between the spectral line intensity and the element content to obtain the element content to be tested.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102854180A (en) * | 2011-06-30 | 2013-01-02 | 中国石油天然气股份有限公司 | Method for detecting chromium content in chromium diethyl hexanoate by plasma emission spectrometry |
| CN104406956A (en) * | 2014-11-11 | 2015-03-11 | 中国纺织科学研究院 | Method for determining content of trace metal element in PAN-based carbon fiber |
| CN105136776A (en) * | 2015-07-21 | 2015-12-09 | 贵研检测科技（云南）有限公司 | Quick measurement method of Zr, Ce, La, Pr, Nd, Ba, Mg and Al in automobile catalyst |
| CN105300786A (en) * | 2015-11-20 | 2016-02-03 | 沈阳黎明航空发动机(集团)有限责任公司 | Composition analysis method for nickel chromium aluminum alloy porous ceramic composite powder |
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| KR930012290A (en) * | 1991-12-23 | 1993-07-20 | 원본 미기재 | Flame Sprayed Composite Film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102854180A (en) * | 2011-06-30 | 2013-01-02 | 中国石油天然气股份有限公司 | Method for detecting chromium content in chromium diethyl hexanoate by plasma emission spectrometry |
| CN104406956A (en) * | 2014-11-11 | 2015-03-11 | 中国纺织科学研究院 | Method for determining content of trace metal element in PAN-based carbon fiber |
| CN104406956B (en) * | 2014-11-11 | 2017-06-30 | 中国纺织科学研究院 | A kind of method of trace metal element content in measure PAN base carbon fibres |
| CN105136776A (en) * | 2015-07-21 | 2015-12-09 | 贵研检测科技（云南）有限公司 | Quick measurement method of Zr, Ce, La, Pr, Nd, Ba, Mg and Al in automobile catalyst |
| CN105300786A (en) * | 2015-11-20 | 2016-02-03 | 沈阳黎明航空发动机(集团)有限责任公司 | Composition analysis method for nickel chromium aluminum alloy porous ceramic composite powder |
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